for the state veterinary laboratory monitoring of residues of banned and harmful substances in live

1

PLAN for the state veterinary laboratory monitoring

of residues of banned and harmful substances in live animals, animal products and feeds

for 2013

2013

2

CONTENT

1. Plan for state veterinary laboratory monitoring of residues of banned and harmful substances in live animals, animal products and feeds

3

1.1. General information and address data of the competent executive authorities

6

1.2. Structure of state authorities involved in implementation of the Monitoring Plan

6

2. National plan for the state veterinary laboratory

monitoring of residues of banned and harmful substances in

live animals, animal products and feeds for 2013 and its

variances from the Plan for 2012

8

2.1. General principles for drawing up the Plan. Legal basis

for monitoring

11

2.2. Plan Structure and Explanations Necessary for Table Completion

13

2.3. Statistical data on livestock population in the Russian Federation, sample size and number of samples

13

2.4. Sampling procedure 14

2.5., 2.6., 2.7., 2.8. Planning. Selection of controlled

xenobiotics and veterinary drugs. MAL.

15

2.9., 2.10. Sample size and average sample size.

Preparation of documents

18

2.11. Summary of implementation of the Plan for 2013 21

2.12. Administrative measures taken in case of detection of

non-compliances

23

3. Laboratory network 3.1. List of laboratories involved in the Plan implementation

30

3.2. Data on certification (accreditation) of laboratories and capabilities for sample examination

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3.3. Residue control in the RF Subjects Table 5-20

38 39

LIST OF ABBREVIATIONS

225

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1. Plan for state veterinary laboratory monitoring of residues of banned and harmful substances in live animals, animal products and feeds. Introduction

The Plan for the state veterinary laboratory monitoring of residues of banned and

harmful substances in live animals, animal products and feeds was developed by the

working group in order to implement legal acts of the Russian Federation in the

veterinary sphere with the aim of verification of animal product safety as well as in

conformity with the requirements of the European Directive 96/23/EC of April 29,

1996 regarding monitoring of residues of banned and harmful substances in live

animals and animal products.

International requirements, rules and regulations for the safety of food products

and monitoring arrangement are laid down in the Section “General Principles of Food

Hygiene” of Codex Alimentarius, by the International Veterinary Code, WTO

Agreement on Technical Barriers to Trade, WTO Agreement on Application of

Sanitary and Phytosanitary Measures for 2002 -2005, EC Directives, the Customs

Union regulatory documents and other international legal and regulatory acts.

The systematic approach “from farm to fork” is laid down in Codex Alimentarius

and the EU requirements on food safety, approved by the European Parliament and

European Council in January, 2002 (EU Regulation 178/2002). The given EU

document sets up that the scientific analysis and risk assessment of food product

contamination by different chemical substances should be conducted independently,

objectively and should be based on recent scientific developments. These

requirements are laid down in the EC Directive 93/43 on food hygiene and received

further development in the HACCP system (hazard analysis and critical control

points), that is the major model for managing quality and safety of products at food-

processing plants of the developed countries of the world.

The following Community documents, regulating the product safety and the

procedure of monitoring arrangement, were used for drawing up the Plan:

Commission Regulation (EC) No. 466/2001 of March 8, 2001; Regulation (EC) No.

852/2004 of the European Parliament and Council of April 29, 2004; Regulation (EC)

No. 853/2004 of the European Parliament and Council of April 29, 2004; Regulation

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(EC) No. 854/2004 of the European Parliament and Council of April 29, 2004;

Commission Regulation (EC) No. 2073/2005 of November 15, 2005; Decisions

2004/432, 2003/181/EC, 2004/25/EC; Directive 2006/13/EC of February 03, 2006;

and other documents (Commission Decision No. 2002/657/EC of August 12, 2002;

Regulation No. 396/2005 of the European Parliament and Council of February 23,

2005; Commission Regulation No. 839/2008 of July 31, 2008; as well as Codex

Alimentarius documents).

The Plan for the state veterinary laboratory monitoring was developed using the

following national regulatory documents of the Russian Federation and the Customs

Union as the fundamental documents:

Law of the Russian Federation “Veterinary Law” No. 4979-01 of May 14,

1993;

Federal Law “Quality and Safety of Food Products” No 29-FZ, of January

02, 2000;

Federal Law “Safe Handling of Pesticides and Agrochemicals” No. 109-

FZ of July 19, 1997;

Federal Law “Radiation Safety of Population” of January 9, 1996;

Federal Law “Drugs Circulation” No. 61-FZ of April 12, 2010;

Regulation of the Russian Federation Government “State Surveillance and

Control for Food Product Safety and Quality” No. 987 of December 21,

2000;

Statute on monitoring of quality and safety of food products and public

health approved by the Regulation of RF Government No. 883 of

November 22, 2000;

Order of the RF Ministry of Agriculture “Implementation of the Plan for

State Veterinary Laboratory Monitoring” No. 780 of May, 30, 2003;

Regulation of the RF Government “Delineation of the Federal Executive

Body Powers in the Sphere of Biological and Chemical Safety in the

Russian Federation” No. 303 of May 16, 2005;

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Statute on social hygiene monitoring, approved by Regulation of the RF

Government No. 60 of February 02, 2006;

“Conception of state veterinary laboratory Monitoring of residues of

banned and harmful substances in live animals, animal products and feeds

in the Russian Federation for 2008 and subsequent years” approved be the

Head of the Federal Service for Veterinary and Phytosanitary Surveillance,

S.A. Dankvert on May 05, 2008;

Decision of Customs Union Commission “Application of Animal Health

Measures within the Customs Union” No. 317 of June 18, 2010;

Common health and epidemiological and hygiene requirements to

commodities subject to sanitary and epidemiological surveillance

(control), approved by CU Commission Decision No. 299 of May 28,

2010 as amended by No. 34 of August 17, 2010.

Veterinary regulatory and methodical documents and veterinary

legislation;

National standards of the Russian Federation and GOSTs.

Activities according to the Plan for state veterinary laboratory monitoring of

residues of banned and harmful substances in live animals, animal products and

feeds and also additional target programmes are performed in the territory of the

Russian Federation in 2013 at cost of the Federal Budget within the framework of

the Plan of Rosselkhoznadzor activities for compliance with the requirements of

WTO SPS Agreement during Russia’s accession to the WTO.

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1.1. General information and address data of the competent executive authorities

Ministry of Agriculture of the Russian Federation

107139, Moscow, Orlikov per., 1/11

Cable address: Moscow 84 Rosselkhoznadzor

Fax: +7(495) 607-5111, tel: +7(495) 975-4247

E-mail: [email protected]

http://www.fsvps.ru

1.2. Structure of state authorities involved in implementation of the Monitoring

Plan

New structure of the Ministry of Agriculture of the Russian Federation with the

distribution of execution and control functions was set by the Decree of the President

of the Russian Federation No. 314 of March 9, 2004 “System and Structure of Federal

Executive Authorities”. Federal Service for Veterinary and Phytosanitary Surveillance

(Rosselkhoznadzor) acting under the Provision approved by the Resolution of the

Russian Federation Government No. 327 of June 30, 2004 “Approval of the Provision

on the Federal Service for Veterinary and Phytosanitary Surveillance” was

established. The structure of the Service as well as its activity spheres and measures

were determined. The Rosselkhoznadzor comprises the following jurisdictional

institutions: Federal Governmental Budgetary Institution “Central Scientific and

Methodical Veterinary Laboratory”, Federal Governmental Budgetary Institution

“Central Research and Production Radiological Laboratory”, eighteen inter-oblast

veterinary laboratories, two research veterinary institutions FGBI VGNKI and FGBI

ARRIAH, FGBI “National Safety Center for Fishery and Aquaculture Products”,

FGBI “Federal Centre for Grain and Grain Product Quality and Safety Assessment”,

seventeen Rosselkhoznadzor reference centres including 8 of them carrying out

activities in the field of veterinary laboratory control.

63 territorial administrations of the Federal Service for Veterinary and

Phytosanitary Surveillance organize control in the regions with the purpose of

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implementation of the Plan for the state veterinary laboratory monitoring of residues

of banned and harmful substances in live animals, animal products and feeds.

8

2. National plan for the state veterinary laboratory monitoring of residues of banned and harmful substances in live

animals, animal products and feeds for 2013 and its variances from the Plan for 2012 Table 1

Submitted information

Federal Service for Veterinary and Phytosanitary Surveillance

(Rosselkhoznadzor)

107139, Moscow, Orlikov per.,1/11

For telegrams: Moscow 84, Rosselkhoznadzor

Fax:(495) 607-5111, Tel.: (495) 975-4347

Е-mail: [email protected]

http://www.svfk.ru

2. National plan for the state veterinary laboratory monitoring of residues of banned and harmful substances in live animals,

animal products and feeds (and results of the previous year)* 2012/2013

Exported by the RF commodities which are currently listed in Commission Decision 2004/432/EC (according to the last

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amendment)

Cattle Ovine/Caprine ׁ◌ Swine Equine Poultry Fish and non-fishery objects

Milk Eggs Rabbits Wild game Farmed game Honey

Please specify commodities, which are not currently in the RF export list in Commission Decision 2004/432/EC but which the RF

wishes to include in the list when ЕС Decision is updated, i.e. commodities which the RF wishes to export to the EU (specified

commodities are annually included by the RF into the Plan of residue monitoring and results are annually sent to the EU).

Fish and non-fishery objects (aquaculture), rabbits, wild game

Commodities, included in the Commission Decision 2004/432/EC, which the RF no longer wishes to export to the EU:

Russia does not plan to decrease the volume of food exports in the EU.

Commodities which are covered by the current Plan for the state veterinary laboratory monitoring of residues of banned and

harmful substances in live animals, animal products and feeds:



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Commodities, which safety is guaranteed by the Plan for the state veterinary laboratory monitoring of residues of banned and

harmful substances in live animals, animal products and feeds:



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2.1. General principles for drawing up the Plan. Legal basis for monitoring

The Plan for the state veterinary laboratory monitoring of residues of banned

and harmful substances in live animals, animal products and feeds was developed

based on the articles and statements of Council Directive 96/23 of April 29, 1996,

laid out in the abovementioned documents of p.1, Order of the RF Ministry of

Agriculture “Implementation of the Plan for State Veterinary Laboratory

Monitoring” No. 780 of May 30, 2003.

The Monitoring Plan was elaborated taking into account the requirements of

EU Council Directive 96/23/EC of April 29, 1996 “Measures for Monitoring of

Certain Substances and their Residues in Live Animals and Animal Products” (this

Directive is a fundamental document for development of control system of banned

and harmful substances for third countries planning export to the EU) and using the

data of the DG SANCO web-site http://ec.europa.eu/atoz_en.htm.

The annual collected volume of the RF Ministry of Agriculture “Agro-

industrial complex in Russia” is the source for the necessary data calculations

concerning animal population, production volume in the territory of the Russian

Federation, amounts of prepared feeds and so on. The calculation of the necessary

sample quantity and sampling frequency per different animal species and products

is carried out in accordance with Annex IV “Sampling Levels and Frequency” to

EU Council Directive 96/23/EC; the programme posted on the EU Council web-

site (http://ec.europe/eu/food/food/chemicalsafety/residues/index_en.htm) which

allows to calculate the minimal quantity of samples/tests taking into account the

data for the Russian Federation in accordance with the requirements of EU

Directive 96/23/EC and based on the results of laboratory tests of different product

types for the previous year.

The legal implementation of the Plan is ensured by the following Legal Acts

of the Russian Federation: the RF Law “On Veterinary Medicine” No. 4979-01 of

May 14, 1993, Statute of the Rosselkhoznadzor (Regulation of the RF Government

No. 327 of June 30, 2004), Statute of the State Veterinary Surveillance in the

Russian Federation (Regulation of the RF Government No. 706 of June 19, 1994)

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and other Russian and international legal acts in the sphere of animal health and

public health (See Point 1 of this Document).

2.2. Plan Structure and Explanations Necessary for Table Completion

Farmed and wild animals, animal products and feeds produced in the territory

of Russia are the objects under control in the monitoring.

The list of monitored objects is as follows:

biomaterials from live animals collected while alive at sites of their raising

and keeping (feeds, water)

biomaterials from live animals collected at sites of slaughter;

meat and meat products including offal and fat;

milk and milk products;

eggs and egg products;

fish, fishery objects and their products;

caviar;

honey and bee products

The tables consist of the following columns:

In the column “Group of monitored substances according to 96/23/EC of

April 29, 1996” groups of substances are indicated in conformity with Annex I to

Directive 96/23/EC of April 29, 1996 (A, B, B3). According to this Annex the

names of substance subgroups are also indicated.

In the column “Number of samples tested” the number of tested samples

planned for sampling and examination is demonstrated by the type of material.

In the column “Preparation name” names of monitored preparations, names

of active substances and metabolites, which presence can raise a suspicion in the

use of given preparations, are indicated.

In the column “Type of product” the list of products and biomaterials

intended for testing is shown. In the notes under the mark* more detailed

explanations about material type are given in tables.

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Contamination control methods in the RF laboratories are applied in

accordance with EU Commission Decision 2002/657/EC.

In the column “Screening method” the permitted mass screening methods for

testing large numbers of samples, which are used in laboratories for preliminary

laboratory control and detection of positive samples are demonstrated. The given

methods are available and possess sufficient sensitivity for screening.

The column “Confirmation method” shows methods used for confirmatory

test of screening-detected positive samples as well as for carrying out arbitrary

tests. (Commission Decision 2002/657/EC). Confirmatory tests are carried out

using foreign analytical equipment.

In columns “Detection limit of screening method” and “Determination limit

of confirmation method” the corresponding sensitivity limits of methods are

indicated.

The column “Admissible content levels” demonstrates maximum admissible

levels (hereinafter “MAL”) of toxic substances and drugs in products that are in

force now in the Russian Federation in terms of approved regulatory documents.

The column “Laboratories” indicates the laboratories participating in the

implementation of the programme, sampling and conducting of product safety

examinations.

2.3. Statistical data on livestock population in the Russian Federation,

sample size and number of samples

The total number of samples to be tested in respect of chemical criteria of

safety in 2013 is planned according to the EU requirements laid down on the EU

Commission web-site

(http://es.europa/eu/food/food/chemicalsafety/residues/index_en.htm).

The calculations are based on the animal population in the Russian Federation

in 2013 published in the data book of the RF Ministry of Agriculture for 2012,

whereas official statistical data for 2012 have not been summarized at the time of

planning.

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The cattle population is 20,1 million animals, pigs – 17.2 million animals,

small ruminants – 22.8 million animals, poultry – 473.4 million birds.

The production of meat is 10.9 million tons, milk – 31.6 million tons, eggs –

41113 million, honey – 54 thousand tons, feeds – 18,7 million tons.

The planned number of tested samples per product type is shown in Annex I

of this Plan.

2.4. Sampling procedure

The planned number of tests for 2013 is based on the production data of the

Russian Federation.

All agricultural products, exported by the Russian Federation in the EU and

other countries are subject to the total animal health control including complex

laboratory tests for the conformity of products with the requirements of the

importing countries.

Testing of products imported into the territory of the Russian Federation is

carried out for the compliance with the requirements of the Customs Union

separately.

Collection of samples for the state veterinary laboratory monitoring of

residues of banned and harmful substances in live animals, animal products and

feeds is conducted according to the approved Monitoring Plan as well as to the

current national standards and regulatory documents of the Russian Federation and

the Customs Union.

Due to the necessity of the harmonization of legal acts it is recommended to

be also guided by the requirements of Commission Decision 97/747/EC of October

27, 1997, Council Directive 96/23 of April 29, 1996 (Annex IV) and others during

the sampling.

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2.5., 2.6., 2.7., 2.8. Planning. Selection of controlled xenobiotics and veterinary

drugs. MAL.

The Rosselkhoznadzor specialists are basically guided by the EU

requirements (Council Directive 96/23/EC of April 29, 1996, Annex I) when select

controlled substances and draw up the Plan for state veterinary laboratory

monitoring of residues of banned and harmful substances in live animals, animal

products and feeds for 2013. National peculiarities of the current stage of the RF

agricultural industry development, risk level according to the data for 2012 and

global environment pollution are also taken into account during the process of

making out a list of controlled substances.

The list of residues of controlled harmful and banned substances in live

animals, animal products and feeds includes xenobiotics that are potentially

dangerous for human and animal health, affect ecological situation, easily pass the

biological chains and accumulate in animals and animal products.

Veterinary drugs, banned for use in the EU and RF, are also under control.

Residues of persistent organic pollutants (hereinafter POP) and pesticides

currently banned for use in Russia but widely used before are controlled either.

Besides, residues of drugs, agrochemicals, pesticides registered and approved

for use in Russia are monitored.

The list of controlled residues is drawn up in accordance with the

international documents (EU), CU and RF documents:

Council Directive 96/23/EC of April 29, 1996 on measures to monitor

certain substances and residues thereof in live animals and animal

products;

Council Directive 96/22/EC of 29 April 1996 concerning the

prohibition on the use of substances having a hormonal or thyreostatic

action and of beta-agonists in animal production;

Directive 2003/74/EC of the European Parliament and of the Council

of 22 September 2003 amending Council Directive 96/22/EC;

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Commission Regulation No 37/10 (EU) of 22 December 2009 laying

down a Community procedure for the establishment of maximum

residue limits of veterinary medicinal products in foodstuffs of animal

origin;


of 7 May 2002 on undesirable substances in animal feed;

Commission Regulation (EC) No 839/2008 of 31 July 2008 amending

Regulation (EC) No 396/2005 of the European Parliament and of the

Council as regards Annexes II, III and IV on maximum residue levels

of pesticides in plant products;

Commission Directive 2006/13/EC of 3 February 2006 amending


on undesirable substances in animal feed as regards dioxins and dioxin-

like poly-chlorinated biphenyls (hereinafter PCBs);

CU Commission Decision No.317 of June 18, 2010 “Application of

veterinary and sanitary measures in the Customs Union”;

Common veterinary (veterinary and sanitary) requirements for the

commodities subject to veterinary control (surveillance), approved by

CU Commission Decision No.317 of June 18, 2010;

Common sanitary and epidemiological and hygiene requirements for

the commodities subject to veterinary control (surveillance), approved

by CU Commission Decision No.299 of May 28, 2010 with

amendment No.34 of August 17, 2010.

The list of controlled substances for 2013 is also determined by the result analysis

of preliminary review data obtained in 2012 and evaluation of pollution risk level.

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GROUPS OF SUBSTANCES

subjected to the state veterinary monitoring according to the RF Monitoring

Plan for 2013

Group A (A) – substances with an anabolic effect and banned substances

1. Stilbenes, their derivatives, salts and ethers 2. Thyreostatics 3. Steroids 4. Resorcylic acid lactones including zeranol 5. Beta-Agonists 6. Substances included in the Annex (Table 2) of Commission Regulation

No. 37/10 (EC) Chloramphenicol Nitrofurans (including furazolidone) Nitroimidazols

Group B (B) – veterinary drugs and ecological pollutants

1. Antibacterial substances including sulfanilamides and quinolones 2. Other veterinary drugs

a) Anthelmintics b) Coccidiostats c) Carbamates and pyrethroids d) Sedative substances e) Non-steroid anti-inflammatory substances f) Other pharmacologically active substances

3. Other substances and environmental contaminants

a) Organochlorine compounds including PCB b) Organophosphorous compounds c) Chemical elements d) Mycotoxins e) Colorants f) Other substances including unpatented drugs that may be used for

veterinary purposes (histamine, radionuclides, agrochemicals, microbiological criteria etc.)

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Plan for 2013 includes all groups of chemical substances which regulation is

expedient for the Russian Federation for each type of products.

Products exported from the RF should correspond to the international

requirements and the requirements of importing countries. Products imported to

Russia should correspond to the CU and RF requirements.

2.9., 2.10. Sample size and average sample size. Preparation of documents

Sampling procedure is harmonized to a maximum degree with Council

Directive 96/23/EC of 29 April 1996 and international regulatory documents.

National requirements are also taken into account in sampling. Sampling

procedure is aimed at maximum facilitation of violation detection.

The established average sample sizes (total amount of sample for A and B

samples) are calculated for the purpose of chemical tests within the state veterinary

laboratory monitoring of residues of banned and harmful substances in live

animals, animal products and feeds, as well as for tests conducted under veterinary

and sanitary expertise according to mandatory safety requirements laid down in

CU documents, Federal Laws (Special technical Regulations), SanPiN 2.3.2.1078-

01 “Hygiene requirements for safety and nutritional value of food products”,

GOST and National standards and Methodical instructions.

In the Russian Federation sampling is traditionally conducted according to

GOST.

Besides, requirements of current diagnostic regulatory documents of

veterinary legislation and “Unified rules for sampling agricultural products, food

products and environmental objects for detection of pesticide micro quantities”

(approved by the Deputy Head of the USSR Chief Sanitary Officer of 21.08.1979

No. 2051-79) are observed in sampling biomaterial.

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Table 2

Name of test material (products) Average sample size

Products:

Meat, offal and meat products 0.2-1.0 kg

Milk 0.5 l

Dry milk products 0.3 kg

Eggs 20 items

Honey 500 g

Fish and fish products 0.6-3.0 kg

Frozen fish products 0.4-0.6 kg

Fish glue (edible and inedible) 0.6-1.0 kg

Dried spinal cord 0.25 kg

Pearl paste 0.4 kg

Caviar 0.15-0.45 kg

Biomaterial:

Blood 20-200 ml

Urine 500 ml

Liver 500 g and more

Bile (Liver or its part is collected with the

gall bladder)

Muscles 500 g

Contents of stomach, intestine, etc. 500 g

Feeds 1.0-2.0 kg

Water for animals and aquaculture water

bodies

1-2 l

Sample sizes specified in Table 2 are considered sufficient for preliminary

(screening) and confirmation monitoring tests.

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Transportation and storage of samples generally comply with international

requirements (EU) and National standards, GOST, “Unified rules for sampling

agricultural products, food and environmental objects for detection of pesticide

micro quantities” (approved by the Deputy Head of the USSR Chief Sanitary

Officer of 21.08.1979 No. 2051-79).

Each average sample after collection should be packed in an airtight, clean,

dry and waterproof container and (or) special strongbox. Each package should be

labeled with indication of number and name of the sample, date and place of

collection. The label (particulars) should be wrapped in a cellophane

(polyethylene) bag and packed together with the sample. Each container or bag

should be sealed (in such a way that it is impossible to open it without seal removal

(broken seal).

Coding of samples is carried out by the Rosselkhoznadzor specialists.

Samples should be transported under conditions preventing access of

unauthorized persons.

Samples should be delivered to a laboratory chilled and not later than 24

hours after collection. Biomaterial samples should be delivered to the laboratory

immediately.

If the materials received by a laboratory are unfit for testing (due to opening

of the container, package or sample damage) the laboratory has a right to

decommission the samples and prepare a report indicating the sample state and the

reason for their decommissioning. In case of delivery of samples which are unfit

for testing the laboratory has a right to request for repeated sample submission.

A control sample of each batch to be tested is remained in the laboratory.

Samples are stored in a separate specially equipped room in the laboratory.

Perishable samples (food products, biomaterials, succulent fodders, etc.) are stored

in freezing or refrigerating chambers. Other samples are stored at room

temperature. Storage period depends on expiry date of a product batch, time

allowed for claims for supplied products but should be at least 3 months from the

date of testing.

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Collected samples and control samples are disposed after testing and shelf-

life expiration, unless otherwise specified by the agreement between contractor and

customer.

In general, testing of samples takes from 1 to 4-6 weeks depending on

number of samples and types of controlled parameters. These terms are not

applicable in case of emergency diagnosis as well as in case of control for

contamination of products with novel previously non-tested toxic substance for

detection of which additional reference samples, reagents, diagnostica, etc. are

required.

2.11. Summary of implementation of the Plan for 2013

In 2013 samples were collected according to the numbers specified in the

plan. Pursuant to the Order of the Ministry of Agriculture of the Russian

Federation “Implementation of the plan for state veterinary laboratory monitoring”

No. 780 of 30 May 2003 a report on the results of monitoring carried out in the

previous year and plan for monitoring in current year were prepared in the first

quarter of 2013 for submission to the European Commission. (Preliminary reports

are collected each quarter to gather information on the Plan implementation).

All veterinary laboratories forward a 4-vet B Form urgent report in case of

detection of positive results or banned chemical substances, veterinary drugs and

bacterial contamination (disease) from 2008 in accordance with the Order of the

Ministry of Agriculture of the Russian Federation “Procedure for entry of

information into state agriculture database” No. 189 of 2 April, 2008.

Laboratories (regional, interregional, zonal) that have got positive results

should forward urgent report to higher-level laboratories of the Subjects of the

Russian Federation within 12 hours after issuing their opinions.

Veterinary Laboratories of the RF Subjects, Interoblast Veterinary

Laboratories (regional), Reference Centres communicate the data by telephone/fax

(495) 700-01-37 according the established procedure to the FGBI “Central

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Scientific and Methodical Veterinary Laboratory” (the FGBI “CSMVL”) within 12

hours of obtaining positive results or receipt of relevant information. The FGBI

“CSMVL” performs assessment and compiles data obtained from veterinary

laboratories and forwards the information to the Rosselkhoznadzor and to the

Veterinary Department of the RF Ministry of Agriculture (Moscow, Orlikov per.,

1/11).

The following is considered to be a positive result:

Non-compliance with requirements of the Customs Union regulatory

documents;

Exceeding “Temporal maximum acceptable level (MAL) of some chemical

elements and gossypol in feeds for farmed animals and feed additives”

approved by the GUV of the USSR Gosagroprom on August 7, 1987;

Exceeding admissible levels mentioned in “Maximum admissible residue

levels of pesticides in feed for farm animals”: State Veterinary Department

of the Ministry of Agriculture of the USSR (agreed with the Ministry of

Health of the USSR on 31.03.77, 05.04.79, 03.02.81, No. 123-5/126-23): of

May 17, 1977, April 03, 1981 No. 117-11.;

Exceeding maximum admissible levels of mycotoxins in feeds, approved by

the regulatory documentation of the Veterinary Service and GOST;

Detection of residues of medical preparations not registered in the Russian

Federation;

Detection of growth promoters prohibited by “Rules for the state veterinary

monitoring of hormone growth promoters and thyreostatics in animal

products”, approved by the Ministry of Agriculture and Food of the Russian

Federation on August 18, 1999, No. 604;

Incompliance of products with the safety requirements of the Federal

legislation (specific technical regulations), national standards and GOST;

Exceeding international safety criteria (EU) in the exported products.

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Note 1. For the purpose of control of the hormonal growth promoter application in

the Russian Federation there are test-systems, techniques and regulatory

documentation, which are currently fully harmonized with the international ones

(EU).

Note 2. During the monitoring of Group A3 substances, natural level of

nortestosterone in a number of animals is taken into account and during tests for

A4 a possibility of P.Fusarium intake by the animals with feed is taken into

account and excluded.

In 2013 a significant growth in the number of monitored substances is

planned. The highest priority will be given to the monitoring of veterinary drugs

(B1, B2) in animal products due to the relevance of this issue both for domestic

and imported products. Considerable attention will be given to control of dioxins in

products.

2.12. Administrative measures taken in case of detection of non-compliances

In the Russian Federation when samples are taken on farms or at different

stages of the product turnover, it is always possible to trace the origin of products

under control, because products of animal origin are accompanied by standard

veterinary documents during transportation within the country (Veterinary

certificate Form No.2, Form No. 3 and No.4) (veterinary card – valid for

transportation within the region). Implementation of computer technologies in

routine veterinary procedures significantly facilitates tracing of products and

makes the work of veterinary specialists transparent.

Automatic computer systems “Argus”, “Mercury”, “Cerberus”, “Assol”

(reporting) have been implemented by the Rosselkhoznadzor. Computer

programme “Vesta” is used in laboratories.

It is the owner (producer) of products who is responsible for their quality and

safety.

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In case low-quality products are detected, administrative actions are taken

against owners (producers) according to the following documents of the Russian

Federation:

Law of the Russian Federation "On Veterinary Medicine". No. 4979-01

dd. 14 May 1993 (as amended by FZ-199);

Federal Law “On Quality and Safety of Food Products” No. 29-FZ dd.

2 January 2000;

Regulation on the expertise of poor-quality and hazardous food

ingredients and foodstuff and their utilization or disposal approved by

Government Decree No. 1263 dd. 29 September 1997;

RF Government Decree No. 295 dd. 16.04.2001.

Authorities providing state surveillance and control of food quality and safety

carry out the expertise of poor-quality and hazardous food raw materials and food

products within their competence. These authorities also make decisions on

whether it is possible to further use these products or they shall be disposed.

Such hazardous food products shall be withdrawn from sales, examined,

recycled or disposed.

Poor-quality and hazardous food products shall be kept in a separate room in

a warehouse, in a refrigerator (isolated chamber) over the whole period required to

examine them, make and execute a decision on their further use or disposal under

conditions that exclude any access to them.

Food products for temporary storage shall undergo a strict registration

procedure.

Owner of the products is responsible for their safe-keeping and shall bear

costs for transportation of poor-quality and hazardous food products, their storage,

expertise, use or disposal.

Expertise (sanitary and hygienic, veterinary and sanitary, trade examination,

etc.) of poor-quality and hazardous food products is carried out by the state

authorities providing surveillance and control within their competence.

25

Decisions made by the state surveillance and control authorities on whether

the food products shall be banned for human consumption or disposed, may be

appealed in the manner prescribed by the RF legislation.

26

Ministry of Agriculture of the Russian Federation

Laboratories:

Federal Service for Veterinary and Phytosanitary Surveillance

Territorial Administrations of the Federal Service for Veterinary and

Central Scientific and Methodical Veterinary Laboratory

Central Scientific and Production Veterinary Radiological Laboratory

Interoblast Veterinary Laboratories (18)

National Centre for Quality and Safety of Aquatic products and Aquaculture FGBI NTSBRP

Rosselkhoznadzor reference centres, carrying out activities in the field of veterinary control

All-Russian State Centre for Quality and Standardization of Veterinary Drugs and Feeds – FGB VGNKI

Federal Centre for Animal Health, Vladimir – FGB ARRIAH

27

List of substances and groups of substances the residues of which will be monitored in the RF according to the Monitoring Plan for 2013 (by animal species and products) Table 3

Animal species and types of products included in the Plan for 2013

Cattle Small ruminant

Pigs Horses Poultry Aquaculture*

Milk Eggs Rabbits Field game

Farmed game

Honey

Mea

t

Bef

ore

slau

ghte

r

Fish

Non

-fis

hery

ob

ject

s

Monitored substances and groups of substances А1 Stilbenes А2 Thyreostatics А3 Steroids (natural and

synthetic)

А4 Resorcylic acid lactones А5 -Agonists

А6 Substances from Table 2 of Annex 37/10 (EC)

Chloramphenicol

Nitrofurans

Nitroimidazoles

В1 Antibacterial Substances В2а Anthelminthics В2b Coccidiostatics B2c Carbamates

Pyrethroids B2d Sedatives B2e Nonsteroidal anti-

inflammatory drugs

28

Phenylbutazone B2f Other pharmacologically

active substances

Carbadox, Olacvindox B3a Organochlorine

compounds, including PCB

B3b Organophosphorous compounds

B3c Chemical elements B3d Mycotoxins B3e Colorants (benzal green,

p-tetratmethyldiaminotrypheny methane, red violet)

B3f Other substances including unpatented drugs, pesticides, biotoxins and radionuclides, etc.

Substances subject to mandatory monitoring, according to the Monitoring Plan of the RF and applicable normative documents for the products.

Monitoring of the substances is highly desirable according to the Monitoring Plan, EC requirements and applicable regulatory documents

of the RF. Monitoring of these substances in the mentioned objects is not required.

Monitoring is obligatory of the mentioned groups of substances and xenobiotics in feeds according to the Monitoring plan and regulatory

documents.

29

Structure of the residue monitoring in the Russian Federation

Fig.2.

FGBI ARRIAH

FGBI VGNKI

FGBI CSMVL

FGBI CSPVRL

18 Federal State Interoblast

Laboratories of the

Rosselkhoznadzor (FGBI IVL)

Territorial Administrations of the Rosselkhoznadzor and State Veterinary Service of the RF Subjects

(sample collection in the area of responsibility)

The Rosselkhoznadzor bodies conducting

studies in the veterinary field

(reference centres in the RF Subjects)

FGBI NSCFAP

ROSSELKHOZNADZOR

30

3. Laboratory network 3.1. List of laboratories involved in the Plan implementation

The following federal budgetary veterinary laboratories of the Russian Federation subordinate to the Rosselkhoznadzor participate in the implementation of the Plan for the state veterinary laboratory monitoring of residues of banned and harmful substances in live animals, animal products and feeds for 2013:

Table 4 No. Laboratory Name Address, telephone 1. All-Russian State Center for

Quality and Standardization of Veterinary Preparations and Feed (FGBI “VGNKI”)

123002, Moscow, Zvenigorodskoye shosse, 5 (495) 253-14-69 (495) 256-44-42 (accounting office) [email protected] http://www.vgnki.ru

2. Federal Center for Animal Health (FGBI “ARRIAH”)

600901, Vladimir, Yur’evets Director’s office: (4922) 26-06-14 Tel/fax (4922) 26-15-73, fax (4922) 26-38-77 [email protected] http://www.arriah.ru

3. FGBI “Belgorodskaya Interoblast Veterinary Laboratory”

308807, Belgorod, Studencheskaya ul., 32 (4722) 34-11-15 (director’s office) 34-92-79 (fax) [email protected] http://www.belmvl.ru

4. FGBI “Bryanskaya Interoblast Veterinary Laboratory”

41520, Bryanskaya Oblast, Bryansky Rayon, s. Suponevo, Shosseynaya ul., 7 (4832) 92-24-84 92-17-28 92-18-31 (acc. office) [email protected] http://bmvl.bryansktel.ru

5. FGBI “Irkutskaya Interoblast Veterinary Laboratory”

664005, Irkutsk, Botkina ul., 4 (3952) 39-49-09 38-75-74 (acc. office) 38-72-89 (director’s office) [email protected] http://www.vetlab38.ru

31

6. FGBI “Kamchatskaya

Interoblast Veterinary Laboratory”

684007, Kamchatskaya Oblast, Elizovo, Novaya ul, 8 (41531) 6-22-89 6-14-62 [email protected] http://www.kamchmvl.ru

7. FGBI “Kaliningradskaya Interoblast Veterinary Laboratory”

236038, Kaliningrad, Tankovaya ul., 15 Post address: 236035, Kaliningrad, POB 5162 (4012) 35-28-57 46-35-38 46-07-81 [email protected], [email protected] http://www.kmvl.ru http://кмвл.рф

8. FGBI “Kemerovskaya Interoblast Veterinary Laboratory”

650021, Kemerovo, Pavlenko ul, 3 (3842) 57-20-86 57-00-60 [email protected] http://www.kmvl.kemv.ru

9. FGBI “Krasnodarskaya Interoblast Veterinary Laboratory”

350004, Krasnodar, Kalinina ul, 15 (8612) 21-64-72 (fax) 21-61-62 21-61-70 [email protected] http://krasnodarmvl.ru

10. FGBI ”Krasnoyarsky Reference Center”

660049, Krasnoyarsk, POB 5431 (post address) 660049, Krasnoyarsk, ul. Markovskogo, 45 (legal address) (3912) 27-08-92 27-67-95 (fax) 27-26-08 (fax) [email protected] http://www.krs-ref-ru

11. FGBI “Leningradskaya Interoblast Veterinary Laboratory”

196158, St. Petersburg, Moskovskoe shosse, 15 (812)

32

373-51-43 (director’s office) 382-57-69 (fax) [email protected] http://www.vetlab.spb.ru

12. FGBI “Magadanskaya Interoblast Veterinary Laboratory”

685000, Magadan, Chukotskaya ul, 20a (4132) 636242 636247(director’s office) [email protected] http://www.magrsn.ru/new/

13. FGBI ”Natsrybbezopasnost” – for aquaculture

Russia, 129223, Moscow, pr-t Mira, All-Russian Exhibition Centre, 119, bld. 334, POB 49 (495) 984-69-70 984-69-71 984-69-72 984-69-73 984-69-74 http://www.fishquality.ru [email protected]

14. FGBI “Novosibirskaya Interoblast Veterinary Laboratory”

630007, Novosibirsk, Serebrennikovskaya ul, 5 (3832) 23-42-40 18-81-93 (fax) 17-72-01 [email protected] http://www.nmvl.ru

15. FGBI “Nizhegorodsky Reference Centre”

66-40-78 (fax) 66-37-58 [email protected] http://www.refcenter-pro.ru

16. FGBI “Orlovsky Reference Centre”, 302040, Orel, Pozharnaya ul, 72 (legal address)

302040, Orel, Pozharnaya, 72 (physical address) (4862) 42-38-06 (director’s office) 42-38-08 (dep. dir.) 42-38-04 (ac. office) http://www.refcenter57.ru [email protected]

17. FGBI “Omsky Reference Centre”

644031, Omsk, 10 Let Oktyabrya ul, 197 (3812) 32-91-30 (director’s office)

33

32-90-38 (dep. dir.) [email protected] http://omskrefcentr.ru

18. FGBI “Orenburgsky Reference Centre”

460052, Orenburg, Montazhnikov ul, 34 (3532) 75-90-92 [email protected] http://oren-refcentr.ru

19. FGBI “Primorskaya Interoblast Veterinary Laboratory”

692502, Primorsky Krai, Ussuriysk, Belinskogo ul, 3 (42343) 32-70-05 32-70-38 35-63-90 [email protected] http://prim-mvl.ru

20. FGBI “Saratovskaya Interoblast Veterinary Laboratory”

410064, Saratov, Leninsky Rayon, Blinova ul, 13 (8452) 62-56-53 (director’s office) 62-16-54 [email protected] http://mvl-saratov.ru

21. FGBI “Sahalinskaya Interoblast Veterinary Laboratory”

693000, Yuzhno-Sakhalinsk, Saranskaya ul, 17a (4242) 42-97-27 (fax) 42-35-87 [email protected] http://ww.fgu-sakhmvl.ru

22. FGBI “Stavropolskaya Interoblast Veterinary Laboratory”

355000, Stavropol, Taromaryevskoe shosse, 34 (8652) 28-17-56 28-16-53 (fax) [email protected] http://stavmvl.ru

23. FGBI “Tatarskaya Interoblast Veterinary Laboratory”

420087 Kazan, Rodiny ul., 25a (8432) 29-17-10 (fax) 29-17-20 29-13-72 (secretary) [email protected]

24. FGBI “Tverskaya Interoblast Veterinary Laboratory”

170007, Tver, Shishkova ul, 100 (4822) 53-50-01 52-52-79 (fax)

34

[email protected] http://www.tmvl.ru

25. FGBI “Tulskaya Interoblast Veterinary Laboratory”

301130, Tulskaya Oblast, Leninsky Rayon, Leninsky s., Mira ul, 13 (legal address) 300045 Tula, Nekrasova ul, 1a (physical address) (4872) 36-07-34 30-45-74 30-45-70 30-45-73 [email protected] [email protected] http://www.fguvetlab.ru

26. FGBI “Chelyabinskaya Interoblast Veterinary Laboratory”

454008, Chelyabinsk, Sverdlovsky tract, 20 (3517) 22-48-33 26-16-50 (fax) 21-09-23 (secr.) [email protected] http://www.mvl74.ru

27. FGBI “Central Scientific and Methodical Veterinary Laboratory”

(FGBI CSMVL) 111622, Moscow, Oranzhereynaya ul, 23 700-01 -37 (director’s office) 700-05-23 700-39-52 (acc. office) http://www.cnmvl.ru

28. FGBI “Central Scientific and Production Veterinary Laboratory” (FGBI “CSPRVL”)

656056, Barnaul, u. Gorkogo, 4 (3852) 24-25-48 (fax) 24-49-91 (director’s office) 24-08-44 (acc. office) [email protected] http://www.fgu-radiovetlab.ru

29 FGBI “Rostovsky Reference Centre”

344034, c. Rostov-na-Donu, Sinyavskiy l., h.21v, (863) 224-13-38 224-09-37 http://www.referent61.ru [email protected]

35

Structure of the Laboratory Network of the Russian Federation

FGBI ARRIAH

FGBI CSMVL

FGBI VGNKI

FGBI CSPVRL

18 Federal State Interoblast

Laboratories of the Rosselkhoznadzor (FGBI

IVL)

The Rosselkhoznadzor bodies conducting studies in

the veterinary field (reference centres) - 8

74 State Veterinary Laboratories of the RF Subjects,

2 State Municipal Veterinary Laboratories (Moscow, Saint-Petersburg)

FGBI CSPVRL

36

3.2. Data on certification (accreditation) of laboratories and capabilities for sample examination

All interoblast veterinary laboratories and Reference Centers of the

Rosselkhoznadzor, participating in the Plan implementation, are accredited by the

Federal Agency for Technical Regulation and Metrology according to GOST-R of

the Russian Federation for compliance with GOST-R ISO/IEC 17025-2005.

Besides, all FGBI IVL and FGBI RC of the Rosselkhoznadzor engaged in

Plan implementation are also accredited by the Rosselkhoznadzor for veterinary

and grain quality control.

3.3. Residue control in the RF Subjects

The worked out Plan of “Monitoring of residues of banned and harmful

substances in live animals, animal products and feed in 2013” is harmonized with

the system adopted in the EU, as well as based on considerable national experience

of veterinary control of food and feed safety criteria. Monitoring pan for 2013 was

elaborated taking into account national peculiarities of use of veterinary

preparations, pesticides, agrochemicals in the Russian Federation, as well as

considering positive results obtained in 2012. In 2013 the Rosselkhoznadzor will

conduct control activities in the territory of all subjects of the Russian Federation.

Control of pesticides and agrochemicals in products and biomaterials will be

conducted taking into account data specified in the “State register of pesticides and

agrochemicals allowed for use in the territory of the Russian Federation in 2012-

2013”. Control of persistent organic pollutants and previously used pesticides

which residues can be detected in the territory of the RF will be also performed.

Any violations associated with illegal, unauthorized use of banned and

unregistered drug preparations and pesticides will be especially strictly monitored.

Antibacterial agents and other veterinary drug preparations are used in Russian

agriculture under control of veterinary service. Hormonal growth promoters are

banned for use in Russia.

37

List of control parameters for the state veterinary monitoring of residues of drug preparations, banned and toxic substances for Veterinary Laboratories in the Russian Federation for 2013 (cattle)

Table 5

Group of substances

according to 96/23/ЕС of

29.04.96

Number of samples

Name of the product (active substance),

metabolites

Type of product (object

of testing)

Screening methods

Confirmation

methods

Detection limit for the screening method μg/kg

Detection limit for the

confirmation method μg/kg

Admissible levels

(standards)

А

А1) Stilbenes, (А2) Thyreostatics, (А3) Synthetic steroids, (А3) Natural steroids

4194

4194

4194

4194

Diethylstilbestrol, Hexestrol, Dienestrol Thiouracil, Methyluracil, etc. 19-Nortestoterone, Trebolone, Methyltestoterone, Acetylgestagen, including Medroxyprogesteron acetate Ethinylestradion Trenbolone acetate Testosterone, Progesterone, Oestradiol -17

Biomaterials from cattle, etc.

ELISA GC-МS

ELISA GC-МS

ELISA GC-МS

ELISA

GC-МS

GC-МS

- // -

- // -

0.25-2.8

μg/kg

0.1 –0.5 μg/kg

0.25-2.8 μg/kg

0.1 –0.5 μg/kg

0.25 μg/kg

0.5 μg/kg

0.1 –0.5 μg/kg

- // -

- // -

Non-admissible Non-admissible Non-admissible 0.015 mg/kg 0.015 mg/kg 0.0005 mg/kg

38

А

(А4) Resorcylic acid lactones (А5) -Agonists

See above 4194

Zeranol Clenbuterol, Salbutamol, Terbutaline, Mapenterol, Cymbuterol, etc.


ELISA GC-МS

- // -

0.05μg/kg

0.25-2.8 ng/g

0.25-2.8 μg/kg

0.1 –0.5 μg/kg

0.25-2.8 μg/kg

0.1 –0.5 μg/kg

- // -

- // -

Non-admissible Non-admissible

39

(А6) Substances (Table 2), Annex 37/10 (EC)

4194

Chloramphenicol Nitrofurans and metabolites: AOZ, SEM, AHD, AMOZ Nitroimidazole derivatives (dimetridazol, metronidazol, ronidazol, etc.)


ELISA, HPLC- MS-MS

ELISA, HPLC- MS-MS

HPLC- MS-MS (HPLC)

GS-MS, HPLC- MS-MS

HPLC- MS-MS

HPLC- MS-MS (HPLC)

0.25 mg/kg

\

0.1 μg/kg 0.2 μg/kg

0.25-1.0 μg/kg

0.25-1.0 μg/kg

0.1-0.3 μg/kg

0.25 –1.0 μg/kg

0.25-1.0 μg/kg

Non-admissible Non-admissible Non-admissible

В (В1) Antibacterial substances, including sulfanilamides and quinolones

12080

Tetracycline (Oxytetracycline, Metacycline, Doxycycline), Bacitracin, Grisin, etc.


HPLC Microbiological ELISA HPLC-MS-МS

HPLC-MS-МS

0.1-0.2 μg/kg 0.01 U/g 6.0 μg/kg 0.5-0.01 U/g 0.5-5.0 μg/kg

0.5-5.0 μg/kg Non-admissible

40

Sulfanilamides (sulfamethazine, sulfadimethoxine, sulfadiazine, etc. (at least 8 compounds)

ELISA (imp.)

MS-MS HPLC

HPLC-MS-МS

20 μg/kg 1.0-10.0

μg/kg

1.0 –10.0 μg/kg SanPin 2.3.2.2804-10, CU CR, Decision No. 299.

Fluoroquinolones (enrofloxacine, ciprofloxacine,etc.)

ELISA (imp.) HPLC- MS-МS

HPLC-MS-МS

10 μg/kg 0.1-10.0

μg/kg

0.1 –10.0 μg/kg SanPin 2.3.2.2804-10, CU CR, Decision No. 299.

В

(В2a) Anthelminthics

170

Blue vitriol (Copper sulphate)


(for copper) Colorimetry ААS

AAS, AAS-ETA

0.25 – 0.4 mg/kg

CU CR, Decision No. 299

-

41

20

7420

Hexychol (hexachlorparaxylene)

HPTLC

HPLC

HPLC-MS-

MS

0.03-0.05

mg/kg

0.5-5.0 μg/kg


Avermectines (Ivermectin, Doramectine, Abamectine, Moxidectine, Emamectine) Other anthelminthics (benzimedazol derivatives)

HPLC HPLC-MS-MS 1.0-2.0 μg/kg

0.5-5.0 μg/kg


42

В

(В2с) Carbamates and Pyrethroids

4150

Carbamates: Thiram (tetramethylthiuram disulfide (TMTD), thigam, thigam C, ophtanol T, raksyl + TMTD, vitavax 200, vitavax 200 FF, vitathiuram, phenoram, chemicar Т, orlok Sevin (carbaryl) Polycarbacyn


HPTLC, Colorimetry

HPLC

GC GC-MS

1.0-100.0 μg/kg

0.1 –1.0 μg/kg

0.1 –1.0 μg/kg


43

Pyrethroids: Alphamethrin Deltamethrin Permethrin Sumicydin (fenvalerate) Cypermethrin (fyury)

GC, HPLC

GC

HPLC GC-MS

HPLC-MS-MS

1.0-100.0 μg/kg 0.5 –5.0 μg/kg

0.5 –5.0 μg/kg

ADD-0.005 mg/kg

ADD-0.003

mg/kg ADD – 0.035

mg/kg

AL – 0.0015 mg/kg

0.0015 mg/kg

44

В2 В2f Other pharmacologically active substances (including В2b+B2d+B2e)

3340 According to the registration

HPLC-MS HPLC-MS SanPin 2.3.2.2804-10, CU CR, Decision No. 299.

45

В3

(В3a) Organochlo-rine compounds, including PCB (dioxins)

125

125

125

125

Aldrin Heptachlor

Hexachlorocyclohexane (α-,β-, γ- isomers) DDT and its metabolites

Biomaterials from cattle, etc

GC GC-MS

- \\ -

- \\ -

- \\ -

GC-MS

0.1- 1.0 μg/kg

- \\ -

- \\ -

- \\ -

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

Non-admissible

Non-admissible

meat: 0.1 mg/kg

fat and others: 0.2 mg/kg meat: 0.1 mg/kg

fat and others: 1.0 mg/kg

46

B3

(В3a) Organochlorine compounds, including PCB (dioxins)

125

130

PCB (polychlorinated biphenyls)


GC-ECD

GC-MS

1.0 μg/kg (for PCB-105)

10.0-15.0 (for total isomers)

0.0005 -1.0 μg/kg

CU CR, Decision No. 299.

Polychlorinated dibenzo-p-dioxins and Dibenzofurans


GC-MS

GC-HRMS

0.01 ng/kg TEQ WHO

(В3b) Organophos-phorous compounds

251

251

Trichlormetafos-3

Heterophos

Diazinon (bazudin)

Dimethyl-dichlor-

phosphate


GC (NP)

enzymatic method (all

OPC, including activation)

- // -

- // -

- // -

GC (NP)

GC-MS

- // -

- // -

- // -

0.1- 50 μg in a sample

(0.001-100 μg in 0.1 ml of a sample), low

detection level 0.0001-

0.001 μg

0.0005 -1.0 μg/kg

- // -

- // -

- // -

SanPin 2.3.2.2804-10, CU CR, Decision No. 299.

47


251

(dichlorvos) Dursban (chlorpyrifos) Karbofos (malathion) Metaphos (parathion-methyl,wofatox) Phosalone (phosalone) Phthalophos Antio Phosphamide Aktellik


GC

(NP), enzymatic method (all

OPC, including

activation) - // -

- // -

- // -

- // -

- // -

- // -

- // -

Per group

GC (NP)

GC-MS

(0.5-3.0 μg in

a sample)

(0.5-3.0 μg in a sample)

See above

- // -

- // -

- // -

- // - (10.0 μg/kg)

0.0005 -1.0 μg/kg

- // -

- // -

- // -

- // -

- // -

- // -

- // -

SanPin 2.3.2.2804

-10, CU CR,

Decision No. 299.

48

B3

(В3b) Organophosphorous compounds

Temephos (abate) Chlorophos Cyodrin (crotoxiphos) Dibrom Coumaphos (coral)


- // - GC

(ND) enzymatic method (all

OPC, including

activation) - // - - // -

- // -

Per group

GC (NP)

GC-MS

- // -


(0.001-100 μg in 0.1 ml of a sample), low

detection level 0.0001-

0.001 μg

- // -

Per group

0.0005 -1.0 μg/kg

SanPin 2.3.2.2804-10, CU CR, Decision No. 299.

49

Fat - 0.1 mg/kg

Arsenic

2.5 μg/kg - \\ - - \\ - meat, fat - 0.1 mg/kg offal -1.0

mg/kg Cadmium

20.0 μg/kg

- \\ - - \\ - meat -0.05 mg/kg

offal – 0.3 mg/kg

kidneys -1.0 mg/kg

Mercury Screening

Colorimetry flameless.

AAS

2.5 μg/kg

twice a year 5% of establishments (one sample)

meat, fat -0.03

mg/kg

offal – 0.1 mg/kg kidneys -0.2 mg/kg

50

В3

(B3d) Mycotoxins

50 Ochratoxin А Zearalenon


HPTLC, ELISA

HPLC GC GC-МS HPLC-MS-МS

2 μg/kg 0.25 μg

- // -

0.1 – 0.5 μg/kg

- // -

Non-admissible

- // -

(В3f) Other substances including unpatented drugs

240

240

50

50

20

50

Free choice

Nitrates

Nitrites

Organomercury

compounds

2.4-D acid, salts and ethers

DNOC (dinitroorthocresol)

Atrazine

Captan

Biomaterials from

cattle, etc.

Color.

Color.

HPTLC,

GC

HPTLC, GC

- \ \ -

- \ \ -

- \ \ -

GC-MS

GC GC-MS

0.4 mg/kg

0.2 mg/kg

1. 0 μg/kg

1. 0 μg/kg

1. 0 μg/kg

1. 0 μg/kg

MAL meat-50 mg/kg

MAL meat – 3 mg/kg

SanPin

2.3.2.2804-10, CU CR,

Decision No. 299.

51

В3


10

10

20

10

20

20

10

(Free choice)

for pesticides

and rodenticid

es

Baygon (propoksur)

Fenthion (lebythid)

Nitraphen

CTAC (chlorcholine

chloride)

Aversectin С

Formaldehyde

Rodenticides: Zoocoumarine

Glyfluor

Krysid

Intandione derivatives

Biomaterials for

cattle, etc.

- \ \ -

- \ \ -

- \ \ -

HPTLC

HPLC TLC, GC,

HPLC, HPTLC

HPTLC,

GC

- \ \ -

- \ \ -

- \ \ - HPTLC,

GC, GC-MS, HPLC-MS-MS - \ \ -

- \ \ -

- \ \ -

- \ \ -

- \ \ -

- \ \ -

- \ \ -

- \ \ -

- \ \ -

0.00071 μg

3.0 μg/kg

(2 μg/kg in a sample)

-

10 μg

0.3 μg/kg

- \\ -

SanPin

2.3.2.2804-10, CU CR,

Decision No. 299.

Non-admissible

Non-admissible

- \\ -

- \\ -

- \\ -

52

В3


.

(ethylphenacine, etc.)

Radionuclides:

Cesium-137, Strontium –90

Microbiological criteria Criteria of parasite

freedom

Biomaterials from

cattle, etc.


HPLC Spectrometry, radiometry

CU CR Decision No. 299

- \ \ -

Spectrometry, radiometry with radiochemistry


CU CR Decision No. 299 CU CR Decision No. 299

53

В3


in case of suspicion in their

use

Unpatented drugs


ELISA GC, HPLC

GC-MS

HPLC-MS-MS

54

В3

(В3c) Chemical elements

1810

1810

1810

Plumbum

Arsenium

Cadmium

Biomaterials: plasma and serum, hair.

IVA. AAS

AAS AAS-ETA ICP-MS

50 μg/kg

0.01-1.0 μg/kg

CU Common

requirements. Decision

No. 299

IVA. AAS

AAS AAS-ETA ICP-MS

2. 5 μg/kg 0.01-1.0 μg/kg

CU Common


No. 299

ААS AAS AAS-ETA ICP-MS ICP-MS

20 μg/kg

0.01-1.0 μg/kg

CU Common


No. 299

55

B3


1810

Mercury

Biomaterials: plasma and serum, hair

Color. Plasmaless ААS

ААS – MHG ААS-ETA

2.5 μg/kg

0.01-1.0 μg/kg

CU Common


No. 299

500

20

500

Fluor Ionometry. chem.

Ionometry. chem

3.0 μg 3.0 μg Biochem. norm.

Selenium AAS AAS-ETA

ICP-MS

AAS AAS-ETA ICP-MS

10 μg/kg 10 μg/kg

Natrium 1.0 μg/kg 1.0 μg/kg

Calium 1.0 μg/kg 1.0 μg/kg

Magnesium 1.0 μg/kg 1.0 μg/kg

Manganese 1.0 μg/kg 1.0 μg/kg

56

В3 (В3c) Chemical elements

500

Cobalt Biomaterials: plasma and serum, hair

AAS AAS-ETA

ICP-MS

AAS AAS-ETA ICP-MS

0.1 μg/kg 0.1 μg/kg Biochem.norm.

Nickel 0.1 μg/kg 0.1 μg/kg

Cuprum 0.1 μg/kg 0.1 μg/kg

Zinc 1.0 μg/kg 1.0 μg/kg

Total of 63414 samples of biological materials from cattle and others ( feed, water) were subjected to chemical investigations

57

Table 6 List of control parameters for the state veterinary monitoring of residues of drug preparations, banned and toxic substances for veterinary

laboratories in the Russian Federation, 2013 (small ruminants)

Groups of substances according to 96/23/ЕС of April 29, 1996

Number of

samples

Name of the preparation (active

substance), metabolites

Type of product (object of the

investigation)

Screening methods

Confirma-tion

methods

Detection limit of the screening method

Detection limit of the

of the confirma-

tion method

Admissible levels of

substances (standards)

А

А1) Stilbenes (А2) Thyreo-statics (А3) Synthetic steroids, (А3) Natural steroids

381

381

281

100

Diethylstilbestrol Hexestrol Dienestrol Thiouracil Methylthiouracil, etc. 19-Nortestosterone Trenbolone Methyltestoterone Acetylgestagen, including Medroxyprogesteron acetate Melengestrol acetate Ethinylestradiol Trenbolone acetate Testosterone Progesterone

Biomaterials from small rumi-nants, etc.

ELISA GC-MS

ELISA GC-MS

ELISA GC-MS

ELISA

GC-MS

HPLC-MS-MS

GC-MS HPLC-MS-MS

0.25-2.8

μg/kg

0.1-0.5

μg/kg

0.25-2.8 μg/kg

0.1-0.5

μg/kg

0.1 –0.5 μg/kg

- // -

- // -

Non-admissible Non-admissible Non-admissible Biochemical natural levels

58

А

(А4) Resorcylic acid lactones (А5) Beta-agonists

See above

381

Oestradiol -17 Zeranol Clenbuterol, Salbutamol, Terbutaline, Mapenterol, Cymbuterol, etc.


ELISA GC-MC

- // -

- // -

- // -

0.25 μg/kg

0.5 μg/kg

0.05 μg/kg

0.25-2.8 ng/g

0.25-2.8 μg/kg

0.1-0.5

μg/kg

0.25-2.8

μg/kg

0.1-0.5

μg/kg

- // -

- // -


59

(А6) Substances included in the Annex IV of Council Regulation No. 2377/90 (EEC) of June 26, 1990

381

Chloramphenicol Nitrofurans and metabolites: AOZ, SEM, AHD, AMOZ Derivatives of Nitroimidazole, Dimetridazole, Metronidazole, Ronidazole, etc.


ELISA, HPLC-MS-

MS

ELISA HPLC-MS-

MS

HPLC-MS-MS

0.25

μg/kg

0.1 μg/kg

0.2 μg/kg

0.25-1.0 μg/kg

0.25-1.0 μg/kg

GC-MS

HPLC-MS-MS

HPLC-MS-MS

HPLC-MS-MS

0.1-0.3 μg/kg

0.25-1.0 μg/kg

0.25-1.0 μg/kg


60

В (В1) Antibacterial substances including sulfanilamides and quinolones

3657

Tetracycline (Oxytetracyclin Metacyclin Doxycyclin) Bacitracin Grisein Others


HPLC Microbiolo-gical ELISA HPLC-MS-MS

HPLC-MS-MS

0.1-0.2 μg/kg

0.01 units/g 6-60 μg/kg 0.5-0.01 units/g 0.5-5.0 μg/kg

0.5-5.0 μg/kg

Non-admissible

Sulphonamides (sulfamethazine, sulfadimethoxine, sulfadiazine, etc. (not less than 8 compounds)

ELISA (imp.)

HPLC-MS-MS

HPLC-MS-MS

20 μg/kg 1.0-10.0

μg/kg

1.0 –10.0 μg/kg

SanPiN 2.3.2.2804-

10 CU

Common Require-ments,

Decision No.299

Fluoroquinolones (enrofloxacin, ciprofloxacin, etc.)

ELISA (imp.)

HPLC-MS-MS

HPLC-MS-MS

10 μg/kg 0.1-10.0

μg/kg

0.1 –10.0 μg/kg

SanPiN 2.3.2.2804-

10 CU


Decision No.299

61

В

(В2a) Anthelmin-tics

2285

Blue vitriol (Copper sulphate)


(for copper) Colorime-

tric AAS

AAS, AAS-ETA

0.25 – 0.4 mg/kg

SanPiN 2.3.2.2804-

10 CU


Decision No.299

62

В


2285

Avermectins (ivermectin, doramectin, abamectin, moxidectin, emamectin)

Other anthelmintics (benzimidazole

derivatives) Others

HPLC

HPLC-MS

HPLC-MS-MS

HPLC-MS

1.0-2.0 μg/kg

0.5-5.0 μg/kg

SanPiN

2.3.2.2804-10

CU Common Require-ments, Decision No.299

Carbamates: Thiram (tetramethylthiuram disulfide (TMTD), thigam, thigam C, ophtanol T, raksyl + TMTD, vitavax 200, vitavax 200 FF, vitathiuram, phenoram, chemicar Т, orlok Sevin (carbaryl) Polycarbacyn


HPTLC, colorimetric

HPLC-MS/MS

GC-MS HPLC-MS/MS

1.0-100.0 μg/kg

0.1-1.0 μg/kg

0.1 –1.0 μg/kg

Non-admissible

Non-admissible

0.02 mg/kg

63

Pyrethroids: Alphamethrin Deltamethrin Permethrin Sumicydin (fenvalerate) Cypermethrin (fyury)

HPTLC,

GC, HPLC, HPLC-MS-

MS

GC,

HPLC GC-MS HPLC-MS-MS

1.0 μg/kg 0.5-5.0 μg/kg

0.5 –5.0 μg/kg

SanPiN 2.3.2.2804-

10 CU Common Require-ments, Decision No.299

64




HPLC-MS

HPLC-MS SanPiN 2.3.2.2804-

10 CU


Decision No.299

65

В3

(В3a) Organo-chlorine

compounds, including

PCB (dioxins)

20

20

40

40

Aldrin Heptachlor



GC GC-MS

- \\ -

- \\ -

- \\ -

GC-MS

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

Non-admissible

Non-admissible

Meat - 0.1 mg/kg

Fat, etc . -0.2 mg/kg Meat - 0.1

mg/kg

Fat, etc .- 1.0 mg/kg

66

В3

(В3a) Organochlo-

rine compounds,

including PCB (dioxins)

55

55



GC-ECD

GC-MS

1.0 μg/kg (for

PCB-105) 10.0-15.0 (for

a sum of isomers)

0.0005-1.0

μg/kg

CU Common Requirem

ents, Decision No.299

Polychlorinated dibenzo-p-dioxins and dibenzofurans


GC-HRMS

GC-HRMS

0.01 ng/kg TEQ WHO


76

Trichlormetafos-3

Heterophos


GC (NP)

enzymatic method (all

OPC including activated

GC

(NP)

GC-MS

- // -


(0.001-100 μg in 0.1 ml of a

0.0005-1.0 μg/kg

- // -

CU Common Requirem


67

В3


76

Diazinon (bazudin)

Dimethyl-dichlor-phosphate

(dichlorvos) Dursban (chlorpyrifos) Karbofos (malathion) Metaphos (parathion-methyl, wofatox) Phosalone (phosalone) Phthalophos Antio


ones) - // -

- // -

- // -

GC

(NP) enzymatic method (all

OPC, including activated

ones) - // -

- // -

- // -

- // -

- // -

- // -

- // -

- // -

For group

GC (NP)

GC-MS

sample), lower

detection limit 0.0001-0.001

μg



See above

- // -

- // -

- // -

- // -

- // -

0.0005 -1,0 μg/kg

- // -

- // -

- // -

- // -

- // -

Common

CU Requirem


68

Phosphamide Aktellik Temephos (abate)

- // -

- // -

- // -

- // -

(10.0 μg/kg)

- // -

- // -

- // -

- // -

- // -

69

Fat - 0.1 mg/kg

Arsenic

2.5 μg/kg - \\ - - \\ - Meat, fat -0.1 mg/kg Offal -1.0 mg/kg -

Cadmium

20.0 μg/kg

- \\ - - \\ - Meat -0.05

mg/kg Offal –

0.3 mg/kg Kidneys -1.0 mg/kg

Mercury Screening

Colorimetry Flameless

AAS

2.5 μg/kg

twice a year 5% of establishments (one sample

per establishm

ent)

Meat, fat – 0.03 mg/kg

Offal – 0.1 mg/kg Kidneys -0.2 mg/kg

70

В3

(B3d) Mycotoxins

10

10

Ochratoxin А Zearalenon

Biomateri-als from small rumi-nants, etc.

HPTLC, ELISA

HPLC GC GC-MS HPLC-MS-MS

2 μg/kg 0.25 μg

- // -

0.1 – 0.5 μg/kg

- // -

Non-admissible

- // -


(В3f) Other

30

30

30

30 5 5

Free choice

50

Nitrates Nitrites Organomercury compounds 2.4-D acid, its salts and ethers DNOC (dinithroorthcresol) Atrazine Captan Baygon (propoksur)

Biomateri-als from small rumi-nants, etc. Biomateri-als from small rumi-

Colorimet-

ry Colorimet-

ry GC

GC-MS

GC GC-MS

- \ \ -

- \ \ - - \ \ -

- \ \ -

GC GC-MS

GC GC-MS

0.4 mg/kg

0.2 mg/kg

1.0 μg/kg

1.0 μg/kg

1.0 μg/kg

1.0 μg/kg

MAL for meat-50 mg/kg

MAL for meat – 3 mg/kg

CU Common Requirements

Decision No.299

CU Common Requirements

Decision

71

В3

substances including unpatented drugs

100

(Free choice)

for pesticides

and rodenticid

es

Fenthion (lebycid) Nitraphen CCC (chlorcholine chloride) Aversectin С Formaldehyde Rodenticides: Zoocoumarine Glyfluor Krysid Intandione derivatives (ethylphenacine, etc.)

nants, etc.

- \ \ -

- \ \ -

HPTLC

HPLC TLC, GC,

HPLC HPTLC

GC

- \ \ -

- \ \ -

- \ \ - HPTLC, HPLC

Spectro-

GC, GC-MS, HPLC-MS-MS

- \ \ -

- \ \ -

- \ \ -

GC/MS - \ \ -

- \ \ -

- \ \ - - \ \ - - \ \ -

Spectro-

0,00071 μg in

a sample

3 μg/kg

2 μg in a sample

- 10 μg 0.3 mg/kg

- \\ -

No.299

Non-admissible

- \\ -

- \\ -

- \\ -

72

В3


Radionuclides: Cesium-137,

Strontium –90 Microbiological criteria Criteria of freedom from parasites

Bio-materials from ruminants, etc.

Bio-materials from ruminants, etc.

metry, radio-metry

CU Common Require-ments,

Decision No.299

metry, radio-metry with radiochemistry Common

CU Require-ments,

Decision No.299

CU Common

Requirements Decision No.299

73

В3


In case of suspicion in their

use

Unpatented substances

Biomaterials from small ruminants, etc.

ELISA GC HPLC

GC-MS HPLC-MS-MS

Non-admissible

٭

74

В3


900

900

50

Plumbum

Аrsenic

Cadmium

Biomaterials, plasma and serum., hair

IVA AAS

AAS AAS-ETA ICP-MS

50 μg/kg

0.01-1.0 μg/kg

Meat – 0.5 mg/kg

Offal – 0.6 mg/kg Kidneys- 1.0 mg/kg Fat - 0.1 mg/kg

IVA AAS

AAS AAS-ETA ICP-MS

2. 5 μg/kg

0.01-1.0 μg/kg Meat and fat -0.1 mg/kg

Offal – 1.0 mg/kg -


20 μg/kg

0.01-1.0 μg/kg Meat - 0.05 mg/kg ;

Fat - 0.03 mg/kg ; Offal –

0.3 mg/kg ;

Kidneys – 1.0 mg/kg

75

B3


900

Mercury

Biomaterials, plasma and serum, hair

Colorimetry Flameless ААS

ААS – MHG ААS-ETA ICP-MS

2.5 μg/kg

0.01-1.0 μg/kg Meat and fat - 0.03 mg/kg; Offal – 0.1 mg/kg; Kidneys - 0.2 mg/kg

20 5

Fluorine Ionometry. chem.

Ionometry. chem.. ICP-MS


Selenium AAS AAS-ETA ICP-MS

AAS AAS-ETA ICP-MS

10 μg/kg 10 μg/kg

200

Sodium 1.0 μg/kg 1.0 μg/kg

Potassium 1.0 μg/kg 1.0 μg/kg



76


200

Cobalt Biomaterials, plasma and serum., hair

AAS AAS-ETA ICP-MS

AAS AAS-ETA ICP-MS





* Total of 14813 samples of biological materials from small ruminants and others (feeds, water) were subjected to chemical investigation.

77

Table 7 List of control parameters for the state veterinary monitoring of residues of drug preparations, banned and toxic substances for veterinary

laboratories in the Russian Federation, 2013 (pigs)*

Groups of substances

according to 96/23/ЕС April 29,

1996

No. of samples



Type of product (object of the

investigation

Screening methods

Confirma-tion

methods

Detection limit of the screening method μg/kg

Detection limit of the confirma-

tion method μg/kg

Admissib-le levels of substances

(norms)

А

(А1) Stilbenes (А2) Thyreo-statics (А3) Synthetic steroids (А3) Natural

540

540

540

Diethylstilbestrol Hexestrol Dienestrol Thiouracil Methyluracil, etc. 19-Nortestosterone Trenbolone Methyltestoterone Acetylgestagen, including Medroxyprogesteron Melengestrol acetate Ethinylestradiol Trenbolone acetate

Biomaterials, etc.

ELISA GC-MS

ELISA GC-MS

ELISA GC-MS

ELISA

GC-MS

HPLC-MS-MS

GC-MS HPLC-MS-MS

0.25-2.8 μg/kg

0.1-0.5 μg/kg

0.25-2.8 μg/kg

0.1 –0.5 μg/kg

- // -

Non-admissible Non-admissible Non-admissible Biochemical norm of

78

А

steroids (А4) Resorcylic acid lactones (А5) Beta-agonists

540 See above 540

Testosterone, Progesterone, Oestradiol -17 Zeranol Clenbuterol Salbutamol Terbutaline, Mapenterol Cimbuterol, etc.

Biomaterials, etc.

ELISA GC-MS

- // -

- // -

- // -

0.1-0.5 μg/kg

0.25 μg/kg

0.5 μg/kg

0.05 μg/kg

0.25-2.8 ng/g

0.25-2.8 μg/kg

0.1-0.5 μg/kg

0.25-2.8

μg/kg 0.1-0.5 μg/kg

- // -

- // -

- // -

natural level

Non-admissible

Non-admissible

80

(А6) Substances included into Table 2 of Annex 37/10 (EC)

540

540

540

Chloramphenicol Nitrofurans and metabolites: AOZ, SEM, AHD, AMOZ Nitroimidazole derivatives Dymetridazole Metronidazole Ronidazole, etc.

Biomaterials, etc.

ELISA, HPLC-MS-

MS

ELISA HPLC-MS-

MS

HPLC-MS-MS

0.25 μg/kg

0.1 μg/kg

0.2 μg/kg 0.25-1.0

μg/kg

0.25-1.0 μg/kg

GC-MS HPLC-MS-

MS (HPLC)

HPLC-MS-MS

HPLC-MS-MS

0.1-0.2 μg/kg

0.25-1.0 μg/kg

0.25-1.0 μg/kg


81

В (В1) Antibacterialdrugs including sulfanilamides and quinolones

2,430

Tetracycline (Oxytetracyclin Metacycline Doxycyclin) Bacitracin Grisein Others

Biomaterials, etc.

HPTLC Microbiolo-gical ELISA HPLC-MS-MS

HPLC HPLC-MS-MS

0.1-0.2 μg/kg

0.01 units/g 6-60 μg/kg

0.5-0.01 units/g

0.5-5.0 μg/kg

0.5-5.0 μg/kg

Non-admissible

Sulphonilamides (sulfamethazine, sulfadimethoxine, sulfadiazine, etc.) (not less than 8 compounds)

ELISA (import) MS-MS HPLC

HPLC-MS-MS

20 μg/kg 1.0-10.0

μg/kg

1.0 –10.0 μg/kg

SanPiN 2.3.2.2804-

10, CU Common

reqirements Decision No.299

Fluoroquinolones (enrofloxacin, ciprofloxacin, etc.)

ELISA (import)

HPLC-MS-MS

HPLC-MS-MS

10 μg/kg 0.1-10.0

μg/kg

0.1 –10.0 μg/kg

SanPiN 2.3.2.2804-

10, CU Common


82

В

(В2a) Anthelmin-tics

1,940

500

Avermectin (ivermectin,

doramectin, abamectin, moxidectin, emamectin)

Other anthelmintics (benzimidazole

derivatives)

Biomaterials, etc.

HPLC-MS-MS

HPLC-MS-MS

1.0-2.0 μg/kg

0.5-5.0 μg/kg

SanPiN 2.3.2.2804-10, CU Common reqirements

Decision No.299

Carbamates: Thiram (tetramethylthiuram disulfide(TMTD), thigam, thigam C, ophtanol T, raksyl + TMTD, vitavax 200, vitavax 200 FF, vitathiuram, phenoram, chemicar Т, orlok Sevin (carbaryl) Polycarbacyn

Biomaterials, etc.

HPTLC, Colorimetry

GC

GC-MS

1.0-100.0

μg/kg

0.1 –1.0 μg/kg

CU Common reqirements

Decision No.299

83

В


400

Pyrethroids: Alphamethrin Deltamethrin Permethrin Sumicydin (phenvalerat) Cypermethrin (fury)

Biomaterials, etc.

GC, HPLC

GC


1.0 μg/kg

0.5 –5.0 μg/kg

ADD-0.005 mg/kg ADD-0.003 mg/kg ADD – 0.035 mg/kg AL – 0.0015 mg/kg AL -0,0015 mg/kg

84



Biological materials, etc.

HPLC-MS

HPLC-MS SanPiN 2.3.2.2804-10, CU Common reqirements

Decision No.299

85

В3

(В3a) Organochlorine compounds,

including PCB (dioxins)

500

500

500

500

Aldrin Heptachlor



GC GC-MS

- \\ -

- \\ -

- \\ -

GC-MS

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

Non-admissible

Non-admissible

Meat - 0.1 mg/kg

Fat, etc. - 0.2 mg/kg

Meat - 0.1 mg/kg

Fat, etc. -1.0 mg/kg

86

В3


100

20



GC-ECD GC-MS

GC-MS

1.0 μg/kg (for

PCB-105) 10.0-15.0 (for

a sum of isomers)

0.0005 -1.0 μg/kg


Decision No.299 With

annexes



GC-HRMS

GC-HRMS

0.01 ng/kg TEQ WHO

(В3b) Organophosphorous compounds (OPCs)

200

Trichlormetaphos-3

Heterophos

Diazinon (bazudin)

Dichlorvinyl-dimethyl phosphate


GC (NP)

Enzymatic method (all

OPCs including

activated ones) - // -

- // -

GC

(NP)

GC-MS

- // -

- // -


(0.001-100 μg in 0.1 ml of a

sample), lower

detection limit: 0.0001-

0.001 μg

0.0005 -1.0 μg/kg

- // -

- // -


Decision No.299

with annexes

87

В3


200

(dichlorphos) Dursban (chlorpyrifos) Karbofos (malathion) Metaphos (parathion-methyl,wofatox) Phosalone (phosalone) Phthalophos Antio Phosphamide Aktellik


- // -

GC (NP)


OPCs including


- // -

- // -

- // -

- // -

- // -

- // -

- // -

Per a group

GC (NP)

GC-MS



See above

- // -

- // -

- // -

- // -

(10.0 μg/kg)

- // -

0.0005 -1.0 μg/kg

- // -

- // -

- // -

- // -

- // -

- // -

- // -

CU Common reqiremnets

Decision No.299

88

B3


200

Temephos (abate) Chlorophos Cyodrin (crotoxiphos) Dibrom Coumaphos (coral)


- // -

GC (NP)


OPCs including

activated ones)

- // - - // -

- // -

Per a group

GC (NP)

GC-MS

- // -

0.1- 50 μg in a

sample (0.001-100 μg in 0,1 ml of a sample, lower


0.001 μg)

- // -

Per a group

0.0005- 1.0 μg/kg


Decision No.299

89

Fat - 0.1 mg/kg

Arsenic

2.5 μg/kg - \\ - - \\ - Meat, fat -0.1 mg/kg Offal -1.0

mg/kg Cadmium

20.0 μg/kg

- \\ - - \\ - Meat -0.05 mg/kg

Offal – 0.3 mg/kg

Kidneys -1.0 mg/kg

Mercury Screening

Colorimetry Flameless

AAS

2.5 μg/kg

twice a year 5% of establishments (one sample)

Meat, fat -0.03 mg/kg

Offal – 0.1 mg/kg Kidneys -0.2 mg/kg

В3

(B3d) Mycotoxins

50 Ochratoxin А Zearalenon

Biological materials from pigs, etc.

HPTLC, ELISA


2 μg/kg 0.25 μg

- // -

0.1 – 0.5 μg/kg

- // -

Non-admissible - // -

(В3f) Other

500

Nitrates

Porcine biological

Colorimetry

0.4 mg/kg


Decision

90

В3


(В3f) Other substances including

500

50

50

20

50

(Free choice)

for pesticides

and rodenticid

es

Nitrites Organomercury compounds 2,4-D acid, its salts and esters Formaldehyde Rodenticides: Zoocoumarine Glyfluor Krysid Intandione derivatives (ethylphenacine, etc.)

materials, etc. Porcine biological

Colorimetry

GC GC-MS

HPTLC,

GC

GC

HPTLC

- \ \ -

- \ \ -

- \ \ - Spectro- metry, radiometry

GC GC-MS

GC

GC-MS

GC-MS

GC, GC-MS, HPLC-MS-MS

Spectro-

0.2 mg/kg

1.0 μg/kg

1.0 μg/kg

3 μg/kg

0.3 mg/kg

1.0 μg/kg

1.0 μg/kg

No.299

Non-admissible

- \\ -

- \\ -


91

unpatented drugs (В3f) Other

100

Radionuclides:

Cesium – 137, Strontium –90

Microbiological criteria

Criteria of parasite freedom

Unpatented drugs in

case their use is

materials, etc. Porcine biological materials,


Decision No.299

GC-MS HPLC- MS-

MS

metry, radio-metry with radiochemistry

CU Common


GC-MS HPLC- MS-

MS

- \\ -

Decision No.299

92

В3


suspected

etc.

93

В3


500

500

Plumbum

Arsenium

Biomaterials. plasma and serum. hair

IVA, AAS

AAS AAS-ETA ICP-MS

50 μg/kg

0.01-1.0 μg/kg

0.5 μg/kg – meat

0.6 μg/kg – offals 1.0 μg/kg – kidney 0.1 μg/kg - fat

IVA, AAS

AAS AAS-ETA ICP-MS

2.5 μg/kg 0.01-1.0 μg/kg

0.01 – 1.0 μg/kg – meat

and fat 1.0 μg/kg -

offals

94

500

Cadmium


20 μg/kg

0.01-1.0 μg/kg

0.05 mg/kg – meat;

0.03 mg/kg – fat;

0.3 mg/kg – offals;

1.0 mg/kg -

kidneys

B3


500

Mercury


Color. Flameless ААS


2.5 μg/kg

0.01-1.0 μg/kg

0.03 μg/kg – meat and fat; 0.1 μg/kg – offals; 0.2 μg/kg - kidneys

20

50


Ionometry. chem.. ICP-MS

3.0 mg 3.0 mg Biochem. norm.


AAS AAS-ETA ICP-MS

10 μg/kg 10 μg/kg


95

100 Calium 1.0 μg/kg 1.0 μg/kg



В3 (В3c)Химичес-кие элементы

100

Cobalt Biomaterials, plasma and serum, hair

AAS, AAS-ETA, ICP-MS


0.1 μg/kg 0.1 μg/kg Biochem. norm.

* Total of 16400 samples of biological materials from pigs and others (feeds, water) were subjected to chemical investigation.

96

Table 8 List of control parameters for the state veterinary monitoring of drug preparation, banned and toxic substance residues for veterinary

laboratories of the Russian Federation in 2013 (poultry)



29 April 1996

Number of

samples


metabolites


of examina

tion)

Screening methods

Confirma- tion

methods

Detection limits for the

screening method

Detection limits for the confirmation

method

Admissible levels

(standards)

А

А1) Stilbenes (А3) Synthetic steroids (А3) Natural steroids

2,800

2,800

2,800 See

Diethylstilbestrol, Hexestrol, Dienestrol 19-Nortestosterone, Trenbolone, Methyltestosterone, Acetylgestagen, including medroxyprogesteron acetate, Melengestrol acetate Ethinylestradiol Trenbolone acetate Testosterone, Progesterone, Oestradiol -17

Biological materials and others

ELISA GC-MS

ELISA GC-MS

ELISA

GC-MS

GC-MS

- // -

0.25-2.8

μg/kg

0.1 –0.5 μg/kg

0.25-2.8 μg/kg

0.1-0.5 μg/kg

0.1 –0.5 μg/kg

- // -

- // -

Non-admissible Non-admissible Biochemical natural levels

97

А


above

2,800



ELISA GC-MS

- // -

- // -

0.25 μg/kg

0.5 μg/kg

0.05 μg/kg

0.25-2.8 ng/g

0.25-2.8 μg/kg

0.1-0.5 μg/kg

0.25-2.8 μg/kg

0.1-0.5 μg/kg

- // -

- // -


98

(А6) Substances included in Table 2 of the Annex 37/10 (EC)

2,800

Chloramphenicol Nitrofurans and metabolites: AOZ, SEM, AHD AMOZ Nitroimidazole derivatives (dimetridazole, metronidazole, ronidazole etc.)


ELISA,

ELISA HPLC- MS-MS

HPLC- MS-MS

GC-MS HPLC-MS-MS (HPLC)

HPLC-MS-MS

HPLC-MS-MS

0.25 μg/kg

0.1 μg/kg

0.2 μg/kg 0.25-1.0

μg/kg

0.25- 1.0 μg/kg

0.1-0.3 μg/kg

0.25 –1.0

μg/kg

0.25 - 1.0 μg/kg



2,000

Tetracyclines (Oxytetracyclin, Methacyclin, Doxycyclin), Bacitracin, Grisein others


HPLC Microbiological method ELISA HPLC-

MS-MS

HPLC-MS-MS

0.1-0.2 μg/kg

0.01 U/g 6.0 μg/kg 0.5-0.01 U/g 1.0 μg/kg

0.5 - 5.0 μg/kg

Non-admissible

99

Sulphonamides (sulfamethazine, sulfadimethoxine, sulfadiazine etc. (at lest 8 compounds)

ELISA (imported)

HPLC MS-MS

HPLC

MS-MS-

20 μg/kg 1.0-10.0

μg/kg

1.0 –10.0 μg/kg


Fluoroquinolones (enrofloxacin, ciprofloxacin etc.)

ELISA (imp.) HPLC- MS-MS

HPLC-MS-MS

10 μg/kg 0.1-10.0

μg/kg

1.0 –10.0 μg/kg


100

(В2a) Anthelmintics

500

200

According to the registration (free choice)


HPLC-MS-MS

HPLC-MS-MS

SanPiN 2.3.2.2804 -10, CU CR Decision No. 299

Carbamates: Thiram (tetramethylthiuram disulfide (TMTD), thigam, thigam C, ophtanol T, raksyl+TMTD,vitavax 200, vitavax 200 FF, vitathiuram, phenoram, chemicar Т, orlok Sevin (carbaryl) Polycarbacin


HPTLC, colorimetric

method GC

GC GC-MS

1.0-100.0 μg/kg

0.1-1.0 μg/kg

0.1 –1.0 μg/kg


101

В

(В2с) Carbamates and pyrethroids

500

Pyrethroids: Alphamethrin Deltamethrin Permethrin Sumicydin (fenvalerate) Cypermethrin (fury)


HPTLC,

GC, HPLC, HPLC-MS-

MS

GC


1.0-100.0 μg/kg

0.5-5.0 μg/kg

0.5 –5.0 μg/kg

ADD -0.005 mg/kg ADD -0.003 mg/kg ADD – 0.035 mg/kg AL – 0.0015 mg/kg 0.0015 mg/kg

102

В2 В2f Other pharmacologically active substances (including В2b+B2d+B2e), coccidiostats

1,000 According to the registration


HPLC-MS

HPLC-MS SanPiN 2.3.2.2804 -10, CU CR Decision No. 299

103

В3


10

10

2,000

2,000

Aldrin Heptachlor


Biological materials and others .

GC GC-MS

- \\ -

- \\ -

- \\ -

GC-MS

0.5-10 μg/kg 0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

Non-admissible

Non-admissible

0.1 mg/kg meat 0.2 mg/kg fat and others 0.1 mg/kg meat 1.0 mg/kg fat and others

.

104

В3

(В3a) Organochlorine

compounds, including PCB

(dioxins)

100

20

PCB (polychlorina-ted biphenyls)


GC-ECD

GC-MS

1.0 μg/kg (for

PCB-105) 10.0-15.0 (for

sum of isomers)

0.0005-1.0

μg/kg


with annexes



GC-HRMS

GC-HRMS

0.01 ng/kg TEQ WHO

(В3b) Organo-phosphorous compounds

100

Trichlormeta-

phos-3

Heterophos Diazinon (bazudin)

Dichlorvinyl- dimethyl- -


GC (NP)


OPCs including activated

ones) - // - - // -

- // -

GC

(NP)

GC-MS - // -

- // -

- // -

0.1- 50 μg in

a sample (0.001-100 μg in 0.1 ml of a sample),

lower detection

limit: 0.0001-0.001 μg

0.0005 -1,0 μg/kg

- // -

- // -

CU CR Decision No. 299 with annexes

105

В3


100

phosphate (dichlorvos)

Dursban (chlorpyrifos) Karbofos (malathion) Metaphos (parathion-methyl, wofatox) Phosalone (phosalone) Phthalophos Antio Phosphamide Aktellik


GC (NP)



ones) - // -

- // -

- // -

- // -

- // -

- // -

- // -

- // -

Per group

GC (NP)

GC-MS


(0.5-3.0 μg in

a sample)

See above

- // -

- // -

- // -

- // -

(10.0 μg/kg)

- // -

0.0005 -1.0 μg/kg

- // -

- // -

- // -

- // -

- // -

- // -


106

B3


100

Temephos (abate) Chlorophos Cyodrin (crotoxiphos) Dibrom Coumaphos (coral) Others


GC (NP) Enzymatic method (all


ones) - // -

- // -

- // -

Per group

GC (NP)

GC-MS

- // -


(0.001-100 μg in 0,1 ml of a sample),

lower detection

limit: 0.0001-0.001 μg

- // -

Per group:

0.0005 -1.0 μg/kg


107

Arsenic

Cadmium

2.5 μg/kg

-\\-

-\\-

Fat – 0.1 mg/kg 0.1 mg/kg – meat, fat 1.0 mg/kg – offals

20.0 μg/kg

-\\- -\\- 0.05 mg/kg – meat 0.3 mg/kg – offal 1.0 mg/kg - kidney

108

Mercury

Screening

Colori-metric methd

Flameless AAS

2.5 μg/kg Twice a year

1 sample from 5% of

plants

0.03 mg/kg – meat, fat;

0.1 mg/kg -

offal;

0.2 mg/kg -kidneys

3

(B3d) Mycotoxins

100 Ochratoxin А T2-toxin


HPTLC, ELISA


2 μg/kg 0.25 μg

- // -

0.1 – 0.5 μg/kg

- // -

Non-admissible

- // -


50

50

25

25

50

Nitrates Nitrites Organomercury compounds 2,4-D acid, its salts and esters


Colorimetry

Colorimetry

HPTLC, GC HPTLC GC

GC-MS

0.4 mg/kg

0.2 mg/kg

0.01 μg/kg

1.0 μg/kg

3 μg/kg

MAL meat-50 mg/kg



109

В3


50 5

(Free choice) for

pesticides and

rodenticides

Formaldehyde Rodenticides: Zoocoumarine Zinc phosphide Glyfluor Krysid Intandione derivatives (ethylphenacine, etc.)

Radionuclides: Cesium – 137, Strontium –90


HPLC, GC HPTLC

- \\ -

- \\ - -\\- Spectro metry, radio metry

GC-MS GC, GC-MS HPLC-MS-MS

Spectro metry, radio metry with radio chemistry

10 μg

0.3 mg/kg

Non-admissible

- \\ -

- \\ -


110

В3


500

Microbiologic

al criteria Criteria of

freedom from parasites

Unpatented drugs in case of

suspicions in their use


CU CR Decision No. 299 with annexes GC-MS HPLC-MS-MS

CU CR Decision No. 299 with annexes GC-MS HPLC-MS-MS

- \\ -

CU CR Decision No. 299 with annexes Non-admissible

111

В3


1,000

1,000

Plumbum

Arsenium


IVA AAS

AAS AAS-ETA

ICP-MS

50 μg/kg

0.01-1.0 μg/kg

0.5 μg/kg – meat

0.6 μg/kg – offal 1.0 μg/kg – kidney 0.1 μg/kg - fat

IVA AAS

AAS AAS-ETA

ICP-MS

2.5 μg/kg 0.01-1.0 μg/kg 0.01 μg/kg –

meat and fat

1.0 μg/kg - offal

112

1,000

Cadmium ААS AAS AAS-ETA

ICP-MS

20 μg/kg

0.01-1.0 μg/kg 0.05 μg/kg – meat; 0.03

μg/kg – fat;

0.3 μg/kg – offal;

1.0 μg/kg - kidneys

B3


1,000

Mercury

Biomaterials. Plasma and serum.

Color. Flameless ААS

ААS – MHG ААS-ETA

2.5 μg/kg

0.01-1.0 μg/kg 0.03 μg/kg – meat and fat; 0.1 μg/kg – offal; 0.2 μg/kg - kidneys

20

50


Ionometry. chem..



AAS AAS-ETA ICP-MS

10 μg/kg 10 μg/kg

113

50






100

Cobalt Biomaterials. plasma and serum

AAS AAS-ETA ICP-MS

AAS AAS-ETA ICP-MS





* For chemical examination of biological materials from poultry and etc. (food, feed, water) – 27715 samples (the same samples from different groups

can be examined for several parameters (several groups).

114

Table 9 List of control parameters for the state veterinary monitoring of drug preparations, banned and toxic substance residues for veterinary

laboratories of the Russian Federation 2013 (horses, including antemortem control)



29 April 1996

Number of samples

Name of the drug (active substance),

metabolites


of examina

tion)

Screening methods

Confirmation

methods


screening method

Detection limits for

the confirmation method

Admissible levels

(standards)

А

А1) Stilbenes (А2) Thyrostatics (А3) Synthetic steroids (А3) Natural steroids

100

100 100

Diethylstilbestrol, Hexestrol, Dienestrol Thiouracil Methylthiouracil, etc. 19-Nortestosterone, Trenbolone, Methyltestorone, Acetylgestagen, including medroxyprogesterone acetate Melengestrol acetate Ethinylestradion Trenbolone acetate Testosterone, Progesterone,


GC-MS

HPLC-MS-MS

GC-MS HPLC-MS-

MS

GC-MS HPLC-MS-

MS

ELISA

GC-MS

HPLC-MS-MS

GC-MS

HPLC-MS-MS

- // -

0.1-0.5 μg/kg

0.1-0.5 μg/kg

- // -

0.1 –0.5 μg/kg

- // -

- // -


115

А

А4) Resorcylic acid lactones (А5) -agonists

See above 100

Oestradiol -17 Zeranol Clenbuterol Salbutamol Terbutaline Mapenterol Cymbuterol, etc.


GC-MS HPLC-MS-

MS

GC-MS

HPLC-MS-MS

- // -

- // -

0.25 μg/kg

0.5 μg/kg

0.05 μg/kg

0.1-0.5 μg/kg

0.1-0.5 μg/kg

- // -

- // -

- // -

0.015 mg/rg 0.015 mg/kg 0.0005mg/kg Non-admissible Non-admissible

116

(А6) Substances included in Table 2 of Annex 37/10 (EC)

200

100

100

Chloramphenicol (laevomycetin) Nitrofurans and metabolites: AOZ, AMOZ, SEM, AHD Nitroimidazole derivatives (dimetridazole, metronidazole, ronidazole, etc.)


ELISA, HPLC-MS-

MS

ELISA

HPLC-MS-MS

HPLC-MS-MS

0.25 μg/kg


0.5-1.0 μg/kg

0.25-1.0 μg/kg

GC-MS

HPLC-MS-MS

(HPLC)

HPLC-MS-MS

HPLC-MS-MS

0.2 μg/kg

0.5-1.0 μg/kg

0.25-1.0 μg/kg



200

Tetracyclines (Oxytetracyclin Methacyclin Doxycyclin) Bacitracin Grisein, etc.


HPLC Microbiological method ELISA HPLC-MS-MS

HPLC-MS-MS

0.1-0.2 μg/kg

0.01U/g 6.0 μg/kg 0.5-0.01 U/g 0.5–5.0 μg/kg

0.1-5.0 μg/kg

Non-admissible

117

Sulphonamides (sulfamethazine, sulfadimethoxine, sulfadiazine, etc.) (not less than 8 compounds)

ELISA (imp.) HPLC-MS-MS

HPLC-MS-MS

HPLC

20 μg/kg 1.0-10.0

μg/kg

1.0 –10.0 μkg/kg

CU Common

requirements Decision No.299

Fluoroquinolones (ciprofloxacin, enrofloxacin, etc.)


HPLC HPLC-MS-MS

10 μg/kg 0.1-10.0

μg/kg

0.1 –10.0 μg/kg

CU Common


118

В

(В2a) Anthelmintics

50

50



HPLC-MS-MS

HPLC-MS-MS

CU Common requirements

Decision No.299

Carbamates: Thiram (tetramethylthiuram disulfide (TMTD), thigam, thigam C, ophtanol T, raksyl+TMTD,vitavax 200, vitavax 200 FF, vitathiuram, phenoram, chemicar Т, orlok Sevin (carbaryl) Polycarbacyn


HPTLC,

colorimetric method

GC GC-MS

1.0-100.0 μg/kg

0.1 –1.0 μg/kg


Decision No.299

with annexes

119

В

(В2с) Carbamates and pyrethroids

50

Pyrethroids: Alphamethrin Deltamethrin Permethrin Sumicydin (fenvalerate) Cypermethrin (fury)


GC

HPLC GC-MS

HPLC-MS-MS

GC


0.5-5.0 μg/kg

0.5 –5.0 μg/kg


Decision No.299

with annexes

120

В2 В2f Other pharmacologically active substances (including В2b+B2d+B2e) Coccidiostatics



HPLC-MS

HPLC-MS CU Common reqiremnets

Decision No.299

with annexes

121

В3


100

100

100

100

Aldrin Heptachlor


Biological materials, etc. .

GC GC-MS

- \\ -

- \\ -

- \\ -

GC-MS

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

Non-admissible

Non-admissible

0.1 mg/kg Meat

0.2 mg/kg Fat, etc. 0.1 mg/kg Meat

1.0 mg/kg Fat, etc.

.

122

В3

(В3a) Organochlorine compounds, including PCB (dioxins

20

-



GC-EZD GC-MS

GC-MS

1.0 μg/kg

(PCB-105) 10.0-15.0 (for

a sum of isomers)

0.0005-1.0

μg/kg

CU

Common requirement

s Decision No.299

with annexes



GC-HRMS

GC-HRMS

0.01 ng/kg TEQ WHO


100

Trichlormetafos-3

Heterofos

Diazinon (bazudin)

Dichlorvinyl- dimethyl- -phosphate

(dichlorvos)


HPTLC,


OPCs including


- // -

- // -

GC

(NP)

GC-МС

- // -

- // -

- // -


(0.001-100 μg in 0.1 ml of a

sample), lower


0.001 μg

0.0005-1.0 μg/kg -

// -

- // -

- // -

CU

Common requirement

s Decision No.299

with annexes

123

В3


100

Dursban (chlorpyrifos) Karbofos (malathion) Metaphos (parathion-methyl,wofatox) Phosalone (phosalone) Phthalophos Antio Phosphamide Aktellik


HPTLC, Enzymatic method (all

OPCs including


- // -

- // -

- // -

- // -

- // -

- // -

Per a group

GC (NP)

GC-MS

(0.5-3.0 μg in

a sample)


See above

- // -

- // -

- // -

- // -

(10.0 μg/kg)

0.0005 -1.0 μg/kg

- // -

- // -

- // -

- // -

- // -

- // -

- // -

CU Common

requirements

Decision No.299

with annexes

124

Fat - 0.1 mg/kg

Arsenic

2.5 μg/kg - \\ - - \\ - 0.1 mg/kg – meat, fat 1.0 mg/kg – offal

Cadmium

20.0 μg/kg

- \\ - - \\ - 0.05 mg/kg - meat; 0.3 mg/kg -offal; 1.0 mg/kg -kidneys

Mercury

Screening

Colorimetric method., Flameless AAS

2.5 μg/kg

Twice a year 5% of enterprises with one sample

0.03 mg/kg – meat and fat 0.1 mg/kg - offal; 0.2 mg/kg – kidneys.

125

В3

(B3d) Mycotoxins

30 Ochratoxin А Zearalenon Others


HPTLC, ELISA


2 μg/kg 0.25 μg

- // -

0.1 – 0.5 μg/kg

- // -

Non-admissible - // -


200

200

50

10

Nitrates Nitrites Organomercury compounds 2,4-D acid, its salts and esters


Colorimetry

Colorimetry

HPTLC GC

HPTLC

GC

GC-MS

GC-MS

0.4 mg/kg

0.2 mg/kg

1.0 μg/kg

1.0 μg /kg

MAL meat-50 mg/kg

MAL meat-– 3 mg/kg


Decision No.299

with annexes

126

В3


Radionuclides:

Cesium – 137, Strontium –90

Microbiological


Spectrometry, radiometry CU Common requirements

Decision No.299

Spectrometry, radiometry with radiochemistry

CU Common

- \\ -


Decision No.299

with annexes

CU Common

127

В3


200

criteria

Unpatented drugs in case of suspicions in

their use


with annexes

GC-MS

HPLC- MS-MS

requirements

Decision No.299

with annexes

GC-MS

HPLC- MS-MS

- \\ -


with annexes Non-adimissible

128

В3


50

Plumbum

Biomaterials. plasma and serum, hair.

IVA. AAS

AAS AAS-ETA ICP-MS

50 μg/kg

0.01-1.0 μg/kg

0.5 mg/kg – meat

0.6 mg/kg – offal 1.0 mg/kg – kidney 0.1 mg/kg – fat

129

50

50

Arsenium

Cadmium

IVA. AAS

AAS-ETA ICP-MS

2. 5 μg/kg 0.01-1.0 μg/kg

0.01 – 1.0 mg/kg – meat

and fat 1.0 mg/kg -

offal

ААS AAS-ETA ICP-MS

20 μg/kg

0.01-1.0 μg/kg

0.05 mg/kg – meat;

0.03 mg/kg – fat;

0.3 mg/kg – offals;

1.0 mg/kg -

kidneys

B3


50

Mercury

Biomaterials: plasma and serum, hair

Color. Plasmaless ААS


2.5 μg/kg

0.01-1.0 μg/kg

0.03 mg/kg – meat and fat; 0.1 mg/kg – offal; 0.2 mg/kg - kidneys

10


Ionometry. chem..

3.0 mg 3.0 mg Biochem. norm.

130

10

ICP-MS


AAS AAS-ETA ICP-MS

10 μg/kg 10 μg/kg

50


Calium 1.0 μg/kg 1.0 μg/kg




50

Cobalt Biomaterials: plasma and serum, hair

AAS AAS-ETA ICP-MS

AAS AAS-ETA ICP-MS





131

List of control parameters for the state veterinary monitoring of drug preparation, banned and toxic substance residues for veterinary

laboratories of the Russian Federation in 2013 (aquaculture – fish and fish products) Table 10.

Groups of substances according to 96/23/ЕС of

29 April 1996

Number of

samples

Name of the substance (active substance),

metabolites

Type of product

(object of examinat

ion)

Screening methods

Confirmation

methods


the screening method



Admissible levels

(standards)

А (А3) Natural steroids (А1) Stilbenes (А3) Synthetic steroids

1,220 1,220 1,220

Testosterone, Progesterone, Oestradiol -17 Hexestrol, Dienestrol Diethylstilbestrol Nandrolone Trenbolone, Methyltestorone, Medroxiprogesterone Megesterol

Live fish, fresh, chilled, frozen fish, minced fish, fish fillet, fish liver

ELISA GC-MS

ELISA

GC-MS

GC-MS

HPLC-MS-MS

(HPLC)

GC-MS

HPLC-MS-MS

(HPLC)

0.25 μg/kg

0.5 μg/kg

0.05 μg/kg 0.1-0.5 μg/kg

0.25-2.8 μg/g 0.1-0.5 μg/kg

0.1-0.5 μg/kg

- // -

Natural level Non-admissible

132

А6) Substances in Table 2 to Annex 37/2010 (EC)

1,220 Chloramphenicol

ELISA HPLC-MS-

MS

GC-MS

(Chem.ion.)

HPLC-MS/MS

0.2 μg/kg 0.25 μg/kg Non-admissible

А А6) Substances in Table 2 to Annex 37/2010 ( EC)

1,220 Nitrofuran derivatives and metabolites: -AOZ -AMOZ - AHD - SEM Nitroimidazole derivatives

Live fish, fresh, chilled, frozen fish, Minced fish, fish fillet, fish liver

ELISA HPLC-MS-

MS

HPLC-MS-MS

HPLC-MS-MS

HPLC-MS-

MS

0,1– 0.2 μg/kg

1.0-50.0

μg/kg 0.5-1.0 μg/kg

0.5-1.0 μg/kg

0.25 – 1.0

μg/kg

0.5 –1.0 μg/kg

0.25 - 1.0 μg/kg

Non-admissible

Non-admissible

133

В (В1) Antibacterial substances, including sulfanilamides and quinolones (B1)

3,б90

Antibiotics Tetracyclines (Oxytetracycline, Methacycline, Doxycycline), Chlortetracycline Streptomycine Erythromycine Terramycine etc. Others

Microbiological method

ELISA HPLC-MS-

MS (HPLC)

Microbiological method ELISA (imported)

HPLC MS-MS -(HPLC)

0.1-0.2 μg/kg

0.01 U/g

1.5 μg/kg 6 μg/kg 0.5-5.0 μg/kg

0.5-0.01 U/g

17-25 μg/kg

0.5-5.0 μg/kg

Non-admissible

Non-admissible

Sulphonamides (Sulfathiazine, sulfamethazine, sulfadimethoxine, sulfathiazole etc.) (8 drugs)

ELISA (imp.)

HPLC-MS-MS

HPLC MS-MS-

20 μg/kg 1.0-20.0

μg/kg

1.0 –20.0 μg/kg

CU CR Decision No.299

Fluoroquinolones (ciprofloxacin, enrofloxacin etc.)

ELISA HPLC-MS-

MS

HPLC MS-MS-

10 μg/kg 0.1-10.0

μg/kg

0.1 –10.0 μg/kg


134

В

(B2a) Anhelminthics

1,480

Ivermectin Other anhelminthics Albendazole Fenbendazole Flubendazole Mebendazole etc.


(HPLC)

HPLC-MS-MS

HPLC-MS-MS

1.0 μg/kg

25 μg/kg 25 μg/kg 25 μg/kg 25 μg/kg

0.5 –5.0 μg/kg

25 μg/kg -//- -//- -//-

SanPiN 2.3.2.2804-10, CU CR Decision No.299

135

(В2c) Carbamates and pyrethroids

200

Carbamates: Thiram (tetramethylthiuram disulfide (TMTD), thigam, thigam C, ophtanol T, raksyl+TMTD, vitavax 200, vitavax 200 FF, vitathiuram, phenoram, chemicar Т, orlok Sevin (carbaryl) Other carbamates

Colorimetric GC

GC-MS

GC

GC-MS

1.0-100.0

μg/kg

0.1-1.0 μg/kg

0.1 –1.0 μg/kg

CU CR Decision No.299 as amended

136

В

(В2c) Carbamates and pyrethroids

(В2f) Others

200

100

Pyrethroids: Alphametrin Deltamethrin Permethrin Sumicydin (fenvalerate) Cypermethrin (fury)


GC GC-MS HPLC

HPLC-MS-MS

GC GC-MS HPLC

HPLC-MS-MS

0.5-5.0 μg/kg

0.5 –5.0 μg/kg

ADD -0.005 mg/kg ADD -0.003 mg/kg ADD – 0.035 mg/kg AL – 0.0015 mg/kg 0.0015 mg/kg

137

В3

В3

(B3a) Organochlorine compounds, including PCB and dioxins. (B3a) Organochlorine compounds, including PCB and dioxins

2,250

2,250

Hexachlorocyclohexne (α-,β-, γ- isomers) DDT and its metabolites

GC GC-MS

GC GC-MS

GS-MS

GS-MS

0.1-2.0 μg/kg

0.1-0.2 μg/kg

0.1-2.0 μg/kg 0.1-0.2 μg/kg

Liver – 1.0 mg/kg; Sea fish - 0.2 mg/kg Fresh water fish – 0.3 mg/kg; Liver – 3.0 mg/kg; Sea fish - 0.2 mg/kg Fresh water fish – 0.3 mg/kg; Sturgeon, salmon, herring – 2.0 mg/kg

138

B3

(B3a) ChOC

1,000

50

PCB (polychlorinate d biphenyls) (PCB 101, 118, 138, 153, 180, 28, 52)


GC-electron capture detector GC-MS

GC-MS 1.0 μg/kg (for PCB-

105) 10.0-15.0 (for the sum of

isomers)

0.0005-1.0 μg/kg



GC-MS GC-HRMS

0.01 ng/kg TEQ WHO


139

2,250

2,250

2,250

Aldrin Heptachlor Other ChOC


GC-MS

0.0005-1.0 μg/kg

Non-admissible

140

В3 (В3b) Organophosphorous compounds

200 Trichlormetaphos-3 Heterophos Dichlorvinyl- dimethyl- -phosphate (dichlorvos) Diazinon (bazudin) Dursban (chlorpyrifos) Karbofos (malathion) Metaphos (parathion-methyl, wofatox) Phosalone (phosalone) Phthalophos Antio Phosphamide Aktellik


HPTLC, GC Enzymatic method GC-MS

GC GC-MS

0.1- 50 μg in a

sample, low

detection limit:

0.0001-0.001 μg

0.5-3.0 μg in a

sample

0.5-3.0 μg in a

sample See above

0.01

mg/kg

0.0005 – 1.0 μg/kg

CU CR

Decision No.299 as amended

141

В3

(В3с) Chemical elements

2,250

2,250

Plumbum

Cadmium


IVA AAS

-//-

AAS

AAS AAS-EТА ICP-MS

-//- AAS

AAS-ETA ICP-MS

10.0 μg/kg

10 μg/kg 20.0 μkg/kg

0.01 –1.0 μg/kg 0.01-1.0 μg/kg

- // -

0.5 mg/kg 2.0 mg/kg –

tuna, swordfish,

great sturgeon

(liver – 1.0 mg/kg)

0,2 mg/kg

liver – 0.7 mg/kg)

142

В3 (В3с) Chemical elements (В3d) mycotoxins (В3е) Colorants

2,250

2,250

200

500

Mercury Arsenic Free choice (codifier group including feeds- group of aflatoxins, ochratoxins, etc.) Malachite green


Feeds for fish

Commercially cultured fish

Colorimetric

Flameless AAS

IVA ААS

HPTLC ELISA HPLC

ELISA

AAS-MHG

ААS ААS-EТА ICP-MS HPLC HPLC MS-MS HPLC MS-MS

2.5 μg/kg

5.0 μg/kg

0.25-2.0 μg/kg

1 μg/kg

0,01- 1,0 μg/kg

- // -

0,1 – 0,5

μg/kg

1 μg/kg

0.3 mg/kg – fresh water nonpredator

y fish; 0.6 mg/kg – fresh water predatory

fish; 0.5 mg/kg –

sea fish; 1.0 mg/kg –

tuna, swordfish,

great sturgeon

(liver – 0.5 mg/kg)

1.0 mg/kg –fresh water fish; 5.0 mg/kg –sea fish Non-admissible Non-admissible

143

В3


1,000

100

100

500

50

50

50

500

20

Histamine

Nitrates Nitrites Nitrazamines (a sum of nitrozodimethylamine and nitozodiethylamine) Formaline (formaldehyde) Blue copperas (copper sulphate) Organomercury compounds 2,4-D acid, its salts and esters

DNOC (dinitroortocresolum


Colorimetry HPLC

Colorimetry Colorimetric HPTLC

HPTLC Colorimetry

HPTLC, GC

HPTLC, GC

HPTLC, GC

HPLC

HPLC

GC, GC-MS

AAS

GC

GC-MS

GC-MS

GC-MS

10 mg/kg

400 μg/ml 200 μg/kg 1 μg/kg

3 μg/kg

250-400 μg/kg

10 μg/kg

1-800 μg/kg

-

5 mg/kg


- -

0.003 mg/kg

CU CR Decision

No.299 as amended

Non-

admissible (all food products)

Non-


Non-


144

В3


10

100

500 1,000

50

Bioresmetrin (isatrin) Dasomet (tiazon) Bigon Nitrophen Other pesticides and biotoxicity Phosphates Radio nuclides: Cesium – 137, Strontium –90 Microbiological indicators Parameters of freedom from parasites Unpatented veterinary drugs, under suspicion

Live fish, fresh, chilled, frozen fish, Minced fish, fish fillet, fish liver Fish products

Colorimetri

c HPTLC

GC HPTLC

GC HPTLC

GC HPTLC,

GC HPTLC,

GC HPLC

Chem.

Spectrometry, Radiometry CU CR Decision No.299 as amended

GC-MS HPLC-MS-MS

GC

GC-MS -//-

-//-

-//-

-//-

-//-

Chem. HPLC

CU CR Decision No.299 as amended GC-MS HPLC-MS-

MS

10 μg/kg

10-300 μg/kg

10 μg/kg

Spectrometry, radiometry with radiochemical excretion

0.0005 -1.0 μg/kg

CU CR Decision No.299 as amended Non-admissible

145

Table 11 List of control parameters for the state veterinary monitoring of drug preparation, banned and toxic substance residues for veterinary

laboratories of the Russian Federation in 2013 (aquaculture – mollusks, crustaceans and other non-fishery objects).

Group of substances according to 96/23/ЕС of

29 April 1996

Number of

samples

Name of the substance (active substance),

metabolites

Type of product

(object of examinat

ion)

Screening methods

Confirmation

methods





Admissible levels

(standards)

A. (А6))Substances included in Table 2, Annex 37/10 (EC)

220 Chloramphenicol

Mollusks, crustaceans, etc.

ELISA

HPLC-MS-MS

GC-MS

HPLC-MS-MS

0.05-0.08 μg/kg

0.1-0.3 μg/kg

0.1-0.3 μg/kg

Non-admissible

200 Nitrofurans (AOZ, AMOZ, SEM, AHD) Nitroimidazoles (dimetridazole, metronidazole, ronidazole, etc.)


ELISA

HPLC-MS-

MS

HPLC HPLC-MS-

MS

0.1 μg/kg (AOZ),

0.2 μg/kg (AMOZ) 0.25-1.0

μg/kg

0.25 –1.0 μg/kg

Non-admissible

146

В(В1) (В1) Antibiotics

200

200

Tetracyclines, Streptomycine, etc.


Microbiological

ELISA HPLC-MS-

MS

HPLC MS-MS

6-60 μg/kg

0.1-5.0 μg/kg

0.1-5.0 μg/kg

Non-admissible

Sulphonamides (Sulfamethazine, sulfadimethoxine, sulfadiazin etc.) (not less than 8 compounds)


ELISA HPLC-MS-

MS

HPLC HPLC

MS-MS-

2 μg/kg 1.0-10.0

μg/kg

1.0 –10.0 μg/kg

SanPin 2.3.2.2804-10, CU CR Dec. No. 299 with annexes

200 Fluoroquinolones (enrofloxacin, ciprofloxacin etc.)

ELISA HPLC-MS-

MS

HPLC-MS-MS

10,0 μg/kg 0.1-10.0

μg/kg

0.1-10.0 μg/kg

147

В3 (B3) В3 (B3)

(В3а) Organochlorine compounds, including PCB (dioxins) (В3а) Organochlorine compounds, including PCB (dioxins)

300

300

300

300

20

10

Aldrin Heptachlor HCH (α, β-, γ- isomers) DDT and its metabolites


GC GC/MS

- \\ -

- \\ -

- \\ -

GC GC/MS

- \\ -

- \\ -

- \\ -

0.5-10.0 μg/kg

0.1 – 1.0 μg/kg

0.1-1.0 μg/kg



GC-ECD GC-MS

GC-MS 1.0 μg/kg (PCB-105)

10.0-15.0 (for total isomer)

0.0005 – 1.0 μg/kg

Polychlorinated di benzo-p-dioxines and dibenzofurans


GC- HRMS

GC-HRMS

0.01 ng/kg TEQ WHO

0.01 ng/kg TEQ WHO

B(B3)

(B3с) Chemical

300

Plumbum

Mollusks, crustacean

Stripping voltammetr

AAS (AAS-ETA)

50.0 μg/kg 0,01-1,0 μg/kg

10.0 mg/kg

148

elements

300

300

300

Arsenic

s, etc.

- \\ - Mollusks, crustaceans, etc.

y, AAS ICP-MS 2.5 μg/kg 5.0 mg/kg

Cadmium 20.0 μg/kg 2.0 mg/kg

Mercury 2.5 μg/kg 0.2 mg/kg

B(B3) B(B3) Mycotoxins and biotoxins

30 See B3f

ELISA HPLC

HPLC-MS

HPLC HPLC-MS

20

Malachite green and p-

tetratmethyldiaminotripheny methane,

crystal violet

ELISA HPLC-MS/MS

ELISA HPLC-MS/MS

1 μg/kg 1 μg/kg

Non-admissible

B(B3)

(B3f) Other substances and environmental contaminants

200

According to separate

plan

Radionuclides: Cesium-137,

Strontium –90


Spectrometry, radiometry CU CR Dec. No. 299 with annexes

CU CR Dec. No. 299 with annexes

149

B(B3)

- \\ -

20

30

30

2,4-D acid, its salts and esters

Pesticides

Algal toxins:

Saxitoxin (PSP-paralytic

toxin) DSP-

GC GC-MS

ELISA (imp.)

GC GC-MS HPLC-MS/MS biotest.

CU CR Dec. No. 299 with annexes

50 μg/kg

10 μg/kg

5.0(1.0-800.0 μg/kg)

50 μg/kg

10 μg/kg

CU CR Dec. No. 299 with annexes CU CR Dec. No. 299 with annexes

150

30

30

If necessary,

in the course of control

activities

diarrhetic shellfish poison, okadaic

acid ASP- amnesic

shellfish poisoning, domoic acid Microcystin Yessotoxin

Unpatented drugs

GC, HPLC, HPLC-MS, GC-MS

10 μg/kg

10 μg/kg

151

List of control parameters for the state veterinary monitoring of residues of drug preparations, banned and toxic substances for veterinary laboratories in the Russian Federation in 2013 (fish roe, milt and their products)*

Table 12

Groups of substances according to 96/23/ЕС April 29, 1996

Number of tested samples

Name of the preparation,

active substance, metabolites

Type of product

(Object of the

investigation)

Screening methods

Confirmation

methods


Detection limit of


μg/kg

Acceptable levels of

substances (norms)

RF

А (А6) Substances included into Table 2 of the Annex 37/10 (EC)

100 100

Chloramphenicol

Fish roe, milt and their products

ELISA HPLC-MS-MS

HPLC-MS-MS

0.05-0.08 μg/kg

0.1-0.5 μg/kg

0.1-0.5 μg/kg

Non-admissible

Nitrofurans and Metabolites (AOZ, AMOZ, SEM, AGD) Other nitroimidazole derivatives

ELISA HPLC-MS-MS

HPLC-MS-MS

0.1 μg/kg (AOZ),

0.2 μg/kg (AMOZ) 0.25-5.0

μg/kg

0.25-5.0 μg/kg

Non-admissible

152

В Группа (В1) Antibiotics including sulfanilamides and quinolones

200

20 20

(В1) Antibiotics (tetracycline group, etc.) Sulfanilamides (sulfamethazine, sulfadimethoxine, sulfadiazine etc. (at least 8 compounds)


Microbiological ELISA HPLC-MS-MS

HPLC-MS-MS

6-60 μg/kg 1.0 μg/kg

2 μg/kg

1-10 μg/kg

HPLC-MS-MS

HPLC-MS-MS

0.5-5.0 μg/kg

1-10 μg/kg

Non-admissible

Non-admissible

Fluoroquinolones (enrofloxacin, ciprofloxacin etc.)

Microbiological ELISA

HPLC-MS

HPLC HPLC-MS

10,0 μg/kg

1.0-10.0 μg/kg

1.0-10.0 μg/kg


В3 - // -

(В3а) Organochlorine compounds, including PCB and dioxins - // -

300 Aldrin Heptachlor HCH, alpha-, beta- gamma (α, β-, γ- isomers) DDT and its metabolites

Fish roe, milt and

their products

GC GC-MS

- \\ -

- \\ -

- \\ -

GC GC-MS

0.1 – 1.0 μg/kg

0.1-1.0 μg/kg

Non-admissible

Non-

admissible

0.2 mg/kg

2.0 mg/kg

20 PCB (polychlorinated biphenyls

GC

GC-MS 1.0 μg/kg (PCB-105)

10.0-15.0 (for total isomer)

0.0005 – 1.0 μg/kg

2.0 mg/kg

153

20 Polychlorinated dibenzo-p-dioxines and dibenzofurans


GC-MS

GC-HRMS

0.01 ng/kg TEQ WHO


with annexes

В3

(В3d) Chemical elements

300

Plumbum


IVA AAS

AAS-ETA

AAS AAS- ETA

ICP-MS

50 μg/kg

0,01-1,0 μg/kg

1.0 mg/kg

Arsenic

2.5 μg/kg 1.0 mg/kg

Cadmium


Mercury

Colorimetry

Flameless AAS

AAS-MHG


(В3f) Other substances and contaminants of the environment (В3f) Other substances and contaminants of

300 Separate

Radio nuclides: Cesium – 137,

Strontium –90

Microbiological indicators

Parameters of parasite freedom

Fish roe, milt and

their products

Spectrometry and radiometry SanPiN 2.3.2.1078-01

--//--


154

the environment

Total: 300 samples

plan.

50

50

50

50

Preservatives: Sorbic acid

Urotropin (hexamethylene tetramine) Other preservatives including banned ones 2,4-D acid, salts and esters Other pesticides

Fish roe, milt and

their products

Colorimetric

Titrimetric, colorimetr

ic. GC-MS,

HPLC-MS (MS-MS) GC, GC-MS

HPTLC, GC, GC-

MS, HPLC MS/MS

HPLC

HPLC

GC-MS, HELC-

MS (MS-MS)

GC,GC-

MS

GC,GC-MS GC-MS HPLC-MS/MS

500.0 μg/kg

10.0 μg/kg -

5.0 (1,0-800,0

μg/kg)


with annexes

5.0 (1,0-800,0 μg/kg)


--//--

Non-

admissible

CU CR Decision No.299 with

annexes

CU CR Decision No.299 with

annexes

155

Monitoring plan of the residues of dangerous and harmful substances in cow milk in 2013 Table 13-14

Groups of substances according to 96/23/ЕС of

April 29, 1996

Number of

tested samples

*

Name of the preparation

(active substance)

Type of product

Screening methods

Confirmation methods

Limit of the determination

of the screening method

μg/l

Limit of the determination

of the confirmation

method μg/l

Acceptable levels of

substances (norms)

mg/kg (l), not more

RF A

(А6) Substances from Table 2 of Annex 37/10 (EC)

1,770 Chloramphenicol

Milk

ELISA HPLC/MS-

MS

HPLC/MS-MS

0.005-0.025 μg/l

0.2 μg/l

0.2 μg/l

Non-admissible

1,770 Nitrofurans and their metabolities (AOZ, AMOZ, SEM, AHD) Nitroimidazole derivatives (dimetridazole, metronidazole, ronidazole)

ELISA HPLC/MS-

MS

HPLC-MS-MS

HPLC/MS-MS

HPLC-MS-MS

0.1 μg/l (AOZ), 0.2 μg/l

(AMOZ) 0.5 -1.0 μg/l

1.0 μg/l

0.5-1.0 μg/l

1.0 μkg

Non-admissible

Non-admissible

156

B

(B1)Antibacterial drugs, including sulfanilamide drugs and quinolones **

** See “Inhibitory

substances

1,769

1,769

Antibiotics - streptomycin etc. - tetracycline group

- penicillin other antibiotics, including beta-lactams

Milk

microbiologic ELISA, HPLC

HPLC HPLC-MS-

MS

1.5 -15.0 μg/l 0.5-20.0 μg/l

0.2-2 μg/l

0.2 - 2 μg/l

Non-admissible

Sulfanilamids (sulphametasine, sulphadimethoxine, sulphadiazine and others (not less than 8 compounds)

HPLC HPLC/MS-

MS

HPLC HPLC-MS-

MS

1.0 - 10.0

μg/l

1.0 – 10.0

μg/l

CU

Common requiremen

ts, Decision No. 299

with Annexes

157

B2

Fluoroquinolones (enrofloxacin,

ciprofloxacin and others)

ELISA HPLC/MS-MS

HPLC HPLC-MS-

MS

1.0 μg/l

1.0 – 3.0 μg/l

CU Common

requirements,

Decision No. 299

with Annexes

B2а Anthelmentics

20 1,770

50

Hexichol Milk

HPLC HPLC/MS-

MS

HPLC HPLC- MS-MS

1.0 – 5.0 μg/l

1.0 -5.0 μg/l

CU Common

requirements,

Decision No. 299

with Annexes

Axermectins (ivermectin, doramectin, abamectin, moxidectin, emamectin)

Other

anthelmintics (benzimidazole

derivatives)

HPLC HPLC/MS-MS

- // -

HPLC/MS - MS-MS

HPLC/MS-MS

1.0 μg/l 1.0 – 3.0 μg/l

1.0 – 3.0 μg/l

CU Common

requirements,

Decision No. 299

with Annexes

158

B2c. Carbamates and pyrethroids

50

Carbamates:

Thiram (TMTD)

colometric

GC-MS HPLC/MS-

MS

1.0-100 μg/l

0.1-0.5 μg/l

CU Common

requirements,

Decision No. 299

with Annexes

-//-

Sevin -//-

Bigon -//-

Dicrezil

В 2 B2c. Carbamates and pyrethroids

50 Pyrethroids

Milk

GC GC-MS

GC-MS

0.1 – 0.5 μg/l

0.1-0.5 μg/l

-//-

В2e Nonsteroidal antiinflammatory drugs

140 Phenylbutazone and others

GC-MS HPLC- MS

GC-MS HPLC- MS

-//-

159

В2f Other pharmacological active substances

2,000 Test «Inhibiting substances»

GOST 23454-79

GC-MS HPLC- MS

-//-

B3a

B3a. Organochlorine compounds including PCB and dioxins

2,158

Hexachlocyclorxecane (α, β, γ- isomers)

Milk

GC

GC GC-MS

0.5 -10,0 μg/l

0.1- 0.5 μg/l

mg/l

50.0

160

B3a B3a. Organochlorine compounds including PCB and dioxins

2,158 20

20

DDT and metabolites

Milk

GC (HPTLC)

GC-MS 0.5-10.0 μg/l

1.0-5.0 μg/l

μg/l

50.0

Aldrin Non-admissible

Heptachlor Non-admissible

161

20

PCB

GC-ECD GC-MS

GC-MS

1.0 μg/l (for PCB

105) 10.0-150.0

(for the sum of

isomers )

0.0005-1.0 μg/l

-

162

B3 B3

B3b Organophosphorous compounds

400

100

OPC group: Chlorophos (trichlormetaphos) Trichlormeta

phos-3

DDVP

Amydophos

Diazinon (neocidol)

Heterophos

Crotoxiphos

Milk

HPTLC, GC, enzyme method (all OPC including activated)

GC GC-MS

-//-

-//-

-//-

-//-

-//-

-//-

GC, GC-MS

GC, GC-MS

0.1-50 μg in the sample (0.001-100 μg in 0.1 мl of the sample ), lower detection limit (0.0001-0.001 μg)

-//-

-//-

-//-

-//-

-//-

-//- 0.1-5.0 μg in the sample),

0,1 – 0.5

μg/l

163

В(В3)

100

Cumaphos

Dibrom

Metaphos

Temephos

Phention

Phozalone

Milk

HPTLC. GC, enzymatic method (all OPC including activated)

-//- -//- -//- -//- -//- -//-

(0.001-100 μg in 0.1 мl

of the sample lower

detection limit

(0.0001-0.001 μg)

-//-

-//-

-//-

-//-

-//-

-//-

0.1-0.5 μg/l

164

В3с Chemical elements

2,158

Plumbum Arsenic Cadmium Mercury

Milk

IVA AAS

Flameless AAS

AAS AAS-ETA AAS-MHG

ICP-MS

μg/l

10.0

2.5

10.0

2.5

165

B3d Mycotoxins

400

Aphlatoxin M1

ELISA HPLC

(HPTLC)

GC-MS HPLC

HPLC-MS

0.5-3.0 μg/l 0.025-0.5 μg/l

В3 В3

B3(f) Other substances


Microbiology

Microbiology - -

Radionuclides:

Groups and subgroups of substances 96/23 ЕС.

Number of samples

Names of criteria and type of products

Test methods (screening and confirmation)

AL FZ-88

В B3f Others

400 Cesium -137 Spectrometry, radiometry

AL FZ-88

400 Strontium- 90 Spectrometry, radiometry

AL FZ-88

166

Table 15 List of control parameters of the state veterinary monitoring of residues of drugs, banned and toxic substances for veterinary laboratories of

the Russian Federation in 2013 (chicken eggs) *

Groups of substances acc. to 96/23/ЕС of April 29,1996

Number of samples

Name of the preparation (active substance)

Type of product tested

Screening methods

Confirmation

methods

Detection limit of the screening

method

Detection limit of

the confirm. method

Admissible levels (standards)

А (А6) Substances, listed in Table 2 of Appendix 37/10 (EU)

1,600 Chloramphenicol (laevomycetin, CAP)

Chicken eggs and egg products, etc

ELISA (imp.) HPLC-МS-МS

GC-MS HPLC-МS-МS

0.05 μg/kg

0.1-0.3 μg/kg

Non-admissible

167

1,700

1,600

Nitrofurans and their metabolites (AOZ, AMOZ, SEM, AHD) Nitroimidazoles (dimetridazole, metronidazole, ronidazole and others)

ELISA HPLC-МS-МS HPLC-МS-МS

HPLC-MS-MS HPLC-МS-МS

0.1 μg/kg (AOZ) 0.2 μg/kg (AMOZ)

0.25-1.0 μg/kg

0.25-1.0 μg/kg

0.25-1.0 μg/kg

0.25-1.0 μg/kg

Non-admissible

Non-admissible

В1 (В1) Antibacterial substances including sulfanilamid preparations and quinolones

1,600

Antibiotics: Tetracyclin (Oxitetracyclin Metacycline Doxicyclin, Chlortetracyclin) Streptomycin (Erytromycin, Terramycin and others) Bacitracin

Chicken eggs and egg products

HPLC microbiological ELISA HPLC-МS-МS

Microbiological ELISA (imp.)

HPLC-MS-MS

0.1-0.2 μg/kg 5.0 μg/kg

0.01units/g

0.05 μg/kg

0.2-2.0 μg/kg 0.5-0.01 units/g

0.2-2.0 μg/kg

Non-

admissible (< 0.01)

Non-admissible

(< 0.5)

Non-admissible (< 0.02)

168

1,600

Sulfanilamides: Sulfamethazine, Sulfadimetoxine, sulfadiazine and others (not less than 8 compounds) Fluoroquinolones: Enrofloxacin Ciprofloxacin etc. Other antibiotics

ELISA (imp.) HPLC-МS-МS ELISA (imp.) HPLC-МS-МS HPLC HPLC-MS-MS

HPLC-MS-MS HPLC-MS-MS HPLC HPLC-MS-MS

1-20 μg/kg

10.0 μg/kg

0.1-10.0 μg/kg 0.2-2.0 μg/kg

1-10 μg/kg

0.1– 10.0 μg/kg

0.2-2.0 μg/kg


Decision No.299

B2b B2b. Coccidiostats 1,600 Lasalocid, Narazine, Salinomicine, Monenzine, Semduramicin, Maduramicin, Robenidin, Decoquinat, Halofuginone, Nicarbazin, Diclazuril and others


HPLC-МS-МS HPLC-МS-МS



Decision No.299

169

В2 е-f Other pharmacologically active substances

120 Vitamins of groups A,D,E,B, coloring agents and other


HPLC HPLC-МS-МS

HPLC HPLC-МS-МS


Decision No.299

В3

В3

(В3a) Organochlorine compounds (including PCB (dioxins)

(В3a) Organochlorine compounds (including PCB (dioxins)

700

700

700

700

Aldrin and etc. Heptachlor and etc.

Chicken eggs and

egg products

Chicken eggs and

egg products

GC GC-MS

- // -

GC-МS

- // -

0.1-1.0 μg/kg - // -

0.1-1.0 μg/kg

- // -

Non-admissible

Non-admissible

Hexachlorcyclohexan (α-,β-, γ- isomers) DDT and its metabolites

GC

GC-MS

GC-МS

- //-

- //-

0.1 mg/kg

0.1 mg/kg

170

50 20

PCB (Polychlorinated biphenyls) Polychlorinated dibenzo-p-dioxins and dibenzofurans

GC-ECD

GC-МS

1.0 μg/kg (for PCB-105)

10.0-15.0 (for the sum of isomers)

0.0005-1.0 μg/kg


Decision No.299

GC-MS

GC-HRМS

0.01 ng/kg ng\kg TEQ WHO


Decision No.299

В3


700

700

Plumbum

Chicken eggs and

egg products

IVА AAS

AAS-ETA ICP-IC

50.0 μg/kg

0.01- 1.0 μg/kg

0.3 mg/kg Eggs and liquid egg products

3.0 mg/kg Dry egg products

0.5 mg/kg Dry

albumin

Arsenic

AAS AAS-ETA

ICP-IC

2.5 μg/kg - \\ - 0.1 mg/kg Eggs and liquid egg products

171

В3


700


0.2 mg/kg Dry

albumin

Cadmium

Chicken eggs and

egg products

.

ААS

ААS ААS-EТА

ICP-IC

20.0 μg/kg

- \\ -



0.05 mg/kg Dry

albumin

172

В3

700

Mercury

Color. AAS

flameless.

AAS-MHG

2.5 μg/kg

-\\- 0.02 mg/kg Eggs and

egg products


0.03 mg/kg Dry

albumin

(В3f Other substances including unpatented preparations (В3f). Other substances including unpatented preparations

500 100 Separate

Plan

Radionuclides: Cesium– 137, Strontium –90

Pesticides(OPC,

carbamates and others)

Chicken eggs and

egg products

.

.

Chicken eggs and

egg

Spectrometry,

radiometry

GC, GC-МS


Decision No.299



Decision No.299

-

-


Decision No.299

173

200

Unpatented veterinary drugs

products

ELISA

GC HPLC

GC-MS

HPLC-MS

-

Non-admissible

174

Table 16 List of control parameters of the state veterinary monitoring of residues of drugs, banned and toxic substances for veterinary laboratories of

the Russian Federation in 2013 (other eggs)

Groups of substances acc. to 96/23/ЕС of 29.04.96

Number of samples

Name of the preparation (active substance)


Screening

methods

Confirmation methods

Detection limit of the screening

method μg/kg

Detection limit of

the confirm. method μg/kg

Admissible levels (standards)

А (А6) Substances listed in Table 2 of Annex 37/10 (EC)

100 Chloramphenicol (levomycitin, CAP)

Chicken eggs, egg products etc.


GC-MS HPLC-MS-MS

0.05 μg/kg

0.1-0.3 μg/kg

Non-admissib

le

175

100

100

Nitrofurans and their metabolites (AOZ, AMOZ, SEM, AHD) Nitroimidazoles (dimetridazole, metronidazole, ronidazole and others)

ELISA HPLC-MS-MS HPLC- MS-MS

HPLC MS-MS HPLC-MS-MS

0.1 μg/kg (АОZ)

0.2 μg/kg (АМОZ)

0.25-1.0 μg\kg

0.25-1.0 μg/kg

0.25-1.0 μg/kg

0.25-1.0 μg/kg

Non-admissib

le

Non-admissib

le В1 (В1) ) Antibacterial

substances including sulfanilamide preparations and quinolones

100

Antibiotics: Tetracycline (Oxitetracycline Methacycline Doxicycline, Chlortetracycline) Streptomycin (Erytromycin, Terramycin and others) Bacitracin


HPLC microbiological ELISA HPLC-MS-MS

Microbiological ELISA (imp.)

HPLC-MS-MS

0.1-0.2 μg/kg

5.0 μg/kg

0.01 units/g 0.05 μg/kg 0.2-2.0 μg/kg 0.5-0.01 units/g

0.2-2.0 μg/kg

Non-

admissible

(< 0.01)

Non-admissib

le (< 0.5)

Non-

admissible

(< 0.02)

176

100

Sulphanilamides: (Sulfamethazine, Sulfadimetoxine, sulfadiazine and others (not less than 8 compounds)) Fluoroquinolones: Enrofloxacin Ciprofloxacin etc. Other antibiotics

ELISA (imp.) HPLC-MS-MS ELISA (imp.) HPLC-MS-MS HPLC HPLC-MS-MS

HPLC-MS-MS HPLC-MS-MS HPLC HPLC-MS-MS

1-20 μg/kg

10.0 μg/kg 0.1-10.0 μg/kg

0.2-2.0 μg/kg

1-10 μg/kg 0.1 – 10.0 μg/kg 0.2-2.0 μg/kg


B2b B2b. Coccidiostats 100 Lasalocid, Narazine, Salinomicine, Monenzin, Semduramycin, Maduramicine, Robenidin, Decoquinat, Halofuginone, Nicarbazin, Diclazuril and others





177

В2e-f Other pharmacologically active substances

100 Vitamins of groups A,D,E,B, coloring agents and other


HPLC HPLC-МS-МS

HPLC HPLC-МS-МS


В3

В3

(В3a) Organochlorine compounds (including PCB dioxins)

(В3a) Organochlorine compounds (including PCB dioxins)

50

50

50

50

Aldrin and etc. Heptachlor and etc.

Chicken eggs and

egg products

Chicken eggs and

egg products

GC GC-MS

- // -

GC-МS

- // -

0.1-1.0 μg/kg

- // -

0.1-1.0 μg/kg

- // -

Hexachlorcyclohexan (α-,β-, γ- isomers) DDT and its metabolites

GC

GC-MS

GC-МS

- //-

- //-

178

50

20

PCB (Polychlorinated biphenyls)


GC-ECD

GC-МS

1.0 μg/kg (for PCB - 105)

10.0-15.0 (for the sum of isomers)

0.0005-1.0 μg/kg

GC-MS GC-HRМS

0.01 ng/kg ng/kg TEQ WHO


179

В3


100

100

Plumbum

Chicken eggs, egg products,

etc.

IVА AAS

AAS-ETA ICP-IC

50.0 μg/kg

0.01- 1.0 μg/kg



0.5 mg/kg Dry albumin

Arsenic

AAS AAS-ETA

ICP-IC

2.5 μg/kg

- \\ - 0.1 mg/kg Eggs and liquid egg products



180

В3


100

100

Cadmium


etc.

ААS

ААS ААS-EТА

ICP-IC

20.0 μg/kg

- \\ -




Mercury Color. AAS

flame-less.

AAS-MHG

2.5 μg/kg

-\\- 0.02 mg/kg Eggs and

egg products



181

В3

(В3f) Other substances including unpatented preparations (В3f). Other substances including unpatented preparations

50 20

20

Radionuclides: Cesium– 137, Strontium –90

Pesticides (OPC,

carbamates and others)

Chicken eggs, and

egg products,

etc.


etc.

Spectrometry, radiometry

GC, GC-МS




-

-



ELISA

GC HPLC

GC-MS HPLC-

MS

-

Non-admissible

182

Table 17. List of control parameters for the state veterinary monitoring of residues of drug preparations, banned and toxic substances for veterinary

laboratories in the Russian Federation, 2013 (rabbits)

Group of substances according to 96/23/ЕС April 29, 1996

Number of samples




Screening methods

Confirma-tion

methods


Detection limit of the confirma-

tion method μg/kg

Admissib-le levels

(standards)

А


50

50 50

Diethylstilbestrol, Hexestrol, Dienestrol 19-Nortestoterone, Trenbolone, Methyltestoterone, Acetylgestagen, including Medroxyprogesteron, acetate Melengestrol acetate Ethinylestradiol Trenbolone acetate Testosterone,

Biomaterials, etc.

ELISA GC-МS

ELISA GC-МS

GC-МS

GC-МS

0.25 –2.8

μg/kg 0.1 –0.5 μg/kg

0.25 –2.8 μg/kg

0.1 –0.5 μg/kg

0.1 –0.5 μg/kg

- // -

- // -

Non-admissible Non-admissible Biochemical standards of natural level

183

А


See above 50

Progesterone, Oestradiol -17 Zeranol Clenbuterol, Salbutamol, Terbutaline, Mapenterol, Cymbuterol, etc.

Biomaterials, etc.

ELISA GC-МS

ELISA GC-МS

- // -

- // -

- // -

0.25 μg/kg

0.5 μg/kg

0.05 μg/kg

0.25-2.8 ng/g

0.25 –2.8 μg/kg

0.1 –0.5 μg/kg

0.25 –2.8 μg/kg

0.1 –0.5 μg/kg

- // -

- // -


184


50

50

20


Biomaterials, etc.

ELISA, HPLC- MS-MS

ELISA, HPLC- MS-MS

HPLC- MS-MS

0.25 mg/kg

0.1 μg/kg 0.2 μg/kg 0.25-1.0 μg/kg

0.25-1.0 μg/kg

GC-МS HPLC-MS-

МS

HPLC-MS-МS

HPLC-MS-МS

0.2 μg/kg

0.25 –1.0 μg/kg

0.25-1.0 μg/kg



50

Tetracycline (Oxytetracyclin, Methacyclin, Doxycyclin), Bacitracin, Grisin, etc.

Biomaterials, etc.

HPLC Microbiological ELISA

HPLC-MS-МS

0.1-0.2 μg/kg

0.01 U/g 6.0 μg/kg 0.5-0.01 U/g

0.1-2.0 μg/kg

Non-admissible

185

Sulfonamides (sulfamethazine, sulfadimethoxine, sulfadiazine, etc. (at least 8 compounds)

ELISA (imp.) MS-MS HPLC

HPLC-MS-МS

20 μg/kg 1.0-10.0 μg/kg

1.0 –10.0 μg/kg

CU common requirements Decision No. 299

Fluoroquinolones (ciprofloxacine, enrofloxacine, etc.)


HPLC-MS-МS

10 μg/kg 0.1-10.0 μg/kg

0.1 –10.0 μg/kg

CU common requirements Decision No. 299

186

B

(В2a) Anthelmintics (B2c) Carbamates and pyrethroids

20

50


Biomaterials, etc.

HPLC-MS-МS

HPLC-MS-МS

CU CR, Dec. No. 299.

Carbamates: Thiram (TMTD, tigam, tigam C, oftanol Т, raxil+TMTD, vitavax 200, vitavax 200 FF, vitatiuram, phenoram, chemicar Т, orlock Sevin (carbaril) Polycarbacin

Biomaterials, etc.

HPLC, colorimetric

GC HPLC-MS

GC-MS HPLC-MS

0.1-1.0 μg/kg

1.0-1.0 μg/kg

CU CR, Dec. No. 299.

187

B

(B2c) Carbamates and pyrethroids

50

Pyrethroids Alphamethrin Deltamethrin Permethrin Sumicidin (phenvalerat) Cypermethrin (Furi)

Biomaterials, etc.

GC, HPLC, HPLC- MS-MS

GC HPLC

GC-МS HPLC-MS-МS

0.5-5.0 μg/kg

0.5 –5.0 μg/kg

ADD-0.005 mg/kg ADD-0.003 mg/kg ADD – 0.035 mg/kg AL – 0.0015 mg/kg 0.0015 mg/kg

188


100 According to the registration and Annex

1a.

Biomaterials, etc.

HPLC-MS/MS

HPLC-MS/MS

CU CR, Dec. 299

189

В3

(В3a) Organo-chlorine compounds, including PCB (dioxins)

100

100

100

100

Aldrin Heptachlor


Biomaterials, etc.

GC GC-MS

- \\ -

- \\ -

- \\ -

GC-MS

0.1- 1.0 μg/kg

- \\ -

- \\ -

- \\ -

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

Non-admissible

Non-

admissible

0.1 mg/kg Meat

0.2 mg/kg Fat, etc 0.1 mg/kg Meat

1.0 mg/kg Fat, etc.

.

190

В3


10

2


Biomaterials, etc. .

GC-ECD

GC-МS

1.0 μg/kg (PCB-105)

10.0-15.0 (for sum of isomers)

0.0005 -

1.0 μg /kg

CU CR, Dec. No. 299 with annexes


Biomaterials, etc.

GC-HRMS

GC-HRMS

0.01 ng/kg TEQ WHO


50

Trichlormetafos-3

Heterophos

Diazinon (bazudin)


Biomaterials, etc.

GC

(NP) Enzymatic method (all

OPC including activated ones)

- // -

- // -

- // -

GC

(NP)

GC-МS

- // -

- // -

- // -

0.1- 50 µg in a sample

(0.001-100 µg in 0.1 ml sample),

lower detection limit 0.0001-0.001

µg

0.0005 – 1.0 µg /kg

- // -

- // -

- // -


191

В3


50

(dichlorvos) Dursban (chlorpyrifos) Karbofos (malathion) Metaphos (parathion-methyl, wofatox) Phosalone (phosalone) Phthalophos Antio Phosphamide Aktellik

Biomaterials, etc.

GC

(NP) Enzymatic

method ( all OPC including activated ones)

- // -

- // -

- // -

- // -

- // -

- // -

- // -

Per group

GC (NP)

GC-МS

(0.5-3.0 µg in a sample) (0.5-3.0 µg in

a sample)

See above

- // -

- // -

- // -

- // -

(10.0 μg/kg)

0.0005

-1.0 µg/kg

- // -

- // -

- // -

- // -

- // -

- // -

- // -

CU CR, Dec. No.299

192

B3

Temephos (abate)

- // -

- // -

193

Fat - 0.1 mg/kg

Arsenic

2.5 μg/kg - \\ - - \\ - 0.1 mg/kg – meat, fat 1.0 mg/kg

- offal Cadmium

20.0 μg/kg

- \\ - - \\ - 0.05 mg/kg –

meat 0.3 mg/kg

- offal 1.0 mg/kg - kidney

Mercury Screening

Color. Flameless AAS

2.5 μg/kg

Twice a year 5% of establishments per 1

sample

0.03 mg/kg-

meat, fat

0.1 mg/kg - offal 0.2 mg/kg -kidney

В3

(B3d) Mycotoxins

20 Ochratoxin А Zearalenon Other mycotoxins

Biomaterials, etc.

HPTLC, ELISA


2 μg/kg 0.25 μg

- // -

0.1 – 0.5 μg/kg

- // -

Non-admissible

- // -

194

В3



100

100

100

5

5

20

(Free choice)

for pesticides

and rodentcide

s

Nitrates Nitrites Organomercury compounds 2.4-D acid, salts and ethers Formaldehyde Rodenticides: Zoocumarin Glyfluor Crysid Indandion derivatives (ethylfenacin, etc.)

Radionuclide: Ceasium – 137, Strontium –90

Biomaterials, etc. Biomaterials etc.

Color.

Color.

GC

GC GC-MS

HPTLC GC

HPTLC

- \ \ -

- \ \ -

- \ \ - Spectrometry , radiometry

GC-MS

GC GC-MS

GC, GC-

МS, HPLC-MS-МS

Spectrometry, radiometry and radiochemistry

0.4 mg/kg

0.2 mg/kg

1. 0 μg/kg

1. 0 μg/kg

3 μg/kg

10 μg

0.3 mg/kg


3 μg/kg

MAL meat-50 mg/kg



Non-admissible

- \\ -

- \\ -

- \\ -

- \\ - CU CR, Dec. No. 299 with annexes

195

В3

(В3f) Other substances including unpatented

50


Criteria of parasite freedom

Unpatented drugs when their usage is

suspected

Bio-materials, etc.

CU CR, Dec. No. 299 with annexes GC-МS HPLC-MS/МS


GC-МS HPLC-MS-МS

- \\ -

CU CR, Dec. No. 299 with annexes Non-admissible

196

drugs

В3


100

100

Plumbum

Arsenic

Biomaterials, plasma and blood serum, hair.

IVA AAS

AAS AAS-ETA ICP-MS

50 μg/kg

0.01-1.0 μg/kg

0.5 mg/kg- meat

0.6 mg/kg- offal 1.0 mg/kg-kidneys 0.1 mg/kg- fat

IVA AAS

AAS AAS-ETA ICP-MS

2.5 μg/kg 0.01-1.0

μg/kg

0.1 mg/kg – meat and fat 1.0 mg/kg – offal

197

100

Cadmium

AAS AAS AAS-ETA ICP-MS

20 μg/kg

0.01-1.0

μg/kg

0.05 mg/kg - meat;

0.03 mg/kg -fat;

0.3 mg/kg –offal;

1.0 mg/kg -

kidneys

B3


100

Mercury

Biomaterials: blood serum and plasma, hair.

Color. flameless AAS

AAS –MHG AAS-ETA

2.5 μg/kg

0.01-1.0

μg/kg

0.03 mg/kg – meat and fat 0.1 mg/kg – offal 0.2 mg/kg – kidney.

5 5

Fluorine

Ionometry chem.

Ionometry chem.

3.0 mg 3.0 mg Biochemical standards

Selenium AAS, AAS-ETA, ICP-MS


10 μg/kg 10 μg/kg

198

20



Magnesium 1.0 μg/g 1.0 μg/kg

Manganese 0.1 μg/g 0.1 μg/kg


20

Cobalt Biomaterials: blood serum and plasma, hair



0.1 μg/kg

0.1 μg/kg

Biochemical standards



Zink 1.0 μg/kg 1.0 μg/kg

199

Table 18-19 List of control parameters for the state veterinary monitoring of residues of drug preparations, banned and toxic substances for Veterinary Laboratories in the Russian Federation for 2013 (game, including farmed game)٭

Group of substances


29.04.96

Number of samples


metabolites


of testing)

Screening methods

Confirmation

methods


screening method μg/kg


the confirma-

tion method μg/kg

Admissible levels

(standards)

А


100

100 100

Diethylstilbestrol, Hexestrol, Dienestrol 19-Nortestoterone, Trebolone, Methyltestoterone, Acetylgestagen, including Medroxyprogesteron, acetate Melengestrol acetate Ethinylestradiol Trenbolone acetate Testosterone, Progesterone, Oestradiol -17

Biomaterials, etc.

ELISA GC-МS

ELISA GC-МS

ELISA GC-МS

GC-МS HPLC-MS-

МS

GC-МS HPLC-MS-МS

- // -

0.1 –0.5 μg/kg

0.1 –0.5 μg/kg

0.25 μg/kg

0.5 μg/kg

0.05 μg/kg

0.1 –0.5 μg/kg

- // -

- // -

Non-admissible Non-admissible Biochemical standards of natural level

200

А


See above 100


Biomaterials, etc.

ELISA GC-МS

- // -

- // -

0.25-2.8 ng/g

0.1 –0.5 μg/kg

0.1 –0.5 μg/kg

- // -

- // -


201


100

100

100


Biomaterials, etc.

ELISA, HPLC- MS-MS

ELISA, HPLC- MS-MS

HPLC- MS-MS

0.25 mg/kg

0.1 μg/kg 0.2 μg/kg 0.25-1.0 μg/kg

0.25-1.0 μg/kg

GC-МS HPLC-MS-

МS (HPLC)

HPLC-MS-МS

HPLC-MS-МS

(HPLC)

0.2-0.25 μg/kg

0.25 –1.0

μg/kg

0.25-1.0 μg/kg



100

Tetracycline (Oxytetracyclin, Methacyclin, Doxycyclin), Bacitracin, Grisin, etc.

Biomaterials, etc.

HPLC Microbiological ELISA HPLC-MS-МS

HPLC HPLC-MS-МS

0.1-0.2 μg/kg 0.01 U/g 6-60 μg/kg 0.5-0.01 U/g

0.1-5.0 μg/kg

Non-admissible

202

Sulfonamides (sulfamethazine, sulfadimethoxine, sulfadiazine, etc. (at least 8 compounds)

ELISA (imp.) MS-MS HPLC

HPLC-MS-МS

20 μg/kg 1.0-10.0 μg/kg

1.0 –10.0 μg/kg

CU Common Requirements Decision No.299

Fluoroquinolones (ciprofloxacine, enrofloxacine, etc.)


HPLC-MS-МS

10 μg/kg 0.1-10.0 μg/kg

0.1 –10.0 μg/kg


203

B

(В2a) Anthelmintics (В2b) Coccidiostats

26

26

160

According to the registration and usage in holdings (free choice)

Biomaterials, etc.

HPLC-MS-МS

HPLC-MS-МS


Carbamates: Tiram (TMID, tigam, tigam C, oftanol Т, raxil+TMID, vitavax 200, vitavax 200 FF, vitatiuram, phenoram, chemicar Т, orlock Sevin (carbaril) Polycarbacin

Biomaterials, etc.

HPTLC, colorimetric HPLC-MS-

МС

HPLC HPLC-MS/МS

0.1-1.0 μg/kg

0.1-1.0 μg/kg


204

B

(B2c) Carbamates and pyrethroids

160

Pyrethroids Alphamethrin Deltamethrin Permethrin Sumicidin (phenvalerat) Cypermethrin (Furi)

Biomaterials, etc.

GC

HPLC, GC-MS HPLC- MS-MS

GC

HPLC GC-МS HPLC-MS-МS

0.5-5.0 μg/kg

0.5 –5.0 μg/kg

ADD-0.005 mg/kg ADD-0.003 mg/kg ADD – 0.035 mg/kg AL – 0.0015 mg/kg 0.0015 mg/kg

205


250 (В2е – 10)

According to the registration

Biomaterials, etc.

HPLC-MS

HPLC-MS CU Common Requirements Decision No.299

206

В3


300

300

300

300

Aldrin Heptachlor Hexachlorocyclohexane (α-,β-, γ- isomers) DDT and its metabolites

Biomaterials, etc.

GC GC-MS

- \\ -

- \\ -

- \\ -

GC-MS

0.1- 1.0 μg/kg

- \\ -

- \\ -

- \\ -

0.1-1.0 μg/kg

- \\ -

- \\ -

- \\ -

Non-admissible

Non-

admissible

0.1 mg/kg Meat

0.2 mg/kg Fat, etc 0.1 mg/kg Meat

1.0 mg/kg Fat, etc.

.

207

В3


100

50


Biomaterials, etc. .

GC-ECD GC-MS

GC-МS

1.0 μg/kg (PCB-105)

10.0-15.0 (for sum of isomers)

0.0005 -

1.0 μg /kg

CU CR Decision No. 299 with amendments.


Biomaterials, etc.

GC-HRMS

GC-HRMS

0.01 ng/kg TEQ WHO


250

Trichlormetafos-3

Heterophos

Diazinon (bazudin)


Biomaterials, etc.

HPTLC, Enzyme


GC (NP)

- // -

- // -

GC

(NP)

GC-МS

- // -

- // -

- // -

0.1- 50 µg in

a sample (0.001-100 µg

in 0.1 ml sample),

lower detection limit 0.0001-0.001

µg

(0.5-3.0 µg in

0.0005 – 1.0 µg /kg

- // -

- // -

- // -

CU CR Decision No. 299 with amendments.

208

В3


250

(dichlorvos) Dursban (chlorpyrifos) Karbofos (malathion) Metaphos (parathion-methyl,wofatox) Phosalone(phosalone) Phthalophos Antio Phosphamide Aktellik

Biomaterials, etc.

- // -

GC (NP)

HPTLC, Enzyme

method ( all OPC

including activated

ones) - // -

- // -

- // -

- // -

- // -

- // -

- // -

Per group

GC (NP)

GC-МS

a sample) (0.5-3.0 µg in

a sample)

See above

- // -

- // -

- // -

- // -

(10.0 μg/kg)

- // -

0.0005- -1.0 µg/kg

- // -

- // -

- // -

- // -

- // -

- // -

CU CR Dec. No.299 with amendments.

209

B3


250

Temephos (abate) Chlorophos Cyodrin (crotoxiphos) Dibrom Coumaphos (coral) Others

Biomaterials, etc.

- // -

HPTLC, Enzyme


- // - - // -

- // -

Per group

GC (NP)

GC-MS

0.1- 50 µg in

a sample (0.001-100 µg in 0.1 ml of a

sample), lower

detection limit 0.0001-0.001

µg

- // -

Per group

0.0005 -

1.0 µg /kg

CU CR, Dec. No.299 with amendments.

210

Fat - 0.1 mg/kg

Arsenic

2.5 μg/kg - \\ - - \\ - 0.1 mg/kg – meat, fat 1.0 mg/kg

- offal Cadmium

20.0 μg/kg

- \\ - - \\ - 0.05 mg/kg –

meat 0.3 mg/kg

- offal 1.0 mg/kg - kidney

Mercury Screening

Color. Flameless AAS

2.5 μg/kg

Twice a year 5% of establishments per 1

sample

0.03 mg/kg-

meat, fat

0.1 mg/kg - offal 0.2 mg/kg -kidney

В3

(B3d) Mycotoxins

Free choice

Ochratoxin А Zearalenon Other mycotoxins

Biomaterials, etc.

HPTLC, ELISA


2 μg/kg 0.25 μg

- // -

0.1 – 0.5 μg/kg

- // -

Non-admissible

- // -

211

В3



200

200

100

50

20

(Free choice)

for pesticides

and rodent-cides

Nitrates Nitrites Organomercury compounds 2.4-D acid, salts and ethers Rodenticides: Zoocumarin Glyfluor Crysid Indandion derivatives (ethylfenacin, etc.)

Radionuclides: Ceasium – 137, Strontium –90

Biomaterials, etc. Bio-materials etc.

Color.

Color.

GC

GC-MS

GC GC-MS

HPTLC GC - \ \ -

- \ \ -

- \ \ - Spectro-metry ,

GC-MS

GC-MS

GC, GC-

МS, HPLC-MS-МS

Spectrometry, radio-metry

0.4 mg/kg

0.2 mg/kg

1. 0 μg/kg

1. 0 μg/kg

10 μg

0.3 mg/kg

1. 0 μg/kg

1. 0 μg/kg

MAL meat-50 mg/kg


CU CR, Dec. No. 299

Non-admissible

- \\ -

- \\ -

CU CR, Dec. No. 299 with amendments

212

В3

(В3f) Other substances including

50


Criteria of freedom from parasite

Unpatented drugs when their usage is

suspected

Bio-material etc.

radio-metry CU CR, Dec. No. 299 GC-МS HPLC/MS-МS

and radio-chemistry CU CR, Dec. No. 299 GC-МS HPLC-MS/МS

- \\ -

CU CR, Dec. No. 299 with amendments Non-admissible

213

unpatented drugs

В3


300

(150+150)

Plumbum

Biomaterials, blood serum and plasma, etc.

IVA AAS

AAS AAS-ETA ICP-MS

50 μg/kg

0.01-1.0 μg/kg

0.5 mg/kg- meat

0.6 mg/kg- offal 1.0 mg/kg-kidneys 0.1 mg/kg- fat

IVA AAS

AAS AAS-ETA

2.5 μg/kg 0.01-1.0

0.1 mg/kg – meat and fat

214

300 (150+150)

300 (150+150)

Arsenic

Cadmium

ICP-MS μg/kg 1.0 mg/kg – offal

AAS AAS AAS-ETA ICP-MS ICP-MS

20 μg/kg

0.01-1.0

μg/kg

0.05 mg/kg - meat;

0.03 mg/kg -fat;

0.3 mg/kg –offal;

1.0 mg/kg -

kidneys

B3


300

(150+150)

Mercury

Biomaterials, blood serum and plasma, etc.

Colorimetry flameless AAS

AAS –MHG AAS-ETA ICP-MS

2.5 μg/kg

0.01-1.0

μg/kg

0.03 mg/kg – meat and fat 0.1 mg/kg – offal 0.2 mg/kg – kidney

50

Fluor

Ionometry chem.

Ionometry chem.

3.0 mg 3.0 mg Biochemical standards

215

50

Selenium AAS, AAS-ETA, ICP-MS


10 μg/kg 10 μg/kg

50



Magnesium 1.0 μg/g 1.0 μg/kg

Manganese 0.1 μg/g 0.1 μg/kg


20

Cobalt Biomaterials, blood serum and plasma, hair



0.1 μg/kg

0.1 μg/kg

Biochemical standards



Zink 0.1 μg/kg 0.1 μg/kg

216

Plan for state veterinary monitoring for residues of drugs, banned and toxic substances for Veterinary Laboratories of the Russian Federation for 2013 (Honey) Table 20

Groups of substances according to

96/23/ЕС of 29.04.96

Number of tested samples

Name of the product (active

substance)

Type of product

(object of testing)

Screening method

Confirma-tion

methods

Detection limit for


Detection limit for the confirma-

tion method

Admissible levels

(standards)

(А) (А6) Substances included in Table 2 of Annex 37/10 (EU)

300

300

Chloramphenicol (Levomycetine, CAP) Nitrofurans and metabolites: (AOZ, AMOZ, SEM, AHD)

Honey ELISA HPLC-MS-MS ELISA HPLC-MS-MS

GC-МS HPLC MS-MS

HPLC-MS-МS

0.05 μg/kg

100 ng/kg (АОZ), 200 ng/kg (АМОZ) 0.5-1.0 μg/kg

0.3 µg/kg

0.5-1.0 μg/kg

Non-admissible

Non-admissible

217

(В)

(В1) Antibacterial substances including sulfanilamides and quinolones

1,000

Antibiotics: Tetracycline Oxytetracycline, Metacycline, Doxycycline Streptomycin , Dihydrostreptomycin Penicillin and etc.

Honey HPLC HPLC-MS-MS HPLC micro-biological ELISA (imp.)

HPLC-MS-МS

0.25-5.0 µg/kg

0.05 mg/kg 0.5-0.01 U/kg

strepto-micin - 20

µg/l, dihydro-streptomycin – 14 µg/l

.

0.25-5.0 µg/kg

Non-admissible

(В) (В1) 500

Sulfanilamides: (sulfamethazine, sulfadimethoxine, sulfadiazine, etc. (at least 8 compounds)

Honey ELISA (HPLC)

HPLC

HPLC-MS-МS

1 µg/l

1.0-10.0

µg/kg

CU CR, Decision No.229

(В2) (В2с) Carbamates and pyrethroids

1,000

TMTD (tiram), sevin (carbaryl,

varroatin)

Honey HPTLC Colorimetry

GC GC-MS

1.0-100.0 µg/kg

0.1-1.0 µg/kg

CU CR, Decision No.229 with annexes

218

1,000

100

100

50

Pyrethroids

Honey Bees-Bio-materials

GC, GC-MS

GC, GC-MS

0.5-5.0 µg/kg

0.5-5.0 µg/kg


(В2f) Other pharmacologica

lly active substances

Formylic acid

Honey Titrimetric

5 mg/kg 500 mg/kg

Ethane diacid

Titrimetric

10 mg/kg

100 mg/kg

Phenothiazine (thiodiphenylamine) GC

HPLC-MS/MS

GC HPLC- MS/MS

0.5-5.0 µg/kg


219

(В3) (В3a) Organochlorine compounds, including PCB (dioxins)

1,000

1,000

20

1,000

1,000

300

100

20

Aldrin Heptachlor

Dylor (dehydrohepta-

chlor) Hexachlorocyclo-hexane (α-,β-, γ- isomers) DDT and its metabolites Other organochlorine compounds

Honey GC, GC-MS

GC-МS 0.5 µg/kg 0.1-1.0 µg/kg

0.1-1.0 µg/kg




Honey GC-ECD

GC-МS 1.0 µg/kg (for PCB-

105) 10.0-15.0 (for the sum of

isomers )

0.0005 -1,0 µg/kg


220


Honey

GC-HRMS

GC-HRMS

0.0005 µg/kg

221

(В3) (В3b) Organophosphorous compounds

500

500

500

500

500

500

200

500

50

500 500

500

Trichlormetaphos

-3 Heterophos

Diazinon (basudin)

DDVF (dichlorphos)

Dursban (chlorpiriphos)

Karbofos (malathion) Metaphos

(parathionmethyl) Fosalon (fosalon) Cianox

(cianofos) Antio

Phosphamide Phthalophos (phosmet)

Honey Bees - Bio-

materials

HPTLC, GC,

Enzymatic method HPLC- MS/MS

GC GC GC GC

GC GC

GC-МS HPLC- MS/MS

0.1-50 µg in a

sample, lower

limit of detection 0.0001-0.001 µg

0.0005 - 1,0 µg /kg


222

(В3) (В3d) Toxic elements

1,000

1,000

1,000 1,000

Plumbum Arsenic

Cadmium Mercury

Honey Stripping voltammetry,

AAS

AAS ETA

ICP-MS

50.0 µg/kg

2.5 µg/kg 20.0

µg/kg 2.5 µg/kg

0.01-1.0 µg/kg

1.0 mg/kg 0.5 mg/kg

0.05 mg/kg

- (В3) (В3f) Other

substances and environmental pollutants and unpatented drugs

1,000

50

100

1,000 (16,000)

1,000

(10,000)

If appro-

priate When

detected

Organomercury compounds (See.В3d) 2,4-D acid and ethers Other pesticides (Oximethylfur-furol) (Falsification) Radionuclides: Ceasium – 137, Strontium –90


Honey

HPTLC, GC

HPTLC

GC

Colorimetry

Organoleptic and chemical

tests

Spectro-metry ,

radiometry GC

GC-МS HPLC

GC GC-МS

- // -

GC/МS

- // -

- // -

-

GC-МS HPLC-MS

0.01 mg/kg

0.8-0.001

mg/kg -

0.3 mg/kg GOST method 19792-2001


Non-admissible

223

LIST OF ABBREVIATIONS

AAS – atomic absorption spectrometry (method) AAS-ETA – atomic absorption spectrometry and electrothermal atomization HPLC – high performance liquid chromatography HPTLC- high performance thin-layer chromatography HPLC-MS, HPLC-MS/MS – high performance liquid chromatography with mass spectrometric detection (including tandem spectrometry, etc.) HRGC-MS – high-resolution gas chromatography- mass spectrometry GC – gas chromatography (method) GC-MS – gas chromatography - mass spectrometry (gas chromatography with mass spectrometric detection) GOST - state standard HCCH - hexachlorocyclohexane DDT - 1,1,1-trichloro-2,2-bis (p-chlorophenyl) ethane DDD - 1,1-trichloro-2,2-bis (p-chlorophenyl) ethane DDE - 1,1-trichloro-2,2-bis (p-chlorophenyl) ethylene DDVP - 0,0-dimethyl-0-(2,2- dichlorovinyl)-phosphate AL - acceptable level ADD - acceptable daily dose ELISA - enzyme-linked immunosorbent assay ICP-MS - inductively coupled-plasma mass spectrometry MS – mass spectrometry MAL - maximum acceptable level FGBI NSCFAP – Federal Governmental Budgetary Institution «National Safety Centre for Fishery and Aquaculture Products» PCB - polychlorinated biphenyls MAC - maximum acceptable concentration ROSSELKHOZNADZOR - Federal Service for Veterinary and Phytosanitary Surveillance RF- Russian Federation POPs - persistent organic pollutants SanPin – sanitary and epidemiological rules and regulations MT-measurement tools TMTD - thiram, tetramethylthiuram disulphide OPC - organophosphorous compounds (pesticides) OCC- organochlorine compounds (pesticides)

for the state veterinary laboratory monitoring of residues of banned and harmful substances in live

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