Analytix Issue 3, 2011 - Water Determination in Milk and ... · PDF fileWater Determination in...

Issue 3 • 2011

AnalytixWater Determination in Milk and Milk Products

• Water Determination in

Dairy Products

• New UHPLC Solvents

• Salmonella Detection

• New Derivatization Reagents

• New Solvents for GC-Headspace

• Certified Reference Materials

• Reference Material for Herbal

Medicine

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Expanded Quality to Meet Your Analytical Needs – Introducing Cerilliant and Resource Technology Corporation (RTC), the two newest additions to Sigma-Aldrich

Dear Colleague,

In our eff orts to bring you the highest quality

and best of fering of analytical products,

Sigma-Aldrich would like to welcome our two

newest family members, Cerilliant Corporation

of Round Rock, Texas and RTC of Laramie,

Wyoming. The extensive capabilities of these

two companies complement Sigma-Aldrich’s

existing Fluka® and Supelco® analytical brands.

Cerilliant’s quality credentials include accred-

itation to ISO Guide 34 and ISO/IEC 17025, certi-

fi cation to ISO 9001:2008 and incorporation of

cGMP and GLP requirements into their everyday

activities. They are currently pursuing ISO

13485 and expect to receive their certifi cation

in early 2011. Cerilliant off ers over 2,800 products

and more than 30 years of expertise in the

design, development, synthesis, characterisation

and packaging of analytical standards, calibra-

tors, controls and certifi ed reference materials

for the pharmaceutical, clinical diagnostics,

forensic and clinical toxicology, nutraceutical

and environmental markets.

RTC is a premium manufacturer of Certified

Reference Materials (CRMs), Quality Control

(QC) Samples, and Proficiency Testing (PT)

Samples with more than 20 years of experience

and a strong expertise in the environmental as

well as in the pharmaceutical sector. RTC was

one of the original Proficiency Test providers

recognised by the US EPA. Its quality systems

include ISO/IEC 17025, ISO Guide 34 (CRMs),

ISO/IEC 17043 (PT) and ISO 9001:2000.

Add the outstanding expertise of Cerilliant and RTC to the

over 40 years of experience at Supelco and 60 years at Fluka

and you have an unmatched amount of knowledge and

products available for your laboratory needs. These compa-

nies will combine their talents and capabilities with those of

Sigma-Aldrich to create visionary approaches to supply the

analytical industry with a continually expanding list of new

products that meet the most rigorous quality requirements

including cGMP, GLP and ISO requirements.

Currently the products of Cerilliant and RTC are only avail-

able through Cerilliant and RTC themselves or one of

their distributors. Please contact them directly or visit

www.cerilliant.com or www.rt-corp.com to review

products, to ask a question or to place an order.

Kind regards,

Dr. Ingo Haag

Director Marketing

[email protected]

Dr. Ingo Haag

Director Marketing

Analytix is published fi ve times per year by Sigma-Aldrich Chemie GmbH,

MarCom Europe, Industriestrasse 25, CH-9471 Buchs SG, Switzerland

Publisher: Sigma-Aldrich Marketing Communications Europe

Publication director: Ingo Haag, PhD

Editor: Daniel Vogler

sigma-aldrich.com/analytix

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Standards

17 DAIH- and DNPH- Aldehyde and Ketone

Standards

19 New Analytical Standards for the Analysis of

Herbal Medicinal Products

21 New TraceCERT Organic Certified Reference

Materials

Titration

22 Volumetric Titration

VOLPAC® Solution Containers with new adapter

Feature Article

4 Water Determination in Milk and Milk

Products

Karl Fischer Titration with HYDRANAL® Reagents

Microbiology

8 Salmonella’s Tricks and their Detection

Derivatization

11 New Derivatization Reagents

Chromatography

12 UHPLC – State-of-the-Art in Chromatography Sigma-Aldrich introduces LC-MS Ultra CHROMASOLV®

16 New Headspace Grade Solvents

New Product Corner

15 New SELECTOPHORE® Ionophores with

Improved Properties

4

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Water Determination in Milk and Milk ProductsKarl Fischer Titration with HYDRANAL® Reagents

In the production of milk and dairy products, water content plays an important role,

technologically as well as economically. Therefore, national and international laws

and agreements protect and regulate the defi nition of products and the production

processes in dairy technology. Determining the water content in milk and milk pro-

ducts can be easily achieved with Karl Fischer (KF) titration.

Whole milk is a colloidal system composed of a continuous aqueous phase in which

lactose, whey proteins, and minerals are dissolved. The dispersed phase consists of

casein micelles and fat globules. Whole cow’s milk typically contains 90 g/kg of non-

fat solids and between 35 to 40 g/kg of fat. Both the fat globules and the casein

micelles contribute to the whiteness of milk by light scattering. Cream can be consi-

dered a concentrated dispersion of fat globules, while skim milk contains residual

milk fat of less than 0.1%.

Production of Milk and Milk products

An important step in the industrial production of milk products (Figure 1) is the

separation of milk into cream and skim milk. Cream can be considered as the fat part

of the milk, while skim milk is practically fat-free, containing water, milk proteins, and

lactose. Butter is made from cream, whereas buttermilk is the remaining liquid from

this process. Raw milk (or cream and skim milk combined as ingredients) is the basic

material for many other milk products, such as cheese, milk powder, condensed milk,

and fermented milk products.

Drinking Milk – Treatments and classification

The European Commission defi nes diff erent types of consumer milks:

• Raw milk has not been heated above 40 °C

• Whole milk has been heat-treated (pasteurized or sterilized)

Pasteurization is used to destroy all pathogenic micro organisms in milk. The so-called

continuous high-temperature short-time (HTST) procedure prescribes a rapid heating

of the milk to temperatures from 71-74 °C, and holding the product at this temperature

for 15 to 20 seconds.

Sterilization of milk can be achieved by Ultrahigh Temperature heating (UHT). The

characteristic temperature range for UHT heating is 135-150 °C with holding times of

a few seconds. The goal of UHT processing is to accomplish a sterile product storable

at ambient temperature. This heat treatment destroys all microorganisms and the

product is then packaged aseptically into sterile, hermetically sealed packages.

Andrea Felgner, Product Manager Analytical Reagents [email protected]

Thomas Wendt, HYDRANAL Technical Service [email protected]

Figure 1 Production steps of milk and milk products

Drinking Milk

Buttermilk

Butter

Cheese Milk Powder Condensed Milk

Whey

Milk ProteinsSkim MilkCream (Fat)

Raw Milk Drinking Milk

Lactose

Fermented / Cultured Milk Products

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(continued on page 6)

EU Regulation USA Regulation

Non-standardized whole milkUnchanged fat content, not less than 3.5%

Whole milkMinimum fat content of 3.25%

Fat-adjusted whole milkModified fat content, not less than 3.5%

(actual content indicated on the package)

Reduced-fat milkFat content of 2%

Partially skimmed milkAdjusted fat content of 1.5%-1.8%

Low-fat milkFat content of 1%

Skim milkFat content of maximum 0.5%

Skim milkFat content maximum 0.5% (may be called “fat free”)

Table 2 Classification of Drinking Milk (EU and USA)

Product Milk fat content Water content Milk protein in milk solids-not-fat

Cream powder Min. 42% m/m

Max. 5% m/m Min. 34% m/m

Whole milk powder Min. 26% m/m

Max. 42% m/m

Partly skimmed milk powder Min. 1.5% m/m

Max. 26% m/m

Skimmed milk powder Max. 1.5% m/m

Table 3 Composition of milk powders

Other Milk Products

Evaporated / Condensed Milk is produced through the con-

centration and drying of milk. These processing steps lead

to products with a smaller volume and a longer shelf life. To

further enhance the shelf life of these products, heat treat-

ment for sterilization can be applied.

The partial removal of water from milk or cream leads to

production of milk powder or cream powder. The fat and/

or protein content of the milk or cream may be adjusted by

the addition and/or withdrawal of milk constituents. The

accurate control and adjustment of a precise value of water

content is especially signifi cant for milk powders (Table 3).

Application

Water determination in coffee cream, quark

(cheese), milk, milk powder, yoghurt

Milk consists mainly of water; therefore, its water content

determination is straightforward. All of these products

release their water easily in the working medium of the KF

titration; the determination can be carried out with classical

KF reagents. However, it is very often necessary to take into

account the inhomogeneous water distribution or separa-

tion of components during storage. A homogenization

before taking the sample is recommended, especially for

quark and yoghurt. For titration of milk powder, a heating of

the reagents to 50 °C may be benefi cial. Since milk powder

at this temperature releases its water content only slowly,

the determination can be accelerated at higher tempera-

tures. Milk powder with especially high fat content may

need the addition of chloroform to the working medium to

improve the solubility of the sample. Coulometric KF titra-

tion is not recommended for these samples.

Sample sizes and dosage:

Coff ee cream 0.1 g / syringe with needle

Milk 0.05 g / syringe with needle

Milk powder 1.0 g / powder funnel

Quark 0.1 g / syringe without needle

Yoghurt 0.1 g / syringe without needle

Volumetric KF technique

Reagent One-component technique

Titrating agent HYDRANAL®-Composite 5

Working medium HYDRANAL-Methanol Rapid or

HYDRANAL-Methanol dry

Reagent Two-component technique

Titrating agent HYDRANAL-Titrant 5

Working medium HYDRANAL-Solvent

Product Water Protein Fat Carbohydrates Organic acids Minerals

Whole milk 87.7% 3.3% 3.6% 4.6% 0.2% 0.7%

Fat-reduced milk 89.6% 3.4% 1.6% 4.6% 0.2% 0.7%

Skim milk 90.9% 3.5% 0.1% 4.8% 0.2% 0.8%

Buttermilk 91.2% 3.5% 0.5% 4.0% 0.8% 0.8%

Whey (sweet) 93.6% 0.8% 0.2% 4.7% 0.3% 0.6%

Condensed milk 74.7% 6.5% 7.6% 9.2% 0.3% 1.5%

Coffee cream 81.7% 3.1% 10.5% 4.1% - 0.6%

Table 1 Nutritional composition of milk products

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Application

Water determination in cheese

Cheese does not dissolve in methanol and therefore does

not release its water content in classical KF solvents. The

addition of formamide to the working medium as a solubil-

izer is necessary; carrying out the titration at elevated tem-

peratures is also recommended. The sample should be

finely grated or cut into small pieces; this type of sample

will give a turbid solution with the working medium after

stirring for 5-10 minutes; the following titration should take

about 2-3 minutes (sample size 0.2 g / powder funnel).

Coulometric KF titration is not recommended for this

sample.



Titrating agent HYDRANAL®-Composite 5

Working medium HYDRANAL-Methanol dry/Rapid and

HYDRANAL-Formamide dry 1:1

Two-component technique


Working medium HYDRANAL-Solvent and


Application

Water determination in ice cream

The sample should be melted and carefully homogenized

before the analysis. To improve the dissolution of the fat

content, the titration should be carried out in HYDRANAL-

LipoSolver CM, which contains chloroform (sample size

0.05 g / syringe without needle). Coulometric KF titration is

not recommended for this sample.



Titrating agent HYDRANAL-Composite 5

Working medium HYDRANAL-LipoSolver CM (or

HYDRANAL-Methanol dry/Rapid and

HYDRANAL-Chloroform 1:1)



Working medium HYDRANAL-Solvent CM (or

HYDRANAL-Solvent and

HYDRANAL-Chloroform 2:1)

Application

Water determination in whey fat emulsion

This product may coat the electrodes in the titration cell.

Fading end-points and erroneously high results are the

consequences of this interference. The addition of form-

amide to the working medium can prevent this interference,

while addition of chloroform is necessary to dissolve the fat

of the sample (sample size 0.1 g / syringe without needle).

Coulometric KF titration is not recommended for this

sample.




Working medium HYDRANAL-Methanol dry and

HYDRANAL-Chloroform and

HYDRANAL-Formamide dry 1:1:1




HYDRANAL-Chloroform and

HYDRANAL-Formamide dry 2:1:1

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Application

Water determination in whey powder

In our investigations, this sample showed a small side reaction

with iodine. These reactions are often pH-dependent;

HYDRANAL®-Buff er Base or a working medium containing a

portion of salicylic acid helps to suppress this secondary re-

action. A titration at elevated temperatures enhances the side

reaction and is therefore not recommended. To dissolve the

high lactose content contained in the sample, the addition

of formamide is also necessary (sample size 0.5 g / powder

funnel). Coulometric KF titration is not recommended for

this sample.




Working medium HYDRANAL-Buffer Base (or

HYDRANAL-Methanol dry/Rapid and 5 g

HYDRANAL-Salicylic acid) and





HYDRANAL-Formamide dry 2:1 plus 5 g

HYDRANAL-Salicylic acid

Application reports (available upon request from

[email protected]):

L074 Quark (cheese)

L077 Whey fat emulsion

L081 Milk powder (whole milk)

L082 Milk powder (skimmed milk)

L085 Milk

L095 Cheese

L097 Yoghurt

L222 Coff ee cream

L493 Whey (powdered)

L523 Ice cream

Cat. No. Description

Volumetric one-component reagents

34805 HYDRANAL-Composite 5



34741 HYDRANAL-Methanol dry

37817 HYDRANAL-Methanol Rapid

34734 HYDRANAL-CompoSolver E

37855 HYDRANAL-LipoSolver CM

Volumetric two-component reagents

34732 HYDRANAL-Titrant 5 E

34723 HYDRANAL-Titrant 2 E

34801 HYDRANAL-Titrant 5

34811 HYDRANAL-Titrant 2

34730 HYDRANAL-Solvent E

34800 HYDRANAL-Solvent

34812 HYDRANAL-Solvent CM

Auxiliary Reagents (Solubilizers)

37863 HYDRANAL-Chloroform

34724 HYDRANAL-Formamide dry

37865 HYDRANAL-Salicylic acid

34804 HYDRANAL-Buffer Acid

37859 HYDRANAL-Buffer Base

Water standards for titer determination

34849 HYDRANAL-Water Standard 10.0

34696 HYDRANAL-Standard sodium tartrate dihydrate

Table 4 Selected Fluka brand HYDRANAL Karl Fischer reagents

References

[1] Jost, R. Milk and Dairy Products. Ullmann’s Encyclopedia of

Industrial Chemistry, 2007.

[2] Lebensmitteltabelle für die Praxis. Editor: Deutsche

Forschungsanstalt für Lebensmittelchemie, Garching bei

München. Wissenschaftliche Verlagsgesellschaft Stuttgart,

2009.

[3] Codex Alimentarius “Codex standard for milk powders and

cream powder”. CODEX STAN 207-1999. FAO/WHO.

Sigma-Aldrich off ers over 650 application reports. A full list of these reports and all HYDRANAL products can be found

on our website sigma-aldrich.com/hydranal To obtain an application report, please contact one of our HYDRANAL laboratories:

Europe and Global Market

Mr. Thomas Wendt

Technical Service HYDRANAL

D-30926 Seelze, Germany

Tel.: +49 (0) 5137 8238-353

Fax: +49 (0) 5137 8238-698

E-Mail: [email protected]

USA and Canada

Mr. Doug Clark

HYDRANAL Technical Center

St. Louis MO 63103, USA

Toll free: +1 800 493-7262 (USA and Canada)

Fax: +1 314 286-6699

E-Mail: [email protected]

8

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The media used currently for the diff erentiation and identi-

fication of Salmonella are still based on the detection of

carbohydrate fermentation indicated by a pH indicator (see

Table 2 for carbohydrate fermentation ability), the detec-

tion of proteolytic activity, hydrogen sulphide production

and selectivity. Most modern media also combine aspects

of this detection system to make the media more reliable. A

listing of the most common selective and diff erential media

appears in Table 3. For a typical microbiological control

procedure, please see the ISO method illustrated in Figure 2.

In addition, Sigma-Aldrich’s innovative technology has

developed a line of chromogenic media products which

make identifi cation even more reliable and faster as they

detect a characteristic enzyme of Salmonella. These reac-

tions are based on the cleavage of a chromogenic substrate

which results in a visible color change (see Table 4).

New deadly tools of Salmonella have been discovered, presenting opportunities for novel approaches in controlling Salmonella outbreaks.

Salmonella has the “know how” and the tools to invade into

the metabolism of host cells. In a new study, researchers

detected a bacterial sorting platform (bacterial type III pro-

tein secretion system) that organised the necessary pro-

teins. A key role of this cytoplasmic sorting platform is to

line up the secretion of proteins in a specific order to be

able to take control of the host cell’s function. The platform

uses customized chaperones to organise the type III protein

secretion. It organises the building up of a needle complex

through which the eff ector proteins can later be injected

into the host cells. These new fi ndings may introduce new

opportunities for novel antimicrobial strategies [1].

Salmonella contamination is the second leading cause of

food-borne illness worldwide. Controlling outbreaks of

Salmonella is an important task for food regulators, restau-

rants and the food industry in general.

The Salmonella family includes over 2,300 serotypes of bacte-

ria. However, two types, Salmonella enteritidis and Salmonella typhimurium, are responsible for approximately half of all

infections in humans. Most outbreaks of Salmonella may be

traced back to dairy, poultry and meat products; however,

Salmonella can grow on nearly any food. Chicken, eggs and

their derivative products pose a particularly high risk.

Kingdom: Bacteria

Phylum: Proteobacteria

Class: Gamma Proteobacteria

Order: Enterobacteriales

Family: Enterobacteriaceae

Genus: Salmonella

Table 1 Scientific classification

Microbiological control in the food industry plays a critical

role in preventing Salmonella outbreaks. Tests and media

used for the identifi cation of Salmonella take advantage of

unique aspects of Salmonella’s physiology or biochemistry

relative to other genera within the family Enterobacteriaceae.

For example, bacteria from the genus Salmonella are primarily

facultative anaerobes, oxidase-negative, catalase-positive

and Gram-negative rods. Most strains are motile and fer-

ment glucose with production of both acid and gas.

Salmonella’s Tricks and their Detection

Jvo Siegrist, Product Manager Microbiology [email protected]

Figure 1 Colorized scanning electron micrograph (SEM) revealing

the presence of a single Gram-negative Salmonella typhimurium

bacterium that has been isolated from a pure culture (Magnification

20000x; CDC - National Center for Zoonotic, Vector-Borne, and

Enteric Diseases (ZVED); Janice Haney Carr)

Non-selective pre-enrichment

Selective enrichment

Selective isolation

Confirmation

Sample

BPW

37 °C

18 hrs

RVS Broth

41.5 °C

24 hrs

MKTTn

37 °C

24 hrs

MSRV

41.5 °C

24 hrs

(48 hrs if

negative)

XLD

A second media of choice

Salmonella Chromogen Agar,

BGA, XLT4, Hektoen, SS, etc.

Biochemical Test

(e.g. TSI)

Annex D

Nutrient Agar

37 °C

24 hrs

Serological

08105 Buffered Peptone Water (ISO)

17173 Rappaport Vassiliadis Broth, modified

43052 Muller-Kauffmann Tetrathionate

Broth, Base (ISO)

92322 Rappaport Vassiliadis medium (base),

modified, semi-solid

95586 XLD Agar

01993 Salmonella Chromogen Agar Set

76721 XLT4 Agar (Base)

70116 Nutrient Agar No 2

92499 Triple Sugar Iron Agar (acc. to ISO)

51463 Urea Broth

66304 Lysine Decarboxylase Broth

62915 Lysine Iron Agar

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Carbohydrate Fermentation Cat. No. of Fluka

Carbohydrate DiscsAcid Gas

Adonitol - - 55876

Arabinose +/- +/- 80372

Cellobiose - - 56481

Dextrose + +/- 63367

Dulcitol +/- +/- 73044

Fructose +/- +/- 53901

Galactose + +/- 89608

Inositol +/- +/- 89614

Lactose - - 28816

Maltose + +/- 77653

Mannitol + +/- 94438

Mannose +/- +/- 94445

Melibiose + + 93196

Raffinose - - 94226

Rhamnose +/- +/- 93999

Salicin - - 92971

Sorbitol + +/- 93998

Sucrose - - 94309

Trehalose + +/- 92961

Xylose + +/- 07411

Table 2 Typical carbohydrate fermentation ability of Salmonella

Figure 2 Microbiology of food and animal foodstuffs — Horizontal method for the detection of Salmonella spp.; ISO 6579:2002/A1:2007


Figure 3 HiCrome™ MM

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Cat. No. Medium

Non-selective

pre-

enrichment

broth

08105 Buffered Peptone Water (ISO)

D3435 Dey-Engley Neutralizing Broth

70123 Nutrient Broth No. 2



17181 Nutrient Broth pH 6.9 without NaCl

77185 Peptone Water

94217 Peptone Water, phosphate-buffered

(ready-to-use media in the bottle)



with Ferrioxamine E

40893 Peptone Water, phosphate-

buffered, Vegitone

07507 Tryptone Water

(ready-to-use media in the bottle)

70194 Tryptone water

91366 Universal Pre-Enrichment Broth

Selective

enrichment

broth

69965 Mossel Broth

43052 Muller-Kauffmann Tetrathionate

Broth, Base (ISO)

04584 Rappaport Vassiliadis Broth acc. to

DIN EN ISO 6579:2002

17173 Rappaport Vassiliadis Broth,

modified

R0773 Rappaport Vassiliadis Medium

92322 Rappaport Vassiliadis medium

(base), modified, semi-solid

84370 Salmonella Enrichment Broth

70153 Selenite Broth (Base)

84922 Selenite Cystine Broth

86352 TBG Broth

88151 Tetrathionate Broth

Selective

confirmation

media

95388 Bismuth sulfite Agar

B1801 Brilliant Green Agar modified

70134 Brilliant Green Agar, modified

16026 Brilliant Green Phenol Red Lactose

Sucrose Agar

70135 DCLS Agar

90035 DCLS Agar No. 2

D7809 Deoxycholate Citrate Agar

51490 Hektoen Enteric Agar

61792 Leifson Agar

81648 Pril® Mannitol Agar

84368 Salmonella Agar according to Önöz

84369 Salmonella Chromogen Agar

01993 Salmonella Chromogen Agar Set

85640 SS-Agar

95586 XLD Agar

76721 XLT4 Agar (Base)

Cat. No. Medium

Growth and

purification

media


(ready to use media in the bottle)


N9405 Nutrient Agar pH 6.8

17209 R-2A Agar

17221 Tryptone Yeast extract Agar

Confirmation

media

A0715 Andrade Peptone Water

28943 Andrade Peptone Water, Vegitone

36408 Bromcresol Purple Broth

D2935 Decarboxylase Broth Base, Moeller

60787 Kligler Agar

66304 Lysine Decarboxylase Broth

62915 Lysine Iron Agar

39484 Methyl Red Voges Proskauer Broth

69150 Methyl Red Voges Proskauer Saline

Broth

M1053 Motility Test Medium

72548 Nitrate Broth

75315 OF Test Nutrient Agar

85438 SIM Medium

44940 Triple Sugar Iron Agar

92499 Triple Sugar Iron Agar (acc. to ISO)

51463 Urea Broth

Table 3 Salmonella selective and differential media

Brand Cat. No. Name

Fluka® 00563 HiCrome™ MM Agar

Fluka 90918 HiCrome RajHans Medium, Modified

Fluka 78419 HiCrome Salmonella Agar

Fluka 05538 HiCrome Salmonella Agar, Improved

Fluka 84369 Salmonella Chromogen Agar

Fluka 01993 Salmonella Chromogen Agar Set

Table 4 Chromogenic media for Salmonella

Reference:

[1] María Lara-Tejero, Junya Kato, Samuel Wagner, Xiaoyun Liu,

and Jorge E. Galán. A Sorting Platform Determines the Order

of Protein Secretion in Bacterial Type III Systems. Science,

3 February 2011.

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sigma-aldrich.com/derivatization

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New Derivatization Reagents

The primary use of derivatization

is the chemical modification of a

compound by derivatizing the

functional group (e. g. -OH, -COOH,

-NH, and -SH) to promote the use

of chromatographic analysis. If

lef t underivatized, these com-

pounds can demonstrate poor

chromatographic behavior, insuf-

fi cient volatility, and poor thermal

s tabi l i t y or have inadequate

detector response. By chemically

modifying these compounds into

derivatives, they gain properties

amenable for chromatographic

separation and accurate analysis.

With our broad p or t fo l io of

derivatization reagents, we at

Sigma-Aldrich demonstrate our

commitment towards seeking

new advancements and imple-

menting them in improved and

innovative products. Check out

our latest developments that will

e n a b l e y o u t o e x p e r i e n c e

imp rove d p er fo r man ce an d

achieve solutions for challenging

chromatography.

Brand Product Description Pack size

HPLC Derivatization enhanced sensitivity in electrochemical detection, analysis of steroids

FLUKA® 95159 Ferrocenecarboxaldehyde 100 mg

FLUKA 56257 Ferroceneboronic acid 100 mg

FLUKA 89111 N-Ferrocenyl-maleimide 100 mg

FLUKA 76737 3-Ferrocenylpropionic anhydride 100 mg

FLUKA 50203 Ferrocenoyl azide 100 mg

HPLC Derivatisation for primary amines and diamines

FLUKA 49558 2.6-Dimethyl-4-quinolinecarboxylic acid N-hydroxysuccinimide ester 100 mg

HPLC-UV Derivatization: synthesis of water-soluble prodrugs of lipophilic alcohols, phenols and amines

FLUKA 86546 Dibenzyl chloromethyl phosphate 1 g

Derivatization of non steroidal anti-inflammatory drugs

FLUKA 68768 N-Methyl-N-(trimethyl-d9-silyl)trifluoroacetamide 500 μL

Silylation for GC-Derivatization without solvent or excess of reagent

FLUKA 79271 Trimethylsilyl methallylsulfinate, for GC derivatization 5 mL

FLUKA 79264 Triethylsilyl methallylsulfinate, for GC derivatization 5 mL

FLUKA 79262 tert-Butyldimethylsilyl methallylsulfinate, for GC derivatization 5 mL

For further information, please visit sigma-aldrich.com/derivatization

Michael Kiselewsky, Product Manager Analytical Reagents [email protected]

Michael Jeitziner, Market Segment Manager Analytical Reagents & Standards [email protected]

12

sigma-aldrich.com/lc-ms

Ch

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y

obtained from a fast high throughput method using only a

short 2.1 x 5 mm Ascentis® Express C18 column. Although the

total run-time is only 1 min., all major matrix compounds are

separated from the analyte, which is necessary to optimize

the limit of detection and eliminate suppression effects. A

comparable separation on a standard HPLC system is not

possible or requires extensive modifi cations to the HPLC sys-

tem to minimize peak dispersion and loss of sensitivity.

Figure 2 shows the diff erence between a standard HPLC

column and a Supelco® Ascentis Express column with

Fused-Core particles. UHPLC or optimized HPLC systems

with core-shell particle columns are able to separate com-

pounds into very narrow fractions having high peak

responses from UV, MS or other detectors. This advantage

requires a very high and stable quality for solvents and

additives. Even a slight impurity may result in additional

peaks which may create a complicating issue with steep

and fast gradient runs (Figure 3).

Since the early 1940s, liquid chromatography has pro-

gressed through rapid development. Even in the earliest

publications, smaller packing particles and higher column

pressures were being proposed for greater separation effi -

ciencies and faster run-times. Years before the introduction

of a commercial Ultra High Performance Liquid Chromato-

graphy (UHPLC) system by Waters in 2004, V. Meyer pre-

sented in 1997 a fast chromatography of benzodiazepines

with nonporous 1.5 μm particles, and demonstrated the

advantages of increased chromatographic resolution and

speed [1]. At the present time, all major HPLC manufactur-

ers off er UHPLC systems for pressures up to 1200 bar and

minimized mixing in tubing connections and fittings.

Another major development focused on the improvement

of stationary phases. The combination of small solid mono-

disperse particles coated with a porous functionalized shell

(Fused-Core®) has led to outstanding column effi ciencies

and has opened up new techniques for standard HPLC and

UHPLC users, e.g. very fast separations on short columns. The

separation in Figure 1 represents well the clarity of results

UHPLC – State-of-the-Art in Chromatography Sigma-Aldrich introduces LC-MS Ultra CHROMASOLV®

Rudolf Köhling, LC-MS Application Scientist [email protected]

13


Ch

rom

ato

gra

ph

y

506.238

+=171.104 Da

test run_manual inj_1 ppm.d: BPC 49.000-1201.000 +All MS

test run_manual inj_1 ppm.d: EIC 171.103±0.01 +MS2(506.230)

test run_manual inj_1 ppm.d: EIC 506.235±0.01 +All MS

0.2 0.4 0.6 0.8 1.0 Time [min]0.0

0.5

1.0

1.5

2.0

2.5x104

Intens.

1

171.103

203.095

234.067

277.106 301.072 354.753

398.151

2.0

0

50

100

150

200

100 200 300 400

427.247452.198

500 600 700 m/z

O

S O 2

N

[M+H]+

Chemical Formula: C 30H3 NO 4S

161.082

189.104

229.119

270.128

298.096

351.149

409.164

460.209

1.

100

200

300

Intens.

134.067 546.399583.222 661.466

689.499

+MS, 0.4-0.5min #(60-75), -Peak Bkgrnd

+MS2(506.230), 1.8-1.8min #(260-274)

OH

0.0

0.2

0.4

0.6

0.8

1.0

x107

Intens.

0

2

4

6

x106

Intens.0 5 10 15 20 25 Time [min]

0 1 2 3 4 5 6 Time [min]

1

34

5

13

45

40 min run-time with conventional C18 column,

4.6x100 mm, 3.5 μm, 5 μL injection volume.

7.7 min run-time with Supelco Ascentis Express C18

2.1x50 mm, 2.7 μm, 0.6 μL injection volume(!)

Figure 2 BPC and UV traces of an in-process control sample. The use of Fused-Core® particles leads to much shorter run-times and less

sample and solvent consumption while maintaining peak resolution.

Figure 1 Estradiol can be derivatized with dansyl chloride (Fluka 39220) and detected by APCI as dansyl derivative [2]. Excessive reagent

can be separated from the analyte with a short Ascentis® Express C18 guard column cartridge (Supelco® 53501-5). Using UHPLC allows a

complete chromatography even with this short column (2.1 x 5 mm!). The analysis of 10 ppb estradiol resulted in a S/N=60 (MS and MRM).


1414


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Brand Product Name Description Pack size

Fluka 14261 Acetonitrile LC-MS Ultra CHROMASOLV, ≥99.9%, tested for UHPLC-MS 1 L, 2 L

Fluka 14262 Methanol LC-MS Ultra CHROMASOLV, ≥99.9%, tested for UHPLC-MS 1 L, 2 L

Fluka 14263 Water LC-MS Ultra CHROMASOLV, tested for UHPLC-MS 1 L, 2 L

Fluka 14264 Trifluoroacetic acid LC-MS Ultra eluent additive, ≥ 99.0% suitable for UHPLC-MS 1 mL, 2 mL

Fluka 14265 Formic acid LC-MS Ultra eluent additive, ≥ 98% suitable for UHPLC-MS 1 mL, 2 mL

Fluka 14266 Ammonium formate LC-MS Ultra eluent additive, suitable for UHPLC-MS 25 g

Fluka 14267 Ammonium acetate LC-MS Ultra eluent additive, suitable for UHPLC-MS 25 g

Table 1 New LC-MS Ultra CHROMASOLV solvents and LC-MS Ultra eluent additives.

Reference:

[1] Meyer, V. Praxis der Hochleistungs-Flüssigchromatographie, 1. Aufl., Wiley-VCH, Weinheim, 2004.

[2] Nelson, R. E., et al. Clinical Chemistry 2004, 50 (2), 373–384.

Figure 3 Standard gradient grade acetonitrile quality (blue) compared to our new LC-MS Ultra CHROMASOLV® Fluka® 14261 (red) under

equal conditions (gradient from 0 to 100% acetonitrile within 2 min). In both cases, LC-MS Ultra CHROMASOLV Water, Fluka 14263,

is used as aqueous phase.

In combination with very sensitive detection systems, e.g. UV

detectors with fi ber optics, focusing quadropols, or time-of-

fl ight or ion trap mass spectrometers, UHPLC sets new limits

for the purity of solvents and the additives used as mobile

phase buff ers. Generally, this is a much more challenging task

than the removal of particles.

-2.5

0.0

2.5

5.0

7.5

10.0

Intens.

[mAU]

-5.0

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 Time [min]

15

sigma-aldrich.com/selectophore

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New SELECTOPHORE® Ionophores with Improved Properties

Michael Jeitziner, Market Segment Manager Analytical Reagents & Standards [email protected]

The performance of chemical sensor devices depends on three “S” factors: Selectivity,

Sensitivity and Stability. The ionophore plays the most critical role in optimizing

these factors (see Figure 1). Sigma-Aldrich has successfully developed and intro-

duced many new ionophores with improved characteristics over previously existing

ones. The Fluka® branded ionophores are application tested using the electrode

body IS-561, Fluka 45137. Two examples of ionophores with improved properties are

listed below.

Magnesium Ionophore VI, Selectophore function tested, Fluka 63112

ETH 5506, 1,3,5-Tris[10-(1-adamantyl)-7,9-dioxo-6,10-diazaundecyl]benzene

This magnesium-selective ionophore is highly lipophilic

(log PTLC=8.5) and obtains sufficient selectivities for Mg2+

against the main interfering cations; therefore, it can be

used for magnesium measurement even in serum samples.

This ionophore has a linear response between 1•10-6 M and

6•10-2 M magnesium ion.

Nitrate ionophore VI, Selectophore function tested, Fluka 07295

(9-Hexadecyl-1,7,11,17-tetraoxa-2,6,12,16-tetraazacycloeicosane)

Nitrate ionophore VI is the best nitrate-selective ionophore

available. The PVC membrane stability is improved by this

ionophore due to the high lipophilicity of the hexadecyl

group (logP =8.3 (calc.)). The membrane obtains a linear

response between 5•10-6 M and 0.1 M nitrate ion.

Sensitivity

Selectivity

Stability

HN

HN

HN

N

N

OO

OO

N

OO

HN

O O

NH

O

HN

O

NH

C H2( C H2) 14C H3

N N H

N H N

N NH

N HN

N H

H N

O

O

ON

O

NC H3

C H3

Figure 1 Magic

Triangle: Key

Performance

Parameters of

Chemical Sensors

Figure 2 Magnesium ionophore VII

Figure 3 Nitrate ionophore VI

Figure 4 Lead ionophore VIII

Figure 5 Iron(III) ionophore VI

Lead ionophore VIII, Selectophore function tested,

Fluka 61796

This ionophore obtains excellent selectivity properties and

is therefore used within the diagnosis of clinical disorders as

well as in the monitoring of environmental samples.

Recommended Membrane Composition:

10.0 wt% Nitrate ionophore VI (07295)

46.0 wt% Dibutyl phthalate (80100)

0.5 wt% Tetraoctylammonium chloride (87985)

43.5 wt% Poly(vinyl chloride) high molecular weight (81392)

References:

63112 Magnesium ionophore VI O’Donnell, J., et al., Anal. Chim.

Acta 281, 129-134, 1993,

07295 Nitrate ionophore VI unpublished.

61796 Lead ionophore VIII W.-J. Zang et al., Analytical

Letters 40, 2007, 1023–35.

42942 Iron ionohore VI R. Maleki et al., Turk. J. Chem. 33,

2009, 1–10.

Iron ionophore VI, Selectophore function tested,

Fluka 42942

The new Iron(III) ionophore VI obtains an extended linear

range and superior selectivity properties. It can be there-

fore used for clinical analysis as well as for environmental

analysis.

Order a free copy of our guide on ”Selectophore – Ion Sensor Materials” at our

website: sigma-aldrich.com/selectophore or reply using the enclosed BRC.

16C

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sigma-aldrich.com/gc-hs

New Headspace Grade Solvents

Michael Kiselewsky, Product Manager Analytical Reagents [email protected]

When developing a GC-HS method, parameters such as

sample solvent, extraction temperature, extraction time,

sample volume and headspace volume are optimized.

Sigma-Aldrich has developed solvents specifi cally for GC-HS

applications. The purity and handling specifications for

these solvents meet the requirements of the European

Pharmacopoeia (Ph.Eur.) and United States Pharmacopeia

(USP), as well as ICH guidelines. The new GC-HS product line

includes water and three of the most commonly used

organic solvents: dimethyl sulfoxide (DMSO), N,N-dimethyl-

formamide, and N,N-dimethylacetamide. N,N-dimethylfor-

mamide and dimethyl sulfoxide are specifi ed in Ph.Eur. and

USP for water-insoluble substances. Water is the preferred

solvent for water-soluble solutions, as described in Ph.Eur.

and USP monographs. In addition, Sigma-Aldrich has now

expanded its GC-HS portfolio with two new products,

GC-HS Cyclohexane and 1-Methyl-2-pyrrolidinone.

All solvents are microfi ltered at 0.2 μm and packed under

inert gas for extended shelf life.

Literature

[1] United States Pharmacopeia, 31st Edition (2008), <467>

Residual Solvents.

[2] Ph.Eur. 6.0 (2008) Method 2.4.24, Identification and control

of residual solvents.

[3] ICH Guideline Q3C, Impurities: Guideline for Residual

Solvents, The Fourth International Conference on

Harmonization, July 17, 1997.

Cat. No. Brand Product Name Abbreviation BP Pack size

NEW 68809 Fluka® Cyclohexanone, for GC-HS - 155 °C 1 L

44901 Fluka N,N-Dimethylacetamide, for GC-HS DMA 166 °C 1 L

51781 Fluka N,N-Dimethylformamide, for GC-HS DMF 153 °C 1 L

67484 Fluka 1,3-Dimethyl-2-imidazolidinone, for GC-HS DMI 225 °C 100 mL, 1 L

51770 Fluka Dimethyl sulfoxide, for GC-HS DMSO 189 °C 1 L

NEW 69337 Fluka 1-Methyl-2-pyrrolidinone, for GC-HS NMP 202 °C 1 L

53463 Fluka Water, for GC-HS - 100 °C 1 L

Product table Solvents for GC Headspace Analysis

For more information, please visit our website: sigma-aldrich.com/gc-hs

Subscribe today to receive the Fluka eNewsletter Stay abreast of the latest innovations, applications, promotions and regional activities in analytical /

chromatography disciplines from Sigma-Aldrich by signing up for our electronic newsletter.

Our monthly Fluka eNewsletter brings you a brief compilation of product information, application tips, and

promotional off ers related to reagents and standards for

• Titration

• Spectroscopy

• Chromatography

• Microbiology

• Labware

• Monthly Savings

Sign up at sigma-aldrich.com/analytical_newsletter

17

sigma-aldrich.com/standards

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DAIH- and DNPH- Aldehyde and Ketone Standards

Ingrid Hayenga, Senior Chemist, R&D Europe [email protected]

The following table provides a summary of the most important derivatizing agents as well as their advantages

and disadvantages [2].

Reagents Analytical

method

Advantage Disadvantage Air sampling

techniquesa

2.4-Dinitrophenylhydrazine

(DNPH)

HPLC-UV,

HPLC-MS,

(GC-FID, CE)

International standard procedure; large

variety of applications available; reagents

and derivatives stable

Interferences with airborne

oxidants (Nox, O3); limited

sensitivity

I, Cb, D, PSD

Hantzsch reagent UV, fluorescence,

HPLC-UV,

HPLC-fluorescence

Well suitable for on-line analysis;

fluorescence detection

Slow and non-quantitative

reaction; limited to aliphatic

carbonyls

I, flow-through

analyzers

Chromotropic acid +

pararosaniline

UV/Vis Only readily available instrumentation

required

Suitable only for

formaldehyde

I

4-nitrophenyl-hydrazine

(pNPH)

HPLC-UV Slightly red-shifted absorption maxima

of the derivatives compared to the DNP-

hydrazones

Replaced by DNPH because

of its faster derivatization

reaction

C, I

Halogenated aromatic

hydrazines and

hydroxylamines

GC-ECD, GC-FID,

GC-MS

Improved chromatographic resolution

compared to HPLC

Slow reactions with

carbonyls; E and Z isomers

separated

C, I

N-methyl-benzothiazolon-

(2)-hydrazone (MBTH)

4-Amino-3-hydrazino-

5-mercapto-1,2,4-triazol

(Purpald)

UV/Vis, HPLC-UV Only readily available instrumentation

required

Selective for formaldehyde

but cross-selectivity to

other aldehydes

I

Dansylhydrazine (DNSH) HPLC-

fluorescence

Low limits of detection Instability of DNSH and

its derivatives towards

hydrolysis

C, I

N-Methyl-4-hydrazino-7-

nitrobenzofuran (MNBDH)

HPLC-UV,

HPLC-MS

Slightly faster reaction with carbonyl

compounds, higher selectivity and lower

detection limits compared to DNPH as well

as other N-alkylated hydrazine reagents

C, I, PSD

a: C = cartridge, I = impinger, D = denuder, PSD = passive sampling devices

b: reagent coated cartridges are commercially available

The most relevant DNPH- and DAIH-aldehyde and ketone standards are available at Sigma-Aldrich either as solutions or as

pure substances, as analytical standards or as BCR certifi ed reference materials.

Formaldehyde and acetaldehyde are key components of

photochemically generated air pollution. Oxidation of vola-

tile organic compounds (VOC) by reaction of OH radicals is

considered to be their predominant source, but they are

also emitted directly into the urban atmosphere during the

incomplete combustion of fossil fuels. It has been assumed

that these two important intermediate species account for

up to 90% of the total aldehydes in air [1].

For short chain aldehydes and ketones, a number of

derivatization reagents have been developed. Their detection

is performed by photometry or fl uorescence, e.g. reaction

with chromotropic acid or pararosaniline. These reactions

are valid if a sum parameter is to be obtained; however,

their major drawback is the inability to determine diff erent

carbonyls simultaneously within one sample.

The oxidative coupling of aldehydes with two molecules of

N-methyl-benzothiazolon-(2)-hydrazone (MBTH) leads to

an intensively colored product. Although it is possible to

determine dif ferent aldehydes and ketones with this

method, its selectivity depends heavily on the analyte

structure and the experimental conditions.

Therefore, to achieve speciation information, a chromato-

graphic separation is required. For atmospheric detection

of short chain aldehydes and ketones, the use of impreg-

nated silica-gel cartridges has provided good sensitivity,

the impregnating reagents being 2-diphenylacethyl-

12.3-indandione-1-hydrazone (DAIH) or 2.4-dinitrophenyl-

hydrazone (DNPH). These reagents are also applicable as

precolumn derivatizing reagents for liquid phase analysis. [2]


18S

tan

da

rds


Cat. No. Product Description Pack Size

47344 2-Butanone-2.4-DNPH solution 100 μg/ml in acetonitrile ampule of 1 ml

47340-U Acetaldehyde-2.4-DNPH solution 1000 μg/ml in acetonitrile ampule of 1 ml

4M7340-U Acetaldehyde-2.4-DNPH solution 1000 μg/ml in acetonitrile pkg of 5 ampules (1 ml each)

47341 Acetone-2.4-DNPH solution 1000 μg/ml in acetonitrile ampule of 1 ml

4M7341 Acetone-2.4-DNPH solutions 1000 μg/ml in acetonitrile pkg of 5 ampules (1 ml each)

47342 Acrolein-2.4-DNPH solution 1000 μg/ml in acetonitrile ampule of 1 ml

4M7258-U Aldehyde/ketone-DNPH TO11/IP-6A Mix 15 μg/ml each component in acetonitrile pkg of 3 ampules (1 ml each)

47343 Benzaldehyde-2.4-DNPH solutions 100 μg/ml ampule of 1 ml

47345-U Butyraldehyde-2.4-DNPH solution 1000 μg/ml ampule of 1 ml

47649-U CARB carbonyl-DNPH Mix 1 In acetonitrile (varied) ampule of 1 ml

47650-U CARB Method 1004 DNPH Mix 1 3 μg/ml in acetonitrile ampule of 1 ml

47651-U CARB Method 1004 DNPH Mix 2 2 μg/ml in acetonitrile ampule of 1 ml

47672-U Carbonyl DNPH Mix 1 20 μg/ml in acetonitrile ampule of 1 ml

47671-U Carbonyl DNPH Mix 2 2 μg/ml in acetonitrile ampule of 1 ml

47175-U Crotonaldehyde-2.4-DNPH solution 100 μg/ml in acetonitrile ampule of 1 ml

47674-U Cyclohexanone-2.4-DNPH solution 500 μg/ml in acetonitrile ampule of 1 ml

48149-U EPA TO-11A Six Component Carbonyl-DNPH Mix 15 μg/ml each component in acetonitrile pkg of 1.5 ml

47177 Formaldehyde-2.4-DNPH solution 100 μg/ml in acetonitrile ampule of 1 ml

47564-U Glutaraldehyde-2.4-DNPH solution 100 μg/ml in acetonitrile ampule of 1 ml

O

R 2R 1 O2N

N O2 HN

N H2

O2N

N O2 HN

N R 2

R 1

O

R 2R 1

NH 2N

O

O

NN

O

O

R 1 R 2

Figure 1 Derivatization of carbonyl compounds with 2.4-dinitrophenylhydrazone (DNPH)

Figure 2 Derivatization of carbonyl compounds with 2-Diphenylacetyl-1.3-indandione-1-hydrazone

Cat. No. Product Pack size

14423 Acetaldehyde DAIH derivative 50 mg

02819 Acetone, DAIH derivative 50 mg

13173 Acroleine, DAIH derivative 50 mg

55556 Crotonaldehyde, DAIH derivative 50 mg

91547 Cyclohexanone, DAIH derivative 50 mg

06947 Formaldehyde, DAIH derivative 50 mg

51299 Propionaldehyde, DAIH derivative 50 mg

442321-U 2.5-Dimethylbenzaldehyde

-2.4-DNPH

ampule of 100 mg

442339 2-Butanone-2.4-DNPH ampule of 100 mg

442434 Acetaldehyde-2.4-DNPH ampule of 100 mg

442436 Acetone-2.4-DNPH ampule of 50 mg

442441 Acrolein-2.4-DNPH ampule of 25 mg

442469 Benzaldehyde-2.4-DNPH ampule of 100 mg

442504 Butyraldehyde-2.4-DNPH ampule of 100 mg

442529 Crotonaldehyde-2.4-DNPH ampule of 100 mg

442533 Cyclohexanone-2.4-DNPH ampule of 100 mg

Table 1 DAIH- and DNPH – standards, pure substance

Cat. No. Product Description Pack

size

33852 Decanal 2.4-DNPH > 98.5% 10 mg,

100 mg

442597 Formaldehyde-2.4-DNPH ampule of

100 mg

33848 Heptanal 2.4-DNPH > 98.5% 100 mg

442614 Hexaldehyde-2.4-DNPH ampule of

100 mg

442639 Methacrolein-2.4-DNPH ampule of

100 mg

33851 Nonanal 2.4-DNPH > 98.5% 100 mg

33849 Octanal 2.4-DNPH > 98.5% 100 mg

442722 o-Tolualdehyde-2.4-DNPH ampule of

100 mg

442768 Propionaldehyde-2.4-

DNPH

ampule of

100 mg

442735 p-Tolualdehyde-2.4-DNPH ampule of

100 mg

34396 Succinaldehyde > 98.5% 50 mg

442834 Valeraldehyde-2.4-DNPH ampule of

100 mg


19


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New Analytical Standards for the Analysis of Herbal Medicinal Products

Matthias Nold, Product Manager Analytical Standards [email protected]

Herbal medicinal products, pharmaceutical products which

are derived from medicinal plants, are very popular as an

alternative to synthetic drugs. In recent years, regulatory

pressure for herbal medicinal products has increased,

resulting in the need for monitoring the concentrations of

active ingredients and other characteristic components.

Sigma-Aldrich off ers analytical standards as well as primary

reference standards of active ingredients and marker com-

pounds of medicinal plants. This portfolio of products con-

tinues to expand at a quick pace. Just as we presented

several new products in the fi rst two issues of Analytix in

2011, we are once again introducing new additions to this

rapidly growing product line.

Our webpage at sigma-aldrich.com/medicinalplants

contains an up-to-date listing of these products catalogued

not only by alphabetical order, but also according to sub-

stance class and by genus for a wide array of medicinal

plants.

Cat. No. Brand Description Pack Size

42251 Fluka® Apigenin 10 mg

91466 Fluka Betulinic acid 10 mg

43412 Fluka (+) Catechin 10 mg

95082 Fluka Chrysin 50 mg

06536 Fluka trans-Cinnamaldehyde 50 mg

97013 Fluka trans-Cinnamic acid 50 mg

38907 Fluka Isorhamnetin 10 mg

69545 Fluka Kaempferide 10 mg

96353 Fluka Kaempferol 10 mg

49968 Fluka Luteolin-7-glucoside 10 mg

06279 Fluka Mangiferin 10 mg

28660 Fluka Procyanidin A2 10 mg

16654 Fluka Quercetin 3-glucoside 10 mg

69686 Fluka Shikimic acid 50 mg

Table1 New analytical standards and certified reference materials

(CRMs) of active ingredients and marker substances for the analysis

of herbal medicinal drugs


47178-U Hexaldehyde-2.4-DNPH solution 1000 μg/ml in acetonitrile ampule of 1 ml

47886 Isobutyraldehyde-2.4-DNPH solution 100 μg/ml in acetonitrile ampule of 1 ml

47179 Isovaleraldehyde-2.4-DNPH solution 1000 μg/ml in acetonitrile ampule of 1 ml

47180-U Methacrolein-2.4-DNPH solutions 100 μg/ml in acetonitrile ampule of 1 ml

47183 m-Toluoaldehyde-2.4-DNPH solution 100 μg/ml in acetonitrile ampule of 1ml

47032-U o-Phthaldialdehyde-(DNPH)2 solution 10 μg/ml in acetonitrile:DMSO (7:3) pkg of 3x2 ml

47182 o-Tolualdehyde-2.4-DNPH solution 100 μg/ml ampule of 1 ml

47181 Propionaldehyde-2.4-DNPH solution 1000 μg/ml ampule of 1 ml

47184-U p-Tolualdehyde-2.4-DNPH solution 100 μg/ml ampule of 1 ml

40117-U Pyridine-2-Aldehyde-DNPH Standard in acetonitrile pkg of 3x2 ml

40081-U Pyridine-4-Aldehyde-DNPH solution 1mM in acetonitrile:DMSO, 4:1 pkg of 3x2 ml

47285-U TO11/IP-6A Aldehyde/Ketone-DNPH Mix 15 μg/ml each component in acetonitrile ampule of 1 ml

47185-U Valeraldehyde-2.4-DNPH solutions 100 μg/ml ampule of 1 ml

Table 2 DAIH- and DNPH-standards, in solution and mixes


BCR5512 2.4-Dinitrophenylhydrazones, solutions Set of 4x BCR-551 and 1x BCR-552 (blank) set

BCR548 Acrolein-2.4-DNPH 10 mg

BCR5534 Formaldehyde-2.4-DNPH on filter Set of 2x BCR-553 and 1x BCR-554 (blank) set

BCR550 Glutaraldehyde 2.4-DNPH 10 mg

Table 3 BCR certified reference material

References:

[1] Possanzini, M., Di Palo, V. Chromatographia 1997, 46, 5/6, 235.

[2] Vogel, M., Büldt, A., Karst, U., Fresenius, J. Analy. Chem. 2000, 366, 781.

20

sigma-aldrich.com/csp

Sta

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Inorganic Custom StandardsAn Interactive Online Platform

TraceCERT® standards for AAS, ICP and IC are Certifi ed

Reference Materials fulfi lling the highest-quality standards.*

In addition to our comprehensive portfolio of catalogue

products we also off er you a custom service where you

can defi ne your own multi-component standards at the

same high quality, using our Inorganic Custom Standards

Online Platform:

sigma-aldrich.com/csp

For all TraceCERT Custom Standards we guarantee:

• Certification under double accreditation following

ISO/IEC 17025 and ISO Guide 34

• Highest level of accuracy and reliability

• Minimized uncertainties and lot-specific values

• Traceability to at least two independent references

(i.e. NIST, BAM or SI unit kg)

• Printed certificate according to ISO Guide 31

• Light- and gas-tight aluminium foil bag packaging

allowing up to four years’ shelf life

With a few simple mouse clicks you can specify the

desired characteristics among the following:

• Element standard

• Ion standard

• Defining matrix

• Analytes

• Concentrations

The Custom Standards Platform is a dynamic web page:

elements, ions and matrices can only be chosen if the

combinations are chemically allowed.

After your request has been submitted online, we will

evaluate the production costs and respond with a quota-

tion by e-mail.

It’s easy, try it out!

* At sigma-aldrich.com/tracecert you can fi nd the

extensive TraceCERT portfolio of certifi ed single- and

multi-element standards.

21

sigma-aldrich.com/organiccrm

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The primary advantage of 1H quantitative NMR as a relative

primary method is that the integrals of the proton signals

are completely independent of the chemical structure.

Therefore, traceability can be established between two dif-

ferent compounds, in contrast to most other analytical

techniques.

With a small set of NIST traceable internal standards, we are

able to certify basically any organic compound by measur-

ing a gravimetrically produced mixture of the analyte and

the internal standard. The accurately determined mass to

mass ratio then allows for the calculation of the analyte

content with a very high level of confi dence. Typical uncer-

tainties range from 0.5% down to 0.1%.

New organic TraceCERT products

The portfolio of organic TraceCERT CRMs intended for use

as chromatography standards is comprised of over 50 prod-

ucts and is continually growing. The products include

amino acids, PAHs, fatty acids /FAME, pesticides and phar-

maceuticals, as published in previous articles [1].

The most recent product additions comprise several natu-

ral products as listed below.

Please visit our website (sigma-aldrich.com/organiccrm)

where you can find a complete and current listing of all

products and a library of technical articles and examples of

certifi cates that can be downloaded.

Cat. No. Brand Description Pack size

93485 Fluka® AMOZ 50 mg

94664 Fluka Anhydrotetracyclin HCl 50 mg

51868 Fluka trans-Caffeic acid 50 mg

56396 Fluka Caffeine 100 mg

52229 Fluka trans-Ferulic acid 50 mg

76635 Fluka Fumaric acid 100 mg

91215 Fluka Gallic acid 100 mg

52341 Fluka Salicylic acid 100 mg

68654 Fluka Vanillic acid 50 mg

Table 1 NEW organic neat CRMs TraceCERT

References:

[1] TraceCERT Organic Certified Reference Materials, Analytix,

Vol 2 and 3, 2010; Vol 1, 2011.

For analytical testing labs, ISO/IEC 17025 accreditation is

gaining increased importance for demonstrating compe-

tence in testing and calibration. Essential to this accredita-

tion is the use of suitable calibration standards, with the

recommendation that these standards are traceable to

internationally recognized reference materials.

While the availability of inorganic certifi ed reference materials

(CRMs) is usually high (see our corresponding TraceCERT

portfolio at sigma-aldrich.com/inorganiccrm), there has

been a lack of sources for traceable organic CRMs.

In the last year, Sigma-Aldrich has introduced the innova-

tive new product line of organic TraceCERT standards [1].

These premium CRMs are certifi ed in a double accredited

laboratory, fulfi lling both ISO/IEC 17025 and ISO Guide 34,

using high-performance quantitative NMR (HP-qNMR®)

for content determination with direct traceability to NIST and

SI.

The organic TraceCERT reference materials are character-

ized by:

• Certified Content by HP-qNMR

• Superior level of accuracy, calculated uncertainties and

lot-specific values

• Traceability to NIST

• Comprehensive documentation delivered with the

product (certification according to ISO Guide 31)

New TraceCERT® Organic Certified Reference Materials

Matthias Nold, Product Manager Analytical Standards [email protected]

Alexander Rück, Senior Scientist R&D Europe [email protected]

Christine Hellriegel, Senior Scientist R&D Europe [email protected]

22

sigma-aldrich.com/volpac

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Our 5L and 10L VOLPAC solution containers are perfect

when larger volumes of ready-to-use titration solutions are

needed. VOLPAC containers consist of a fl exible polyethylene

bag with an outlet tap and a cubic cardboard supporting

frame. Because of VOLPAC’s clever design, air cannot enter

the container during the dispensing operation. As a result,

VOLPAC containers can be drained completely without

contamination for less waste and more reliable analyses.

Advantages of VOLPAC containers:

• High quality of content and packing

• Easy handling

• No contamination during dispensing

• Reduced storage footprint and packaging material

New! All VOLPAC containers are now supplied with two

diff erent-sized adapters that allow direct connection of

the titrating tube to the VOLPAC container.


Acid solutions

35335-5L-VOLPAC, 35335-10L-VP Hydrochloric acid solution Reag. Ph. Eur. 0.1 mol/L

35329-5L-VP

35329-10L-VP

Hydrochloric acid solution Reag. Ph. Eur. 0.5 mol/L

35328-5L-VOLPAC

35328-10L-VP

Hydrochloric acid solution Reag. Ph. Eur. 1 mol/L

35327-10L-VOLPAC Hydrochloric acid solution 2 mol/L

35358-5L-VP

35358-10L-VP

Sulfuric acid solution Reag. Ph. Eur. 0.05 mol/L

35357-5L-VP

35357-10L-VP


35355-10L-VP Sulfuric acid solution Reag. Ph. Eur. 0.25 mol/L

35354-5L-VOLPAC

35354-10L-VP


35348-5L-VP

35348-10L-VP

Sulfuric acid solution 2.5 mol/L

Volumetric Titration VOLPAC® Solution Containers with new adapter

Andrea Felgner, Product Manager Analytical Reagents [email protected]

23

sigma-aldrich.com/volpac

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Base solutions

35116-5L-VP Potassium hydroxide solution 0.5 mol/L

35125-10L-VOLPAC Potassium hydroxide solution 0.1 mol/L

35262-10L-VOLPAC Sodium hydroxide solution 0.01 mol/L

35263-5L-VOLPAC

35263-10L-VP

Sodium hydroxide solution Reag. Ph. Eur. 0.1 mol/L

35256-5L-VOLPAC

35256-10L-VP

Sodium hydroxide solution Reag. Ph. Eur. 1 mol/L

35261-10L-VP Sodium hydroxide solution 0.2 mol/L

31086-5L-VP

31086-10L-VP

Sodium hydroxide solution 0.25 mol/L

35257-5L-VOLPAC

35257-10L-VP

Sodium hydroxide solution 0.5 mol/L

pH Buffer solutions

33665-5L-VP

33665-10L-VP

Buffer solution pH 4.0 (20 °C) with fungicide (citric acid / sodium hydroxide / sodium

chloride) red colored

pH 4.0

33643-5L-VP

33643-10L-VP

Buffer solution pH 4.0 (20 °C) with fungicide (citric acid / sodium hydroxide / sodium

chloride)

pH 4.0

33666-5L-VP

33666-10L-VP

Buffer solution pH 7.0 (20 °C) with fungicide (potassium dihydrogen phosphate /

disodium hydrogen phosphate) green colored

pH 7.0

33646-5L-VP

33646-10L-VP

Buffer solution pH 7.0 (20 °C) with fungicide (potassium dihydrogen phosphate /

disodium hydrogen phosphate)

pH 7.0

33667-5L-VP

33667-10L-VP

Buffer solution pH 9.0 (20 °C) (borax / hydrochloric acid)

blue colored

pH 9.0

33648-5L-VP

33648-10L-VP

Buffer solution pH 9.0 (20 °C) (borax / hydrochloric acid) pH 9.0

33668-10L-VP Buffer solution pH 10.0 (20 °C) (borax / sodium hydroxide) violet colored pH 10.0

Complexometric solutions

34544-5L-VP Ethylenediaminetetraacetic acid disodium salt solution with zinc complex added

(solution B)

1 mL solution = 1 German degree of hardness in 100 mL of water

35102-5L-VP

35102-10L-VP

IDRANAL® III solution (EDTA-Na2) 0.2 mol/L

34550-5L-VP-R

34550-10L-VP-R

IDRANAL III solution (EDTA-Na2), Reag. Ph. Eur. 0.1 mol/L

35103-5L-VP

35103-10L-VP

IDRANAL IV solution (DCTA-Na4), Reag. Ph. Eur. 0.1 mol/L

Salt solutions

34631-5L-VP Potassium dichromate solution for COD determination according to DIN 38409 0.02 mol/L

34277-5L-VP-R Sodium carbonate solution 0.5 mol/L

34247-10L-VP-R Sodium fluoride solution 40 g/L

34246-10L-VP-R Sodium oxalate solution 25 g/L

35224-5L-VP Sodium thiosulfate solution, for determination of iodine adsorption number

according to ASTM D 1510

34449-10L-VP-R Sodium thiosulfate solution 0.05 mol/L

35233-5L-VP Sodium thiosulfate solution 0.2 mol/L

35245-5L-VP

35245-10L-VP

Sodium thiosulfate solution Reag. Ph. Eur. 0.1 mol/L

34400-5L-VP Luff-Schoorl-Reagent (CuSO4*5H2O) ~25 g/L

Table 1 Complete list of all Fluka brand products that are available in VOLPAC containers (These products can be easily recognized since

they are tagged with a ‘-VOLPAC’ or ‘-VP’ in their product number.)

Special offer on all VOLPAC solution containers!

Receive 45% off your first order of any VOLPAC container. Please quote promotion code 979 when placing your order. Offer valid until July 31, 2011.

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