MICROVAL ISO 16140:2003 Validation of SimPlate Total … TPC-CI MicroVal... · The results are...

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ASSOCIATION LOI DE 1901 - N° SIRET 306 964 271 00036 - N° EXISTENCE 532900006329 - N°TVA FR4530696427100036

BIOCONTROL SYSTEMS Inc.

12822 SE 32nd Street

BELLEVUE, WA 98005

USA

MICROVAL ISO 16140:2003

Validation of SimPlate Total Plate Count

Color Indicator method

Quantitative method

This report includes 64 pages, with 6 annexes.

Only copies including the totality of this report are authorised.

SimPlate TVC

Version 0

December 21, 2009


ADRIA Développement 2/64 December 21, 2009

SimPlate TVC - Version 0

Summary

1 INTRODUCTION _______________________________________________ 4

1.1 Validation standard ________________________________________ 4

1.2 Reference method _________________________________________ 4

1.3 SimPlate Total Plate Count method ___________________________ 4

2 METHODS COMPARISON STUDY ________________________________ 5

2.1 Linearity, relative accuracy, relative sensitivity and determination of

unknown samples _________________________________________ 5

2.1.1 Food categories and food types ________________________________ 5

2.1.2 Experimental design _________________________________________ 6

2.1.3 Calculations and interpretations ________________________________ 7

2.2 Detection and quantification limits ___________________________ 9

3 CONCLUSION ________________________________________________ 10

Annexes __________________________________________________________________ 11

Annex 1 - Diagram of the reference method test procedure ISO 4833 - Horizontal method

for the enumeration of micro- organisms - Colony-count technique at 30 °C __________ 12

Annex 2 - The alternative method test procedure SimPlate Total Plate Count _________ 13

Annex 3 - Raw data of the linearity and the accuracy Summary ____________________ 14

Annex 4 – Linearity: statistical interpretations ___________________________________ 27

Annex 5 - Relative accuracy: Statistical interpretations ___________________________ 41

Annex 6 - Detection and quantification limits ____________________________________ 63




Before comment

Elements which allow the certification of the analysis quality can be consulted

by BIOCONTROL SYSTEMS Inc.

The results are presented according to the NF EN ISO 16140 standard.

Firm: BIOCONTROL SYSTEMS Inc.

12822 SE 32nd Street

BELLEVUE, WA 98005

USA

Expert Laboratory : ADRIA Développement

ZA Creac’h Gwen

F-29196 QUIMPER Cedex

Studied method: SimPlate Total Plate Count Color Indicator

Validation standard: NF EN ISO 16140 (October 2003): Food

microbiology – Protocol for the validation of

alternative methods

Reference method: ISO 4833 method (2003): “Microbiology of food and

animal feeding stuffs - Horizontal method for the

enumeration of microorganisms - Colony-count

technique at 30 °C”.

Products categories: All food categories




1 INTRODUCTION

1.1 Validation standard

The validation study is performed according to the ISO 16140 (October

2003): Food microbiology – Protocol for the validation of alternative methods.

1.2 Reference method

The reference method used for this validation, is: 4833 standard

“Microbiology of food and animal feeding stuffs - Horizontal method for the

enumeration of micro-organisms - Colony-count technique at 30 °C” (Cf.

annex 1)

1.3 SimPlate Total Plate Count method

SimPlate Total Plate Count Color Indicator (TPC-CI) method is used for the

detection and quantification of total aerobic micro-organism populations. It is

based on binary detection technology (BDT) which equates the presence of

total aerobic micro-organisms to the presence of a colour change in the

medium. The medium/sample mixture is dispensed into a SimPlate device,

and incubated for 24 - 28 h. The medium changes colour in the presence of

total aerobic micro-organisms. The total aerobic plate count is determined by

counting the wells with changed colour and referring to the SimPlate

Conversion Table. The SimPlate device is packaged separately.

The protocol of the proprietary method is described in annex 2.

The Single Test Medium of SimPlate TPC-CI consists in a kit with 100

individually-packaged dehydrated TPC-CI Medium containers. The Multiple

Test Medium consists in a kit with 50 multi-test dehydrated TPC-CI Medium

containers. There should be no difference in performance between these two

kit components. The kind of component kit used in the different validation

study parts should be mentioned.




2 METHODS COMPARISON STUDY

2.1 Linearity, relative accuracy, relative sensitivity and

determination of unknown samples

Linearity is the ability of the method when used with a given matrix to give results that are in proportion to the

amount of analyte present in the sample, that is an increase in analyte corresponds to a linear or proportional

increase in results.

The accuracy is the closeness of agreement between a test result and the accepted reference value.

The bias is the difference between the expectation of the test results and an accepted reference value.

The relative sensitivity is defined as the ability of the alternative method to detect two different amounts of analyte

measured by the reference method within a given matrix, at a specified average value, or over the whole

measurement range; that is, it is the minimal quantity variation (increase of the analyte concentration x) which

gives a significant variation of the measured signal (response y).

2.1.1 Food categories and food types

Three food categories were tested, with three food types minimum per

category. The repartition per category and food type is given below:

Table 1 - Number and nature of the samples

Food category Food type Number of samples

analysed

Number of samples

exploited

Meat and meat products Raw meat 13 11

Fermented 4 1

Heat processed 4 3

Dairy products Raw 3 3

Dry 3 2

Heat processed 15 12

Fruits and vegetables Fresh 5 2

Frozen 5 5

Juices and concentrates 12 7

Bakery and others Pastry 11 11

Dressing 1 0

Desserts 8 4

Seafood products Raw 4 2

Smoked 3 2

Heat processed 18 13

TOTAL 109 78




2.1.2 Experimental design

2.1.2.1. Relative linearity and precision profile

Five matrices were studied. Five levels of contamination were tested to cover

a minimum, a central, a maximum and two intermediary levels.

The linearity was investigated with one food item per category. The

contamination levels, the tested samples and the strain are presented in the

table below:

Product Strains Contamination levels (CFU/g)

Ground beef Naturally contaminated samples

Half creamed

pasteurized milk 1

Serratia marcescens Ad 455,

isolated from milk 2.102 to 2.107

Fresh orange juice Xanthomonas maltophilia II.2,

isolated from vegetables 2.102 to 5.106

Pastry Naturally contaminated samples

Scallops terrine Naturally contaminated samples

2.1.2.2. Relative accuracy

In complement to the data obtained according to experimental design

described in 2.1.2, 69 samples were analysed in duplicate by both methods,

i.e. ISO 4833 and SimPlate TVC method. 138 measurements were

performed (69 samples x 2 replicates). 40 samples gave interpretable results.

2.1.2.3. Raw data

All the raw data (linearity and accuracy) are provided annex 3.

1 Note that the linearity was done at first on naturally contaminated samples from a same batch.

Some incoherent results were observed by the alternative method; it was not possible and

“realistic” to perform the lack-of-fit test. A sample from the same batch of milk (n° 1254) is

mentioned in the accuracy study.




2.1.3 Calculations and interpretations

2.1.3.1. Relative linearity and precision profile

Raw data, calculation details and graphs are provided annex 4, the summary

is presented hereafter.

n : number of samples R : ratio SDr(Alt)/SD(Ref)

* x-axis and y-axis choice depends on the selected regression according to R

Statistical Interpretation:

P > 5 % : not significant 1 % < P < 5 % : significant P < 1 % : highly significant

Matrix R Selected

regression Rob.F

Critical

value

P% Correlation

coefficient

Regression equation

Ground beef 1,78 GMFR 17,356 3,58 0 0,993 log Alt = 1,047 log Ref – 0,189

Pasteurized milk 1,06 GMFR 2,208 4,53 18 0,999 log Alt = 1,022 log Ref + 0,194

Fresh orange juice 2,80 OLS1 3,910 4,53 7 0,998 Log Alt = 0,951 log Ref + 0,496

Pastry 1,52 GMFR 0,062 3,29 100 0,987 log Alt =1,062 log Ref – 0,163

Scallops terrine 1,00 GMFR 0,493 3,29 82 0,997 log Alt = 0,988 log Ref + 0,251

All the correlation coefficients are all higher than 0,98. The P Values of the

lack-of-fit tests are all higher than 5, except in the ground beef matrix, despite

a satisfying regression equation:

log Alt = 1,047 log Ref – 0,189.

Note that a highly correlation coefficient value can lead to a failure in the

linearity test robustness.

Based on the experimental design of the relative linearity, the estimation of

the method precision by CL(<yU/L>) mainly comes from the residual

standard deviation sy:x. The precision profiles of the relative sensitivity are

only intrinsic to the alternative method; they are presented annex 4.

The SimPlate TVC method shows satisfying relative linearity

performances for total viable count in the tested meat, dairy,

vegetables, backery and seafood products.




2.1.3.2. Relative accuracy

Raw data, calculation details and graphs are provided annex 5, the summary

is presented hereafter.

n : number of samples R : ratio SDr(Alt)/SD(Ref)

a : ordinate b: slope Critical T : critical value to Student t table

* x-axis and y-axis choice depends on the selected regression according to R

Statistical Interpretation: P > 5 % : not significant 1 % < P < 5 % : significant P < 1 % : highly significant

Category n R Regression

used a t(a) b t(b) Critical T

P% Bias

Intercept (0) Slope (1)

Meat products 16 1,67 GMFR 0,546 1,499 0,872 1,833 2,145 16 9 0,058

Dairy products 17 1,10 GMFR -0,247 0,586 1,106 1,075 2,131 57 30 0,290

Fruits and vegetables 14 3,33 OLS1 -0,527 1,026 1,081 0,769 2,179 32 46 0,153

Bakery and others 15 1,75 GMFR -0,259 1,602 1,087 2,052 2,160 13 6 0,030

Seafood products 17 0,33 OLS2 -0,238 1,883 1,011 0,436 2,131 8 67 0,215

All products 79 1,50 GMFR -0,074 0,532 1,026 0,872 1,991 60 39 0,150

Five disagreements were observed between the alternative and the

reference methods. Some streaks were realised on PCA from several wells

of the SimPlate TVC device. Colonies with different morphologies and

colours were identified by 16S rDNA sequencing. Molecular identifications

were also realised for the different isolates observed by the reference

method. Results are presented hereafter:

Sample

n° Product

Identifications

ISO 4833 SimPlate TVC

Enumeration Identification Enumeration Identification

1138

Frozen

artichoke

hearts

3,60 (log CFU/g)

and

3,60 (log CFU/g)

Brachybacterium sacelli

Dermacoccus sp.

Dermacoccus barathri

Arsenicicoccus bolidensis

1,30 (log CFU/g)

and

2,20 (log CFU/g)

Microbacterium aurum

Microbacterium arborescens


Rathayibacter tritici


1246 Dry sausage

8,58 (log CFU/g)

and

8,56 (log CFU/g)

Lactobacillus sakei

Lactobacillus sakei

7,45 (log CFU/g)

and

7,00 (log CFU/g)

Staphylococcus saprophyticus

Lactobacillus sakei

Staphylococcus saprophyticus

1254 Half creamed

pasteurized milk

3,58 (log CFU/g)

and

3,56 (log CFU/g)

In progress

1,70 (log CFU/g)

and

1,26 (log CFU/g)

Pseudomonas (fluorescens)

Bacillus subtilis

1370 Guacamole

4,60 (log CFU/g)

and

4,43 (log CFU/g)

Lactobacillus plantarum

Microbacterium oxydens

3,62 (log CFU/g)

and

3,49 (log CFU/g)

Enterococcus casseliflavus

Bacillus pumilus

Microbacterium oxydans

Bacillus subtilis

1371 Half creamed

pasteurized milk

3,26 (log CFU/g)

and

3,32 (log CFU/g)

Pseudomonas sp

Microbacterium phyllosphaerae

Pseudomonas sp

Microbacterium sp

Pseudomonas sp

3,88 (log CFU/g)

and

4,67 (log CFU/g)

Pseudomonas sp.

Bold typing indicates common identification results between both methods.




According to the observed biodiversity, the recovery performances could be

different between the alternative and the reference methods. Note that

depending of the analysed ecosystems, total viable count could be higher by

the reference method or by the alternative method. There is as well no

relationship with a production process or a food category.

However, taking into account all the analysed samples, bias between both

methods are characterised by small values, varying from 0,030 to 0,290 Log

CFU/g.

The intercept close to 0 and the slope close to 1 are validated for all the

tested categories.

The SimPlate TVC method shows satisfying relative accuracy

performances for total viable count enumeration:

- meat products,

- dairy products,

- fruits and vegetables,

- bakery and others,

- seafood products.

2.2 Detection and quantification limits

The critical level is the defined as the smallest amount which can be detected (not null), but

not quantified as an exact value. Below this value, it cannot be sure that the true value is not

null.

The detection limit is defined as being higher than the critical level because it involves a

power, the probability 1-, which has to be well over 50 %, for example 95 %.

The quantification limit is defined as the smallest amount of analyte (that is the lowest actual

number of organisms), which can be measured and quantified with defined precision and

accuracy under the experimental conditions by the method under validation.

The detection and quantification limits were determined with a pure culture of

Escherichia coli strain Adria 1.

Five different levels of inoculation were tested, with six replicates per level,

i.e. a total of 30 analyses by the alternative method.




Quantification limit were calculated for six independent blank samples

determinations.

All the data and the details of calculation are provided in the annex 6.

The critical level (50% of detection) were estimated and calculations were

performed to determine the limit of detection (LOD) and limit of quantification

(LOQ). Results are the following:

Calculation formula Calculated values

LC 1,65 So + Xo 3,9

LOD 3,3 So + Xo 5,8

LOQ 10So + Xo 13,5

3 CONCLUSION

The conclusions of the methods comparative study according to the

ISO16140 standard are:

- the SimPlate TVC method shows satisfying relative linearity and

accuracy results;

- the detection and quantification limits are respectively:

5,8 and 13,5 CFU/g.




Annexes




Annex 1 - Diagram of the reference method test procedure ISO 4833 -

Horizontal method for the enumeration of micro- organisms - Colony-count technique at 30 °C

10 g + 90 ml peptone salt

Stomach

Inoculate 2 plates per dilution

Incubate at 30°C 1°C for 72 h 3 h

Reading




Annex 2 - The alternative method test procedure SimPlate Total Plate Count

10 g sample + 90 ml peptone salt

Powdered medium + 9 ml Stomach

sterile deionized water containing 1 ml + 9 ml medium

1 ml of supplement A/100 ml

Pour sample/medium mixture onto

the center of a plate

Replace the lid

Incubate at 30°C 1°C for 24 to 28 h

During the validation, an incubation time of 24 h will be tested

Reading




Annex 3 - Raw data of the linearity and the accuracy

Summary




LINEARITY

Sample N°

Product

Reference method:ISO 4833 Alternative method:Simplate Total Plate Count

Dilution

Replicate 1 Replicate 2 cfu/g

Replicate1 cfu/g

Replicate2 log cfu/g


Replicate2 Dilution

Replicate 1 Replicate 2 Replicate1

(cfu/g) Replicate2

(cfu/g) Replicate1 (log cfu/g)

Replicate2 (log cfu/g) cfu/plate

(a) cfu/plate

(b) cfu/plate

(a) cfu/plate

(b) Positive wells

Result (cfu/g)

Positive wells

Result (cfu/g)

1870

Fre

sh o

rang

e ju

ice

10 22 16 21 18 210 190 2,32 2,28 10 27 640 27 640 640 640 2,81 2,81

100 4 3 0 3

100 2 400 2 400

1871 10 166 189 204 187 1800 1900 3,26 3,28 10 70 2980 75 3720 3000 3700 3,48 3,57

100 22 12 19 16

100 23 5400 11 2400

1872 100 197 211 204 192 20000 19000 4,30 4,28 100 67 26600 68 27600 27000 28000 4,43 4,45

1000 18 21 13 18

1000 13 28000 15 32000

1873 1000 239 184 236 200 210000 210000 5,32 5,32 1000 74 354000 76 392000 350000 390000 5,54 5,59

10000 23 16 22 13

10000 13 280000 16 360000

1874 10000 184 238 182 156 2100000 1700000 6,32 6,23 10000 77 4140000 84 >7380000 4100000 3200000 6,61 6,51

100000 22 23 18 13

100000 10 2200000 15 3200000

1875 10000 >300 >300 >300 >300 5700000 5400000 6,76 6,73 10000 84 >7380000 83 7380000 9000000 7000000 6,95 6,85

100000 60 53 54 54

100000 35 9000000 29 7000000




LINEARITY

Sample N°

Product


Dilution


Replicate1 cfu/g



Replicate2 Dilution


(cfu/g) Replicate2



(a) cfu/plate

(b) cfu/plate

(a) cfu/plate

(b) Positive wells

Result (cfu/g)

Positive wells

Result (cfu/g)

1876

Pas

try

10 29 24 43 38 290 400 2,46 2,60 10 23 540 9 180 540 180 2,73 2,26

100 6 4 4 2

100 1

0

1880 10 22 26 62 64 250 630 2,40 2,80 10 24 560 35 900 560 900 2,75 2,95

100 3 4 5 8

100 3 600 7 1400

1883 10 94 106 80 79 1000 800 3,00 2,90 10 39 1040 24 560 1000 560 3,00 2,75

100 13 10 9 8

100 7 140 2 40

1884 10 136 148 77 124 1500 1000 3,18 3,00 10 68 2760 35 900 2800 900 3,45 2,95

100 13 22 10 14

100 8 1600 4 800

1917 10 67 69 176 134 720 1500 2,86 3,18 10 43 1200 69 2880 1200 2900 3,08 3,46

100 14 9 12 14

100 13 280 28 6800

1918 100 >300 >300 >300 >300 93000 39000 4,97 4,59 100 82 62400 76 39200 62000 39000 4,79 4,59

1000 85 100 31 46

1000 29 70000 3 28000

1981 10 163 130 271 250 1500 2700 3,18 3,43 10 53 1660 24 560 1700 560 3,23 2,75

100 11 16 24 50

100 5 1000 2 400

1982 1000 >300 >300 >300 >300 440000 2600000 5,64 6,41 1000 83 738000 84 >738000 1100000 5100000 6,04 6,71

10000 35 52 257 270

10000 41 1120000 80 5080000

2103 10 90 89 133 111 880 1300 2,94 3,11 10 31 760 53 1660 760 1700 2,88 3,23

100 9 6 19 17

100 4 800 16 3600




LINEARITY

Sample N°

Product


Dilution


Replicate1 cfu/g



Replicate2 Dilution


(cfu/g) Replicate2



(a) cfu/plate

(b) cfu/plate

(a) cfu/plate

(b) Positive wells

Result (cfu/g)

Positive wells

Result (cfu/g)

1877

Sca

llops

terr

ine

10 3 1 2 3 20 25 1,30 1,40 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 1 1 1

100 0

0

1878 10 1 0 2 1 5 15 0,70 1,18 10 1 20 3 60 20 60 1,30 1,78

100 0 0 0 0

100

1879 10 0 4 4 4 20 40 1,30 1,60 10 1 20 2 40 20 40 1,30 1,60

100 0 0 0 1

100

1881 10 2 7 2 3 45 25 1,65 1,40 10 5 100 2 40 100 40 2,00 1,60

100 0 0 0 0

100 0

0

1882 10 8 10 17 10 86 160 1,93 2,20 10 10 220 11 240 220 240 2,34 2,38

100 0 1 3 4

100 1

1

1916 100 >300 >300 >300 >300 >300000 >300000 >5,48 >5,48 100 84

84

>738000 >738000 >5,87 5,87

1000 >300 >300 >300 >300

1000 84 >738000 84 >738000

1979 10 3 5 13 9 40 100 1,60 2,00 10 1 20 14 300 20 300 1,30 2,48

100 0 1 0 0

100 0

1 200

1980 100000 >300 >300 113 127 55000000 13000000 7,74 7,11 100000 84 >73800000 74 35400000 48000000 42000000 7,68 7,62

1000000 53 56 20 15

1000000 21 48000000 19 42000000

2005 10 120 140 118 132 1500 1400 3,18 3,15 10 65 2480 62 2240 2500 2200 3,40 3,34

100 31 32 28 25

100 12 2600 13 2800

2005 bis 100 140 201 137 125 20000 15000 4,30 4,18 100 52 16000 54 17200 16000 17000 4,20 4,23

1000 36 64 29 32

1000 12 26000 10 22000

2074 1000 >300 >300 >300 >300 2000000 490000 6,30 5,69 10000 36 940000 72 3240000 940000 3240000 5,97 6,51

10000 219 183 55 43




LINEARITY

Sample N°

Product


Dilution


Replicate1 cfu/g



Replicate2 Dilution


(cfu/g) Replicate2



(a) cfu/plate

(b) cfu/plate

(a) cfu/plate

(b) Positive wells

Result (cfu/g)

Positive wells

Result (cfu/g)

1919

Gro

und

beef

100 108 80 127 120 9400 13000 3,97 4,11 100 54 17200 51 15600 17000 16000 4,23 4,20

1000 7 11 16 15

1000 5 10000 5 10000

1983 100 226 303 234 276 28000 26000 4,45 4,41 100 76 39200 70 29800 39000 30000 4,59 4,48

1000 38 52 23 33

1000 17 38000 14 30000

1984 10000 6 7 7 4 65000 55000 4,81 4,74 10000 5 100000 3 60000 100000 60000 5,00 4,78

100000 1 0 2 0

100000 0

0

1995 100000 298 297 296 293 30000000 30000000 7,48 7,48 100000 79 47000000 76 39200000 47000000 39000000 7,67 7,59

1000000 24 38 38 34

1000000 18 400000000 12 26000000

1996 1000 114 97 115 102 110000 110000 5,04 5,04 1000 56 184000 50 150000 180000 150000 5,26 5,18

10000 12 9 9 8

10000 8 160000 11 240000

2073 100 134 115 127 110 12000 12000 4,08 4,08 100 43 12000 43 12000 12000 12000 4,08 4,08

1000 9 8 19 9

1000 9 18000 6 12000

2146 1000 >300 >300 >300 >300 410000 460000 5,61 5,66 1000 80 508000 81 556000 510000 560000 5,71 5,75

10000 39 42 47 44

2147 100 25 30 22 25 2800 2400 3,45 3,38 10 52 1600 47 1360 1600 1400 3,20 3,15

1000 0 7 1 4

100 5 1000 9 1800

2013

Pas

teur

ized

hal

f cre

amed

milk

1 171 184 170 171 190 180 2,28 2,26 1 78 440 73 338 440 340 2,64 2,53

10 25 34 26 30

10 15 320 13 280

2014 10 245 237 175 222 2500 2000 3,40 3,30 10 77 4140 79 4700 4100 4700 3,61 3,67

100 29 36 30 19

100 23 5400 21 4800

2015 100 259 263 225 178 26000 20000 4,41 4,30 100 74 35400 75 37200 35000 37000 4,54 4,57

1000 31 22 21 26

1000 22 50000 19 42000

2016 1000 206 207 199 209 220000 200000 5,34 5,30 1000 71 312000 75 372000 310000 370000 5,49 5,57

10000 41 23 20 22

10000 25 580000 14 300000

2017 10000 181 184 248 229 1900000 2400000 6,28 6,38 10000 78 4400000 82 6240000 4400000 6200000 6,64 6,79

100000 29 22 25 33

100000 19 4200000 30 7400000

2018 100000 187 220 238 252 21000000 25000000 7,32 7,40 100000 79 47000000 83 73800000 47000000 74000000 7,67 7,87

1000000 17 30 26 32

1000000 19 42000000 28 68000000




Linearity: summary results

Product ISO 4833 Simplate TVC

Replicate1 Replicate2 Replicate1 Replicate2

Fre

sh o

rang

e

juic

e

2,32 2,28 2,81 2,81

3,26 3,28 3,48 3,57

4,30 4,28 4,43 4,45

5,32 5,32 5,54 5,59

6,32 6,23 6,61 6,51

6,76 6,73 6,95 6,85 P

astr

y

2,46 2,60 2,73 2,26

2,40 2,80 2,75 2,95

3,00 2,90 3,00 2,75

3,18 3,00 3,45 2,95

2,86 3,18 3,08 3,46

4,97 4,59 4,79 4,59

3,18 3,43 3,23 2,75

5,64 6,41 6,04 6,71

2,94 3,11 2,88 3,23

Sca

llops

terr

ine

1,30 1,40 <1,00 <1,00

0,70 1,18 1,30 1,78

1,30 1,60 1,30 1,60

1,65 1,40 2,00 1,60

1,93 2,20 2,34 2,38

>5,48 >5,48 >5,87 5,87

1,60 2,00 1,30 2,48

7,74 7,11 7,68 7,62

3,18 3,15 3,40 3,34

4,30 4,18 4,20 4,23

6,30 5,69 5,97 6,51

Gro

und

beef

3,97 4,11 4,23 4,20

4,45 4,41 4,59 4,48

4,81 4,74 5,00 4,78

7,48 7,48 7,67 7,59

5,04 5,04 5,26 5,18

4,08 4,08 4,08 4,08

5,61 5,66 5,71 5,75

3,45 3,38 3,20 3,15

Pas

teur

ized

hal

f

crea

med

milk

2,28 2,26 2,64 2,53

3,40 3,30 3,61 3,67

4,41 4,30 4,54 4,57

5,34 5,30 5,49 5,57

6,28 6,38 6,64 6,79

7,32 7,40 7,67 7,87




ACCURACY – MEAT PRODUCTS

Sample N°

Product


Dilution


Replicate1 cfu/g



Replicate2 Dilution


(cfu/g) Replicate2


Replicate2 (log cfu/g)

cfu/plate

(a) cfu/plate

(b) cfu/plate

(a) cfu/plate

(b) Positive wells

Result (cfu/g)

Positive wells

Result (cfu/g)

1131 Beef meat (Bavette) 10000 >300 >300 >300 >300 14000000 >30000000 7,15 >7,48 10000 84 >7380000 84 >7380000 >7400000 >7400000 >6,87 >6,87

100000 155 130 >300 >300

1132 Escalope of turkey 10000 >300 >300 >300 >300 41000000 >30000000 7,61 >7,48 10000 84 >7380000 84 >7380000 >7400000 >7400000 >6,87 >6,87

100000 444 381 >300 >300

1133 Sausage with garlic 10000 >300 >300 280 291 9400000 2800000 6,97 6,45 1000 84 >738000 84 >738000 >740000 >740000 >5,87 >5,87

100000 78 110 29 25

1134 Dry sausage 10000 >300 >300 >300 >300 >30000000 >30000000 >7,48 >7,48 1000 84 >738000 84 >738000 >740000 >740000 >5,87 >5,87

10000 >300 >300 >300 >300

1135 Calf olive 10 203 231 253 253 2200 2500 3,34 3,40 10 66 2560 71 3120 2600 3100 3,41 3,49

(ready to eat meal) 100 19 24 25 24

100 10 2200 16 3600

1136 Duck with boletus 1000 171 150 127 138 160000 130000 5,20 5,11 1000 77 414000 65 248000 410000 250000 5,61 5,40

(ready to eat meal) 10000 19 22 12 18

1178 Ground beef 100 54 72 63 81 6200 7000 3,79 3,85 10 81 5560 5 (1/100

dilution)

10000 5600 10000 3,75 4,00

1000 7 4 3 7

1179 Escalope of turkey 1000 122 111 117 119 120000 120000 5,08 5,08 10000 6 120000 8 160000 120000 160000 5,08 5,20

10000 11 9 13 9

1180 Steak 1000 214 142 123 154 170000 140000 5,23 5,15 1000 67 266000 61 224000 27000 22000 4,43 4,34

10000 12 14 19 13

1181 Raw ham 1000 277 311 226 196 300000 210000 5,48 5,32 1000 57 190000 47 136000 190000 136000 5,28 5,13

10000 33 29 15 24

1183 Cooked chicken(columbo)

10000 >300 >300 >300 >300 >3000000 >3000000 >6,48 >6,48 100000 84 >73800000 84 >73800000 >74000000 >74000000 >7,87 >7,87

10000 >300 >300 >300 >300

1184 Cooked beef(Bourguignon)

1000 100 95 125 145 96000 140000 4,98 5,15 1000 38 100000 33 84000 100000 84000 5,00 4,92

10000 4 13 18 12

1246 Dry sausage 1000000 >300 >300 >300 >300 380000000 360000000 8,58 8,56 1000000 13 2,80E+07 5 1,00E+07 2,80E+07 1,00E+07 7,45 7,00

10000000 34 42 31 41




ACCURACY – DAIRY PRODUCTS

Sample N° Product


Dilution


Replicate1 cfu/g



Replicate2 Dilution


(cfu/g) Replicate2



cfu/plate

(a) cfu/plate

(b) cfu/plate

(a) cfu/plate

(b) Positive wells

Result (cfu/g)

Positive wells

Result (cfu/g)

1176 Half creamed pasteurized milk

10 >300 >300 >300 >300 >3000 >3000 >3,48 >3,48 1 84 >738 84 >738 >740 >740 >2,87 >2,87

100 >300 >300 >300 >300

1177 Raw milk 1000 59 63 72 39 61000 54000 4,79 4,73 100 82 62400 81 55600 62000 56000 4,79 4,75

10000 8 5 1 7

1254 Half creamed pasteurized

milk 100 35 39 32 36 3800 3600 3,58 3,56 1 22 50 9 18 50 18 1,70 1,26

1000 5 4 6 5

100 10 2200 2 40

1255 Milk powder 10 73 61 21 52 670 410 2,83 2,61 10 36 940 41 1100 940 1100 2,97 3,04

100 7 6 11 8

1371 Pasteurized milk 100 22 14 26 18 1800 2100 3,26 3,32 100 31 7600 79 47000 7600 47000 3,88 4,67

1000 1 2 1 2

1000 6 12000 28 68000

1985 Cream cheese 10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

100 0

0

2080 Fresh cheese wilth garlic

and herbs

10 ? ? ? ? 1100 1600 3,04 3,20 10 72 3240 77 4140 3240 4140 3,51 3,62

100 8 13 17 15

100 17 3800 16 3600

2081 Cream cheese 10 2 1 2 5 <40 35 <1,60 1,54 10 2 40 2 40 40 40 1,60 1,60

100 2 0 1 2 presence

100 1

1

2082 Cream cheese with pepper 10 12 19 25 40 200 400 2,30 2,60 10 21 480 36 940 480 940 2,68 2,97

100 5 8 14 8

100 4 800 1 20

2083 Cream cheese with nuts 10 10 11 3 7 120 50 2,08 1,70 10 3 60 5 100 60 100 1,78 2,00

100 2 4 1 1

100 2

2 120

2084 Cream cheese with nuts 10 8 7 4 8 150 60 2,18 1,78 10 5 100 6 120 100 120 2,00 2,08

100 1 0 0 1

100 0

1

2099 Raw milk 1000 38 52 39 64 45000 54000 4,65 4,73 1000 81 55600 82 624000 128000 68000 5,11 4,83

10000 7 3 9 7

10000 45 128000 28 68000

2100 Ribot Milk(fermented

typical Brittany product)

100000 >300 >300 >300 >300 55000000 74000000 7,74 7,87 100000 84 >73800000 84 >73800000 124000000 178000000 8,09 8,25

1000000 42 68 78 69

1000000 44 124000000 55 178000000

2101 Milk powder 100 105 165 133 121 14000 12000 4,15 4,08 100 69 28800 63 23200 28800 23200 4,46 4,37

1000 20 14 6 13

1000 10 22000 7 14000

2102 Milk powder 10 1 2 0 2 <40 <40 <1,60 <1,60 10 1 20 1 20 20 20 1,30 1,30

100 0 0 0 0 presence presence

100




ACCURACY – FRUITS AND VEGETABLES

Sample N°

Product


Dilution


Replicate1 cfu/g



Replicate2 Dilution


(cfu/g) Replicate2



cfu/plate

(a) cfu/plate

(b) cfu/plate

(a) cfu/plate

(b) Positive wells

Result (cfu/g)

Positive wells

Result(cfu/g)

1137 Frozen spinash branches 10 32 18 10 14 250 120 2,40 2,08 10 16 360 6 120 360 120 2,56 2,08

100 2 2 1 1

100 3 60 0 <10

1138 Frozen artichoke hearts 100 44 41 35 46 4000 4000 3,60 3,60 10 1 20 8 160 20 160 1,30 2,20

1000 2 2 5 2

1139 Minced celery 10000 >300 >300 >300 >300 >30000000 >30000000 >7,48 >7,48 1000 84 738000 84 738000 740000 740000 >5,87 >5,87

100000 >300 >300 >300 >300

1140 Minceed carots 10000 >300 >300 >300 >300 630000 690000 5,80 5,84 1000 84 738000 84 738000 740000 740000 >5,87 >5,87

10000 61 65 76 62

1141 Pasteurised apple juice 10 0 1 0 0 <40(presence) <10 <1,60 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1142 Carots velvety 10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1190 Fruit salad 10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1191 Fresh pine apple salad 10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1192 Smoothie(Pine apple-Banana-

Coco) 10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1193 Smoothie(Raspberry-srawberry-Bilberry)

10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1194 Sliced up leeks(MAP) 100000 >300 >300 >300 >300 190000000 130000000 8,28 8,11 1000000 68 276000000 70 298000000 280000000 300000000 8,45 8,48

1000000 185 185 111 140

1195 Lettuce(MAP) 10000 87 69 127 114 780000 1200000 5,89 6,08 10000 48 1420000 62 2240000 1400000 2200000 6,15 6,34

100000 8 7 7 10

1250 Frozen vegetables girdle-cake 1000 58 41 44 55 49000 49000 4,69 4,69 1000 5 10000 4 8000 10000 8000 4,00 3,90

10000 5 4 5 4

1251 Frozen french beans 100 161 148 162 137 16000 15000 4,20 4,18 10 81 56000 2(-3) 4000 5600 4000 3,75 3,60

1000 24 19 25 11

1252 Sop(potatoes,peas,courgette) 10 75 77 80 69 770 720 2,89 2,86 10 21 480 13 280 480 280 2,68 2,45

100 10 8 6 4

1370 Guacamole 100 >300 >300 287 265 40000 27000 4,60 4,43 10 75? 3720 38? 1000 4200 2800 3,62 3,45

1000 37 43 17 19

100 19 4200 13 2800




ACCURACY – BAKERY AND OTHERS

Sample N°

Product


Dilution


Replicate1 cfu/g



Replicate2 Dilution


(cfu/g) Replicate2


Replicate2( log cfu/g)

cfu/plate (a)

cfu/plate (b)

cfu/plate (a)

cfu/plate (b)

Positive wells

Result (cfu/g)

Positive wells

Result (cfu/g)

1188 Pastry(Eclair café) 10 128 138 167 147 1300 1500 3,11 3,18 10 24 560 34 860 560 860 2,75 2,93

100 4 8 15 11

1189 Pastry(Religieuse chocolat) 10 9 11 3 7 110 50 2,04 1,70 10 4 80 4 80 80 80 1,90 1,90

100 1 3 1 2

Ne

1244 Pancakes 10 28 56 25 20 420 240 2,62 2,38 10 17 380 37 960 380 960 2,58 2,98

100 3 6 4 3

1245 Baked custard 10 128 129 90 88 1300 880 3,11 2,94 10 41 1120 33 840 1100 840 3,04 2,92

100 21 14 7 9

1364 Whipped cream with

strawberries 10 0 0 0 0 <10 <10 <1,00 <1,00 10 1 20 0 <10 20 <10 1,30 <1,00

100 0 0 0 0

1365 Rice with milk 10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1366 Raspberry and currant

"coulis" 10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1367 Semolina with milk 10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1368 Bavarian cream with

strawberries 100 83 102 74 45 9400 5900 3,97 3,77 10 83 7380 66 2560 7400 2600 3,87 3,41

1000 11 11 5 6

100 28 6800 8 1600

1369 White cheese sauce with

smeet pepper 100 >300 >300 >300 >300 >300000 >300000 >5,48 >5,48 100 84 >73800 84 >73800 >74000 >74000 >4,87 >4,87

1000 >300 >300 >300 >300

1751 Custard 10000 >300 >300 >300 >300 18000000 21000000 7,26 7,32 100000 82 62400000 83 73800000 62000000 74000000 7,79 7,87

100000 177 176 214 206




ACCURACY – SEAFOOD PRODUCTS

Sample N°

Product


Dilution


Replicate1 cfu/g



Replicate2 Dilution


(cfu/g) Replicate2



cfu/plate (a)

cfu/plate (b)

cfu/plate (a)

cfu/plate (b)

Positive wells

Result (cfu/g)

Positive wells

Result (cfu/g)

1143 Whiting-pout fillet 10000 >300 >300 >300 >300 25000000 >30000000 7,40 >7,48 1000 84 >738000 84 >738000 >740000 >740000 >5,87 >5,87

100000 275 215 >300 >300

1144 Cod fillet 10000 >300 >300 235 194 6500000 2200000 6,81 6,34 1000 84 >738000 84 >738000 >740000 >740000 >5,87 >5,87

100000 63 67 26 21

1145 Cooked salmon 10 0 0 0 0 <10 <10 <1,00 <1,00 10 1 20 0 <10 20 <10 1,30 <1,00

100 0 0 0 0

1146 Salt cod pounded with garlic oil

and cream

10 0 0 0 0 <10 <10 <1,00 <1,00 10 0 <10 0 <10 <10 <10 <1,00 <1,00

100 0 0 0 0

1147 Smoked Kipper 10000 >300 >300 >300 >300 5300000 5900000 6,72 6,77 1000 84 >738000 84 >738000 >740000 >740000 >5,87 >5,87

100000 63 42 54 63

1182 Cooked Shark(curry) 10000 >300 >300 >300 >300 31000000 47000000 7,49 7,67 100000 67 26600000 77 41400000 27000000 42000000 7,43 7,62

100000 319 292 480 460

1185 Cooked peeled shrimps 1000 >300 >300 >300 >300 850000 2200000 5,93 6,34 1000 84 >738000 84 >738000 >738000 >738000 >5,87 >5,87

10000 89 81 233 204

1186 Smoked salmon 10000 205 19 278 290 1200000 2800000 6,08 6,45 100000 20 4600000 22 5000000 4600000 5000000 6,66 6,70

100000 11 21 10 27

1187 Smoked trout 10 5 2 6 7 35 65 1,54 1,81 10 5 100 3 60 100 60 2,00 1,78

100 2 0 0 1

Ne Ne

1247 Pink cooked shrimps 100 251 246 >300 >300 26000 50000 4,41 4,70 1000 21 48000 30 74000 48000 74000 4,68 4,87

1000 32 33 39(4-4) 61(7-4)

1248 Fish ready to eat meal 1000 182 188 234 225 190000 230000 5,28 5,36 10000 14 300000 16 360000 300000 360000 5,48 5,56

(Timbale) 10000 29 26 17 19

1249 Whiting fillet 10000 42 42 33 46 430000 410000 5,63 5,61 10000 22 500000 26 620000 500000 620000 5,70 5,79

100000 3 7 6 5

1253 Frozen tropical Sole fillet 1000 60 54 70 76 57000 77000 4,76 4,89 1000 24 56000 28 68000 56000 68000 4,75 4,83

10000 5 6 7 16

1745 Scallops terrine 10000 >300 >300 >300 >300 19000000 19000000 7,28 7,28 100000 69 28800000 74 354000000 29000000 35000000 7,46 7,54

100000 200 172 210 175




Accuracy : summary results

Sample N°


Replicate1 Replicate 2 Replicate1 Replicate 2

1131 Beef meat (Bavette) 7,15 >7,48 >6,87 >6,87

1132 Escalope of turkey 7,61 >7,48 >6,87 >6,87

1133 Sausage with garlic 6,97 6,45 >5,87 >5,87

1134 Dry sausage >7,48 >7,48 >5,87 >5,87

1135 Calf olive 3,34 3,40 3,41 3,49

1136 Duck with boletus 5,20 5,11 5,61 5,40

1137 Frozen spinash branches 2,40 2,08 2,56 2,08

1138 Frozen artichoke hearts 3,60 3,60 1,30 2,20

1139 Minced celery >7,48 >7,48 >5,87 >5,87

1140 Minceed carots 5,80 5,84 >5,87 >5,87

1141 Pasteurised apple juice <1,60 <1,00 <1,00 <1,00

1142 Carots velvety <1,00 <1,00 <1,00 <1,00

1143 Whiting-pout fillet 7,40 >7,48 >5,87 >5,87

1144 Cod fillet 6,81 6,34 >5,87 >5,87

1145 Cooked salmon <1,00 <1,00 1,30 <1,00

1146 Salt cod pounded with garlic oil and cream <1,00 <1,00 <1,00 <1,00

1147 Smoked Kipper 6,72 6,77 >5,87 >5,87

1176 Half creamed pasteurized milk >3,48 >3,48 >2,87 >2,87

1177 Raw milk 4,79 4,73 4,79 4,75

1178 Ground beef 3,79 3,85 3,75 4,00

1179 Escalope of turkey 5,08 5,08 5,08 5,20

1180 Steak 5,23 5,15 4,43 4,34

1181 Raw ham 5,48 5,32 5,28 5,13

1182 Cooked Shark(curry) 7,49 7,67 7,43 7,62

1183 Cooked chicken(columbo) >6,48 >6,48 >7,87 >7,87

1184 Cooked beef(Bourguignon) 4,98 5,15 5,00 4,92

1185 Cooked peeled shrimps 5,93 6,34 >5,87 >5,87

1186 Smoked salmon 6,08 6,45 6,66 6,70

1187 Smoked trout 1,54 1,81 2,00 1,78

1188 Pastry(Eclair café) 3,11 3,18 2,75 2,93

1189 Pastry(Religieuse chocolat) 2,04 1,70 1,90 1,90

1190 Fruit salad <1,00 <1,00 <1,00 <1,00

1191 Fresh pine apple salad <1,00 <1,00 <1,00 <1,00

1192 Smoothie (Pine apple-Banana-Coco) <1,00 <1,00 <1,00 <1,00

1193 Smoothie (Raspberry-srawberry-Bilberry) <1,00 <1,00 <1,00 <1,00

1194 Sliced up leeks(MAP) 8,28 8,11 8,45 8,48

1195 Lettuce(MAP) 5,89 6,08 6,15 6,34

1244 Pancakes 2,62 2,38 2,58 2,98

1245 Baked custard 3,11 2,94 3,04 2,92

1246 Dry sausage 8,58 8,56 7,45 7,00

1247 Pink cooked shrimps 4,41 4,70 4,68 4,87

1248 Fish ready to eat meal 5,28 5,36 5,48 5,56

1249 Whiting fillet 5,63 5,61 5,70 5,79

1250 Frozen vegetables girdle-cake 4,69 4,69 4,00 3,90

1251 Frozen french beans 4,20 4,18 3,75 3,60

1252 Sop(potatoes,peas,courgette) 2,89 2,86 2,68 2,45

1253 Frozen tropical Sole fillet 4,76 4,89 4,75 4,83

1254 Half creamed pasteurized milk 3,58 3,56 1,70 1,26

1255 Milk powder 2,83 2,61 2,97 3,04




Sample N°


Replicate1 Replicate 2 Replicate1 Replicate 2

1364 Whipped cream with strawberries <1,00 <1,00 1,30 <1,00

1365 Rice with milk <1,00 <1,00 <1,00 <1,00

1366 Raspberry and currant "coulis" <1,00 <1,00 <1,00 <1,00

1367 Semolina with milk <1,00 <1,00 <1,00 <1,00

1368 Bavarian cream with strawberries 3,97 3,77 3,87 3,41

1369 White cheese sauce with smeet pepper >5,48 >5,48 >4,87 >4,87

1370 Guacamole 4,60 4,43 3,62 3,45

1371 Pasteurized milk 3,26 3,32 3,88 4,67

1745 Scallops terrine 7,28 7,28 7,46 7,54

1751 Custard 7,26 7,32 7,79 7,87

1920 Cream cheese <1,00 <1,60 2,48 1,00

1921 Fresh cheese wilth garlic and herbs 3,04 2,96 4,28 4,30

1985 Cream cheese <1,00 <1,00 <1,00 <1,00

2080=1921 Fresh cheese wilth garlic and herbs 3,04 3,20 3,51 3,62

2081=1920 Cream cheese <1,60 1,54 1,60 1,60

2082 Cream cheese with pepper 2,30 2,60 2,68 2,97

2083 Cream cheese with nuts 2,08 1,70 1,78 2,00

2084 Cream cheese with nuts 2,18 1,78 2,00 2,08

2099 Raw milk 4,65 4,73 5,11 4,83

2100 Ribot Milk(fermented typical Brittany product) 7,74 7,87 8,09 8,25

2101 Milk powder 4,15 4,08 4,46 4,37

2102 Milk powder <1,60 <1,60 1,30 1,30




Annex 4 – Linearity: statistical interpretations

Annex 4.1: Relative linearity graphs, regression lines

and calculations

Annex 4.2: Precision profiles




Annex 4.1. - Relative linearity graphs, regression lines and calculations




Ground beef Bi-dimensional graphic

Regression straight fit




Statistical interpretation

Bias D 0,110

Reference method Alternative method di

1 3,97 4,040 4,23 4,215 0,175

2 4,45 4,430 4,59 4,535 0,105

3 4,81 4,775 5,00 4,890 0,115

4 7,48 7,480 7,67 7,630 0,150

5 5,04 5,040 5,26 5,220 0,180

6 4,08 4,080 4,08 4,080 0,000

7 5,61 5,635 5,17 5,461 -0,175

8 3,45 3,415 3,20 3,175 -0,240

1 4,11 0,099 4,20 0,021

2 4,41 0,028 4,48 0,078

3 4,74 0,049 4,78 0,156

4 7,48 0,000 7,59 0,057

5 5,04 0,000 5,18 0,057

6 4,08 0,000 4,08 0,000

7 5,66 0,035 5,75 0,409

8 3,38 0,049 3,15 0,035

0,047 0,084

1,78

OLS 2

GMFR

OLS 1

Alternative

Alternative

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Reference

Myi

Rep.2 SDyi

Rep.1

Rep.2

Mxi

SDxi

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

Reference




Pasteurized milk Bi-dimensional graphic

0

1

2

3

4

5

6

7

8

9

0 1 2 3 4 5 6 7 8 9

log

(Alt

ern

ati

ve

me

tho

d)

log(Reference method)

Pasteurized milk


y = 1,0224x + 0,1935

0,00

1,00

2,00

3,00

4,00

5,00

6,00

7,00

8,00

9,00

0,00 1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00 9,00

Alt

ern

ati

ve

Reference

Pasteurized milk-GMFR regression





Bias D 0,303


1 2,28 2,270 2,64 2,585 0,315

2 3,40 3,350 3,61 3,640 0,290

3 4,41 4,355 4,54 4,555 0,200

4 5,34 5,320 5,49 5,530 0,210

5 6,28 6,330 6,64 6,715 0,385

6 7,32 7,360 7,67 7,770 0,410

1 2,26 0,014 2,53 0,078

2 3,30 0,071 3,67 0,042

3 4,30 0,078 4,57 0,021

4 5,30 0,028 5,57 0,057

5 6,38 0,071 6,79 0,106

6 7,40 0,057 7,87 0,141

0,094 0,100

1,06

OLS 2

GMFR

OLS 1

Artificially contaminated samples

Alternative

Alternative

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Reference

Myi

Rep.2 SDyi

Rep.1

Rep.2

Mxi

SDxi

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

Reference




Fresh orange juice Bi-dimensional graphic

0

1

2

3

4

5

6

7

8

0 1 2 3 4 5 6 7 8

log

(Alt

ern

ati

ve

me

tho

d)


Fresh orange juice


y = 0,9512x + 0,4958

0,00

1,00

2,00

3,00

4,00

5,00

6,00

7,00

8,00

0,00 1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00

Alt

ern

ati

ve

Reference

Fresh orange juice-OLS1 regression





Bias D 0,250


1 2,32 2,300 2,81 2,810 0,510

2 3,26 3,270 3,48 3,525 0,255

3 4,30 4,290 4,43 4,440 0,150

4 5,32 5,320 5,54 5,565 0,245

5 6,32 6,275 6,61 6,560 0,285

6 6,76 6,745 6,95 6,900 0,155

1 2,28 0,028 2,81 0,000

2 3,28 0,014 3,57 0,064

3 4,28 0,014 4,45 0,014

4 5,32 0,000 5,59 0,035

5 6,23 0,064 6,51 0,071

6 6,73 0,021 6,85 0,071

0,026 0,073

2,80

OLS 2

GMFR

OLS 1


Alternative

Alternative

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Reference

Myi

Rep.2 SDyi

Rep.1

Rep.2

Mxi

SDxi

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

Reference




Pastry Bi-dimensional graphic

0

1

2

3

4

5

6

7

8

0 1 2 3 4 5 6 7 8

log

(Alt

ern

ati

ve

me

tho

d)


Pastry


y = 1,0619x - 0,1628

0,00

1,00

2,00

3,00

4,00

5,00

6,00

7,00

8,00

0,00 1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00

Alt

ern

ati

ve

Reference

Pastry-GMFR regression





Bias D 0,030


1 2,46 2,530 2,73 2,495 -0,035

2 2,40 2,600 2,75 2,850 0,250

3 3,00 2,950 3,00 2,875 -0,075

4 3,18 3,090 3,45 3,200 0,110

5 2,86 3,020 3,08 3,270 0,250

6 4,97 4,780 4,79 4,690 -0,090

7 3,18 3,305 3,23 2,990 -0,315

8 5,64 6,025 6,04 6,375 0,350

9 2,94 3,025 2,88 3,055 0,030

1 2,60 0,099 2,26 0,332

2 2,80 0,283 2,95 0,141

3 2,90 0,071 2,75 0,177

4 3,00 0,127 2,95 0,354

5 3,18 0,226 3,46 0,269

6 4,59 0,269 4,59 0,141

7 3,43 0,177 2,75 0,339

8 6,41 0,544 6,71 0,474

9 3,11 0,120 3,23 0,247

0,262 0,398

1,52

OLS 2

GMFR

OLS 1

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

Myi

Rep.2 SDyi

Rep.1

Rep.2

Mxi

SDxi

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Reference

Reference Alternative

Alternative

Reference method X Alternative method Y Y^ Myi - Eyi

1 2,46 2,530 2,530 2,73 2,495 2,495 2,52 -0,029

2 2,40 2,600 2,600 2,75 2,850 2,850 2,60 0,252

3 3,00 2,950 2,950 3,00 2,875 2,875 2,97 -0,095

4 3,18 3,090 3,090 3,45 3,200 3,200 3,12 0,081

5 2,86 3,020 3,020 3,08 3,270 3,270 3,04 0,226

6 4,97 4,780 4,780 4,79 4,690 4,690 4,91 -0,223

7 3,18 3,305 3,305 3,23 2,990 2,990 3,35 -0,357

8 5,64 6,025 6,025 6,04 6,375 6,375 6,24 0,140

9 2,94 3,025 3,025 2,88 3,055 3,055 3,05 0,005

1 2,60 0,099 2,26 0,332 Sum = 0,000

2 2,80 0,283 2,95 0,141 RSD' = 0,216

3 2,90 0,071 2,75 0,177

4 3,00 0,127 2,95 0,354

5 3,18 0,226 3,46 0,269

6 4,59 0,269 4,59 0,141

7 3,43 0,177 2,75 0,339

8 6,41 0,544 6,71 0,474

9 3,11 0,120 3,23 0,247

Sx= 1,158 Sy= 1,230

SD(Mxi) = 1,158 SD(Myi) = 1,230

M(x) = 3,481 M(y) = 3,533

MED(x) = 3,025 MED(y) = 3,055

rob.SDwx= 0,262 rob.SDwy= 0,398

q (doses)= 9

p (replicates)= 2

v (df)= 7

SDwy/SDwx SDwx/Sdwy

rob. 1,52 0,658

Orthogonal linear regression:

r(Mx, My) = 0,9865 SD t:H p(t:H) H Tcritique

Res.SD(My) = 0,216 = RSD' b= 1,0619 0,066 0,938 0,380 1

RSD' * SQRT(p) = Res.SD(y) = 0,306 =sr(y) a= -0,1628 0,241 0,676 0,521 0

Lack-of-fit (non-linearity):

vd (df DEN)= 9

vn (df NUM)= 7

rob. F= 0,062

p(rob.F)= 100%

2,36462

SDyiRep.2

Rep.1

Rep.2

Mxi

SDxi

MyiRep.1




Scallops terrine Bi-dimensional graphic

0

1

2

3

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5

6

7

8

0 1 2 3 4 5 6 7 8

log

(Alt

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Scallops terrine


y = 0,9879x + 0,2508

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Reference

Scallops terrine -GMFR regression





Bias D 0,225


1 0,70 0,940 1,30 1,540 0,600

2 1,30 1,450 1,30 1,450 0,000

3 1,65 1,525 2,00 1,800 0,275

4 1,93 2,065 2,34 2,360 0,295

5 1,60 1,800 1,30 1,890 0,090

6 7,74 7,425 7,68 7,650 0,225

7 3,18 3,165 3,40 3,370 0,205

8 4,30 4,240 4,20 4,215 -0,025

9 6,30 5,995 5,97 6,240 0,245

1 1,18 0,339 1,78 0,339

2 1,60 0,212 1,60 0,212

3 1,40 0,177 1,60 0,283

4 2,20 0,191 2,38 0,028

5 2,00 0,283 2,48 0,834

6 7,11 0,445 7,62 0,042

7 3,15 0,021 3,34 0,042

8 4,18 0,085 4,23 0,021

9 5,69 0,431 6,51 0,382

0,315 0,315

1,00

OLS 2

GMFR

OLS 1

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

Myi

Rep.2 SDyi

Rep.1

Rep.2

Mxi

SDxi

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Reference


Alternative


1 0,70 0,940 0,940 1,30 1,540 1,540 1,18 0,361

2 1,30 1,450 1,450 1,30 1,450 1,450 1,68 -0,233

3 1,65 1,525 1,525 2,00 1,800 1,800 1,76 0,043

4 1,93 2,065 2,065 2,34 2,360 2,360 2,29 0,069

5 1,60 1,800 1,800 1,30 1,890 1,890 2,03 -0,139

6 7,74 7,425 7,425 7,68 7,650 7,650 7,59 0,064

7 3,18 3,165 3,165 3,40 3,370 3,370 3,38 -0,007

8 4,30 4,240 4,240 4,20 4,215 4,215 4,44 -0,224

9 6,30 5,995 5,995 5,97 6,240 6,240 6,17 0,067

1 1,18 0,339 1,78 0,339 Sum = 0,000

2 1,60 0,212 1,60 0,212 RSD' = 0,196

3 1,40 0,177 1,60 0,283

4 2,20 0,191 2,38 0,028

5 2,00 0,283 2,48 0,834

6 7,11 0,445 7,62 0,042

7 3,15 0,021 3,34 0,042

8 4,18 0,085 4,23 0,021

9 5,69 0,431 6,51 0,382

Sx= 2,263 Sy= 2,235

SD(Mxi) = 2,263 SD(Myi) = 2,235

M(x) = 3,178 M(y) = 3,391

MED(x) = 2,065 MED(y) = 2,360


q (doses)= 9

p (replicates)= 2

v (df)= 7

SDwy/SDwx SDwx/Sdwy

rob. 1,00 1,000



Res.SD(My) = 0,196 = RSD' b= 0,9879 0,031 0,396 0,704 1

RSD' * SQRT(p) = Res.SD(y) = 0,277 =sr(y) a= 0,2508 0,117 2,138 0,070 0


vd (df DEN)= 9

vn (df NUM)= 7

rob. F= 0,493

p(rob.F)= 82%

2,306

SDyiRep.2

Rep.1

Rep.2

Mxi

SDxi

MyiRep.1




Annex 4.2. - Precision profiles




0,0%

5,0%

10,0%

15,0%

20,0%

25,0%

30,0%

35,0%

40,0%

45,0%

50,0%

0 1 2 3 4 5 6 7

CV

(<x

(y)>

)

Reference method log cfu/g (x)

Precision profiles obtained for the different food matrices

Ground beef Pasteurized milk Fresh orange juice Scallops terrine Pastry




Annex 5 - Relative accuracy: Statistical interpretations

Relative accuracy graphs, regression lines

and calculations




Meat products Bi-dimensional graphic

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Meat p roducts


y = 0,8718x + 0,5458

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Reference

Meat products-GMFR regression





Bias D 0,058


1 3,97 4,040 4,23 4,215 0,175

2 4,45 4,430 4,59 4,535 0,105

3 4,81 4,775 5,00 4,890 0,115

4 7,48 7,480 7,67 7,630 0,150

5 5,04 5,040 5,26 5,220 0,180

6 4,08 4,080 4,08 4,080 0,000

7 5,61 5,635 5,17 5,461 -0,175

8 3,45 3,415 3,20 3,175 -0,240

9 3,34 3,370 3,41 3,450 0,080

10 5,20 5,155 5,61 5,505 0,350

11 3,79 3,820 3,75 3,875 0,055

12 5,08 5,080 5,08 5,140 0,060

13 5,23 5,190 4,43 4,385 -0,805 1180 Steak

14 5,48 5,400 5,28 5,205 -0,195

15 4,98 5,065 5,00 4,960 -0,105

16 8,58 8,570 7,45 7,225 -1,345 1246 Dry sausage

1 4,11 0,099 4,20 0,021

2 4,41 0,028 4,48 0,078

3 4,74 0,049 4,78 0,156

4 7,48 0,000 7,59 0,057

5 5,04 0,000 5,18 0,057

6 4,08 0,000 4,08 0,000

7 5,66 0,035 5,75 0,409

8 3,38 0,049 3,15 0,035

9 3,40 0,042 3,49 0,057

10 5,11 0,064 5,40 0,148

11 3,85 0,042 4,00 0,177

12 5,08 0,000 5,20 0,085

13 5,15 0,057 4,34 0,064

14 5,32 0,113 5,13 0,106

15 5,15 0,120 4,92 0,057

16 8,56 0,014 7,00 0,318

0,063 0,105

1,67

OLS 2

GMFR

OLS 1

Mxi

SDxi

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Myi

Rep.2 SDyi

Rep.1

Rep.2

Reference


Alternative





1 3,97 4,040 4,040 4,23 4,215 4,215 4,07 0,147

2 4,45 4,430 4,430 4,59 4,535 4,535 4,41 0,127

3 4,81 4,775 4,775 5,00 4,890 4,890 4,71 0,181

4 7,48 7,480 7,480 7,67 7,630 7,630 7,07 0,563

5 5,04 5,040 5,040 5,26 5,220 5,220 4,94 0,280

6 4,08 4,080 4,080 4,08 4,080 4,080 4,10 -0,023

7 5,61 5,635 5,635 5,17 5,461 5,461 5,46 0,002

8 3,45 3,415 3,415 3,20 3,175 3,175 3,52 -0,348

9 3,34 3,370 3,370 3,41 3,450 3,450 3,48 -0,034

10 5,20 5,155 5,155 5,61 5,505 5,505 5,04 0,465

11 3,79 3,820 3,820 3,75 3,875 3,875 3,88 -0,001

12 5,08 5,080 5,080 5,08 5,140 5,140 4,97 0,166

13 5,23 5,190 5,190 4,43 4,385 4,385 5,07 -0,685

14 5,48 5,400 5,400 5,28 5,205 5,205 5,25 -0,048

15 4,98 5,065 5,065 5,00 4,960 4,960 4,96 -0,001

16 8,58 8,570 8,570 7,45 7,225 7,225 8,02 -0,792

1 4,11 0,099 4,20 0,021 Sum = 0,000

2 4,41 0,028 4,48 0,078 RSD' = 0,372

3 4,74 0,049 4,78 0,156

4 7,48 0,000 7,59 0,057

5 5,04 0,000 5,18 0,057

6 4,08 0,000 4,08 0,000

7 5,66 0,035 5,75 0,409

8 3,38 0,049 3,15 0,035

9 3,40 0,042 3,49 0,057

10 5,11 0,064 5,40 0,148

11 3,85 0,042 4,00 0,177

12 5,08 0,000 5,20 0,085

13 5,15 0,057 4,34 0,064

14 5,32 0,113 5,13 0,106

15 5,15 0,120 4,92 0,057

16 8,56 0,014 7,00 0,318

Sx= 1,372 Sy= 1,196

SD(Mxi) = 1,372 SD(Myi) = 1,196

M(x) = 5,034 M(y) = 4,934

MED(x) = 5,053 MED(y) = 4,925


q (doses)= 16

p (replicates)= 2

v (df)= 14

SDwy/SDwx SDwx/Sdwy

rob. 1,67 0,600



Res.SD(My) = 0,372 = RSD' b= 0,8718 0,070 1,833 0,088 1

RSD' * SQRT(p) = Res.SD(y) = 0,525 =sr(y) a= 0,5458 0,364 1,499 0,156 0


vd (df DEN)= 16

vn (df NUM)= 14

rob. F= 52,682

p(rob.F)= 0%

2,14479

SDyiRep.2

Rep.1

Rep.2

Mxi

SDxi

MyiRep.1




Dairy products Bi-dimensional graphic

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Milk products Naturally contaminated samples



y = 1,1015x - 0,2471

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Reference

Dairy products-GMFR regression





Bias D 0,290


1 2,28 2,270 2,64 2,585 0,315

2 3,40 3,350 3,61 3,640 0,290

3 4,41 4,355 4,54 4,555 0,200

4 5,34 5,320 5,49 5,530 0,210

5 6,28 6,330 6,64 6,715 0,385

6 7,32 7,360 7,67 7,770 0,410

7 4,79 4,760 4,79 4,770 0,010

8 3,58 3,570 1,70 1,480 -2,090 1254 Half creamed pasteurized milk

9 2,83 2,720 2,97 3,005 0,285

10 3,26 3,290 3,88 4,275 0,985 1371 Half creamed pasteurized milk

11 3,04 3,120 3,51 3,565 0,445

12 2,30 2,450 2,68 2,825 0,375

13 2,08 1,890 1,78 1,890 0,000

14 2,18 1,980 2,00 2,040 0,060

15 4,65 4,690 5,11 4,970 0,280

16 7,74 7,805 8,09 8,170 0,365

17 4,15 4,115 4,46 4,415 0,300

1 2,26 0,014 2,53 0,078

2 3,30 0,071 3,67 0,042

3 4,30 0,078 4,57 0,021

4 5,30 0,028 5,57 0,057

5 6,38 0,071 6,79 0,106

6 7,40 0,057 7,87 0,141

7 4,73 0,042 4,75 0,028

8 3,56 0,014 1,26 0,311

9 2,61 0,156 3,04 0,049

10 3,32 0,042 4,67 0,559

11 3,20 0,113 3,62 0,078

12 2,60 0,212 2,97 0,205

13 1,70 0,269 2,00 0,156

14 1,78 0,283 2,08 0,057

15 4,73 0,057 4,83 0,198

16 7,87 0,092 8,25 0,113

17 4,08 0,049 4,37 0,064

0,105 0,115

1,10

OLS 2

GMFR

OLS 1

Mxi

SDxi

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Myi

Rep.2 SDyi

Rep.1

Rep.2

Reference


Alternative





1 2,28 2,270 2,270 2,64 2,585 2,585 2,25 0,332

2 3,40 3,350 3,350 3,61 3,640 3,640 3,44 0,197

3 4,41 4,355 4,355 4,54 4,555 4,555 4,55 0,005

4 5,34 5,320 5,320 5,49 5,530 5,530 5,61 -0,083

5 6,28 6,330 6,330 6,64 6,715 6,715 6,73 -0,010

6 7,32 7,360 7,360 7,67 7,770 7,770 7,86 -0,090

7 4,79 4,760 4,760 4,79 4,770 4,770 5,00 -0,226

8 3,58 3,570 3,570 1,70 1,480 1,480 3,69 -2,205

9 2,83 2,720 2,720 2,97 3,005 3,005 2,75 0,256

10 3,26 3,290 3,290 3,88 4,275 4,275 3,38 0,898

11 3,04 3,120 3,120 3,51 3,565 3,565 3,19 0,375

12 2,30 2,450 2,450 2,68 2,825 2,825 2,45 0,373

13 2,08 1,890 1,890 1,78 1,890 1,890 1,83 0,055

14 2,18 3,130 3,130 2,00 3,185 3,185 3,20 -0,016

15 4,65 4,650 4,650 5,11 5,110 5,110 4,87 0,235

16 7,74 7,740 7,740 8,09 8,090 8,090 8,28 -0,188

17 4,15 4,150 4,150 4,46 4,415 4,415 4,32 0,091

1 2,26 0,014 2,53 0,078 Sum = 0,000

2 3,30 0,071 3,67 0,042 RSD' = 0,650

3 4,30 0,078 4,57 0,021

4 5,30 0,028 5,57 0,057

5 6,38 0,071 6,79 0,106

6 7,40 0,057 7,87 0,141

7 4,73 0,042 4,75 0,028

8 3,56 0,014 1,26 0,311

9 2,61 0,156 3,04 0,049

10 3,32 0,042 4,67 0,559

11 3,20 0,113 3,62 0,078

12 2,60 0,212 2,97 0,205

13 1,70 0,269 2,00 0,156

14 1,78 0,283 2,08 0,057

15 4,73 0,057 4,83 0,198

16 7,87 0,092 8,25 0,113

17 4,08 0,049 4,37 0,064

Sx= 1,721 Sy= 1,895

SD(Mxi) = 1,721 SD(Myi) = 1,895

M(x) = 4,144 M(y) = 4,318

MED(x) = 3,570 MED(y) = 4,275


q (doses)= 17

p (replicates)= 2

v (df)= 15

SDwy/SDwx SDwx/Sdwy

rob. 1,10 0,909



Res.SD(My) = 0,650 = RSD' b= 1,1015 0,094 1,075 0,299 1



vd (df DEN)= 17

vn (df NUM)= 15

rob. F= 134,327

p(rob.F)= 0%

2,13145

SDyiRep.2

Rep.1

Rep.2

Mxi

SDxi

MyiRep.1




Fruits and vegetables Bi-dimensional graphic

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Fruit and vegetablesArtificially contaminated samples

Naturally contaminated samples


y = 1,0806x - 0,5274

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Reference

Fruits and vegetables-OLS1 regression




Statistical interpretation Bias D 0,153


1 2,32 2,300 2,81 2,810 0,510

2 3,26 3,270 3,48 3,525 0,255

3 4,30 4,290 4,43 4,440 0,150

4 5,32 5,320 5,54 5,565 0,245

5 6,32 6,275 6,61 6,560 0,285

6 6,76 6,745 6,95 6,900 0,155

7 2,40 2,240 2,56 2,320 0,080

8 3,60 3,600 1,30 1,750 -1,850 Frozen artichoke hearts

9 8,28 8,195 8,45 8,465 0,270

10 5,89 5,985 6,15 6,245 0,260

11 4,69 4,690 4,00 3,950 -0,740 Frozen vegetables girdle-cake

12 4,20 4,190 3,75 3,675 -0,515

13 2,89 2,875 2,68 2,565 -0,310

14 4,60 4,515 3,62 3,535 -0,980 Guacamole

1 2,28 0,028 2,81 0,000

2 3,28 0,014 3,57 0,064

3 4,28 0,014 4,45 0,014

4 5,32 0,000 5,59 0,035

5 6,23 0,064 6,51 0,071

6 6,73 0,021 6,85 0,071

7 2,08 0,226 2,08 0,339

8 3,60 0,000 2,20 0,636

9 8,11 0,120 8,48 0,021

10 6,08 0,134 6,34 0,134

11 4,69 0,000 3,90 0,071

12 4,18 0,014 3,60 0,106

13 2,86 0,021 2,45 0,163

14 4,43 0,120 3,45 0,120

0,031 0,105

3,33

OLS 2

GMFR

OLS 1


Alternative

Alternative

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Reference

Myi

Rep.2 SDyi

Rep.1

Rep.2

Mxi

SDxi

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

Reference




Reference method X Alternative method Y Y^

1 2,32 2,300 2,300 2,81 2,810 1,958

2 3,26 3,270 3,270 3,48 3,525 3,006

3 4,30 4,290 4,290 4,43 4,440 4,108

4 5,32 5,320 5,320 5,54 5,565 5,221

5 6,32 6,275 6,275 6,61 6,560 6,253

6 6,76 6,745 6,745 6,95 6,900 6,761

7 2,40 2,240 2,240 2,56 2,320 1,893

8 3,60 3,600 3,600 1,30 1,750 3,363

9 8,28 8,195 8,195 8,45 8,465 8,328

10 5,89 5,985 5,985 6,15 6,245 5,940

11 4,69 4,690 4,690 4,00 3,950 4,541

12 4,20 4,190 4,190 3,75 3,675 4,000

13 2,89 2,875 2,875 2,68 2,565 2,579

14 4,60 4,515 4,515 3,62 3,535 4,352

1 2,28 0,028 2,300 2,81 0,000 1,958

2 3,28 0,014 3,270 3,57 0,064 3,006

3 4,28 0,014 4,290 4,45 0,014 4,108

4 5,32 0,000 5,320 5,59 0,035 5,221

5 6,23 0,064 6,275 6,51 0,071 6,253

6 6,73 0,021 6,745 6,85 0,071 6,761

7 2,08 0,226 2,240 2,08 0,339 1,893

8 3,60 0,000 3,600 2,20 0,636 3,363

9 8,11 0,120 8,195 8,48 0,021 8,328

10 6,08 0,134 5,985 6,34 0,134 5,940

11 4,69 0,000 4,690 3,90 0,071 4,541

12 4,18 0,014 4,190 3,60 0,106 4,000

13 2,86 0,021 2,875 2,45 0,163 2,579

14 4,43 0,120 4,515 3,45 0,120 4,352

Sx= 1,714 Sy= 1,962

SD(Mxi) = 1,746 SD(Myi) = 1,993

M(x) = 4,606 M(y) = 4,450

MED(x) = 4,403 MED(y) = 3,813


q (doses)= 14

p (réplicates)= 2

v (df)= 12

SDwy/SDwx SDwx/Sdwy

rob. 3,33 0,300

OLS1 regression

r(Mx, My) = 0,9440 SD t:H p(t:H) H Critical T

Res.SD(My) = 0,660 = RSD b= 1,0806 0,105 0,769 0,457 1

RSD * SQRT(p) = Res.SD(y) = 0,933 =sr(y) a= -0,5274 0,514 1,026 0,325 0


vd (df DEN)= 14

vn (df NUM)= 12

rob. F= 84,644

p(rob.F)= 0%

2,17881

SDyi

Rep.1

Rep.2

MyiRep.1

Rep.2

Mxi

SDxi




Bakery and others Bi-dimensional graphic

0

1

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5

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7

8

0 1 2 3 4 5 6 7 8

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(Alt

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Bakery and others


y = 1,0874x - 0,2593

0,00

1,00

2,00

3,00

4,00

5,00

6,00

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8,00

9,00

0,00 1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00 9,00

Alt

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Reference

Bakery and others-GMFR regression




Statistical interpretation Bias D 0,030


1 2,46 2,530 2,73 2,495 -0,035

2 2,40 2,600 2,75 2,850 0,250

3 3,00 2,950 3,00 2,875 -0,075

4 3,18 3,090 3,45 3,200 0,110

5 2,86 3,020 3,08 3,270 0,250

6 4,97 4,780 4,79 4,690 -0,090

7 3,18 3,305 3,23 2,990 -0,315

8 5,64 6,025 6,04 6,375 0,350

9 2,94 3,025 2,88 3,055 0,030

10 3,11 3,145 2,75 2,840 -0,305

11 2,04 1,870 1,90 1,900 0,030

12 2,62 2,500 2,58 2,780 0,280

13 3,11 3,025 3,04 2,980 -0,045

14 3,97 3,870 3,87 3,640 -0,230

15 7,26 7,290 7,79 7,830 0,540

1 2,60 0,099 2,26 0,332

2 2,80 0,283 2,95 0,141

3 2,90 0,071 2,75 0,177

4 3,00 0,127 2,95 0,354

5 3,18 0,226 3,46 0,269

6 4,59 0,269 4,59 0,141

7 3,43 0,177 2,75 0,339

8 6,41 0,544 6,71 0,474

9 3,11 0,120 3,23 0,247

10 3,18 0,049 2,93 0,127

11 1,70 0,240 1,90 0,000

12 2,38 0,170 2,98 0,283

13 2,94 0,120 2,92 0,085

14 3,77 0,141 3,41 0,325

15 7,32 0,042 7,87 0,057

0,210 0,367

1,75

OLS 2

GMFR

OLS 1

Mxi

SDxi

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Myi

Rep.2 SDyi

Rep.1

Rep.2

Reference


Alternative





1 2,46 2,530 2,530 2,73 2,495 2,495 2,49 0,003

2 2,40 2,600 2,600 2,75 2,850 2,850 2,57 0,282

3 3,00 2,950 2,950 3,00 2,875 2,875 2,95 -0,074

4 3,18 3,090 3,090 3,45 3,200 3,200 3,10 0,099

5 2,86 3,020 3,020 3,08 3,270 3,270 3,02 0,245

6 4,97 4,780 4,780 4,79 4,690 4,690 4,94 -0,248

7 3,18 3,305 3,305 3,23 2,990 2,990 3,33 -0,345

8 5,64 6,025 6,025 6,04 6,375 6,375 6,29 0,083

9 2,94 3,025 3,025 2,88 3,055 3,055 3,03 0,025

10 3,11 3,145 3,145 2,75 2,840 2,840 3,16 -0,321

11 2,04 1,870 1,870 1,90 1,900 1,900 1,77 0,126

12 2,62 2,500 2,500 2,58 2,780 2,780 2,46 0,321

13 3,11 3,025 3,025 3,04 2,980 2,980 3,03 -0,050

14 3,97 3,870 3,870 3,87 3,640 3,640 3,95 -0,309

15 7,26 7,290 7,290 7,79 7,830 7,830 7,67 0,162

1 2,60 0,099 2,26 0,332 Sum = 0,000

2 2,80 0,283 2,95 0,141 RSD' = 0,230

3 2,90 0,071 2,75 0,177

4 3,00 0,127 2,95 0,354

5 3,18 0,226 3,46 0,269

6 4,59 0,269 4,59 0,141

7 3,43 0,177 2,75 0,339

8 6,41 0,544 6,71 0,474

9 3,11 0,120 3,23 0,247

10 3,18 0,049 2,93 0,127

11 1,70 0,240 1,90 0,000

12 2,38 0,170 2,98 0,283

13 2,94 0,120 2,92 0,085

14 3,77 0,141 3,41 0,325

15 7,32 0,042 7,87 0,057

Sx= 1,445 Sy= 1,571

SD(Mxi) = 1,445 SD(Myi) = 1,571

M(x) = 3,535 M(y) = 3,585

MED(x) = 3,025 MED(y) = 2,990


q (doses)= 15

p (replicates)= 2

v (df)= 13

SDwy/SDwx SDwx/Sdwy

rob. 1,75 0,571



Res.SD(My) = 0,230 = RSD' b= 1,0874 0,043 2,052 0,061 1



vd (df DEN)= 15

vn (df NUM)= 13

rob. F= 0,541

p(rob.F)= 86%

2,16037

SDyiRep.2

Rep.1

Rep.2

Mxi

SDxi

MyiRep.1




Seafood products Bi-dimensional graphic

0

1

2

3

4

5

6

7

8

9

10

0 1 2 3 4 5 6 7 8 9 10

log

(Alt

ern

ati

ve

me

tho

d)


Seafood products


y = 1,0112x - 0,2384

0,00

1,00

2,00

3,00

4,00

5,00

6,00

7,00

8,00

9,00

10,00

0,00 1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00 9,00 10,00

Re

fere

nc

e

Alternative

Seafood products-OLS2 regression





Bias D 0,215


1 0,70 0,940 1,30 1,540 0,600

2 1,30 1,450 1,30 1,450 0,000

3 1,65 1,525 2,00 1,800 0,275

4 1,93 2,065 2,34 2,360 0,295

5 1,60 1,800 1,30 1,890 0,090

6 7,74 7,425 7,68 7,650 0,225

7 3,18 3,165 3,40 3,370 0,205

8 4,30 4,240 4,20 4,215 -0,025

9 6,30 5,995 5,97 6,240 0,245

10 7,49 7,580 7,43 7,525 -0,055

11 6,08 6,265 6,66 6,680 0,415

12 1,54 1,675 2,00 1,890 0,215

13 4,41 4,555 4,68 4,775 0,220

14 5,28 5,320 5,48 5,520 0,200

15 5,63 5,620 5,70 5,745 0,125

16 4,76 4,825 4,75 4,790 -0,035

17 7,28 7,280 7,46 7,500 0,220

1 1,18 0,339 1,78 0,339

2 1,60 0,212 1,60 0,212

3 1,40 0,177 1,60 0,283

4 2,20 0,191 2,38 0,028

5 2,00 0,283 2,48 0,834

6 7,11 0,445 7,62 0,042

7 3,15 0,021 3,34 0,042

8 4,18 0,085 4,23 0,021

9 5,69 0,431 6,51 0,382

10 7,67 0,127 7,62 0,134

11 6,45 0,262 6,70 0,028

12 1,81 0,191 1,78 0,156

13 4,70 0,205 4,87 0,134

14 5,36 0,057 5,56 0,057

15 5,61 0,014 5,79 0,064

16 4,89 0,092 4,83 0,057

17 7,28 0,000 7,54 0,057

0,283 0,094

0,33

OLS 2

GMFR

OLS 1

Mxi

SDxi

SDwy/SDwx<0,5

0,5<SDwy/SDwx<2

SDwy/SDwx>2

Rep.1

Référence

Alternative

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

Myi

Rep.2 SDyi

Rep.1

Rep.2

Reference


Alternative




Reference method X Alternative method Y Y^

1 1,30 1,540 1,540 0,70 0,940 1,319

2 1,30 1,450 1,450 1,30 1,450 1,228

3 2,00 1,800 1,800 1,65 1,525 1,582

4 2,34 2,360 2,360 1,93 2,065 2,148

5 1,30 1,890 1,890 1,60 1,800 1,673

6 7,68 7,650 7,650 7,74 7,425 7,497

7 3,40 3,370 3,370 3,18 3,165 3,169

8 4,20 4,215 4,215 4,30 4,240 4,024

9 5,97 6,240 6,240 6,30 5,995 6,071

10 7,43 7,525 7,525 7,49 7,580 7,371

11 6,66 6,680 6,680 6,08 6,265 6,516

12 2,00 1,890 1,890 1,54 1,675 1,673

13 4,68 4,775 4,775 4,41 4,555 4,590

14 5,48 5,520 5,520 5,28 5,320 5,343

15 5,70 5,745 5,745 5,63 5,620 5,571

16 4,75 4,790 4,790 4,76 4,825 4,605

17 7,46 7,500 7,500 7,28 7,280 7,345

1 1,78 0,339 1,540 1,18 0,339 1,319

2 1,60 0,212 1,450 1,60 0,212 1,228

3 1,60 0,283 1,800 1,40 0,177 1,582

4 2,38 0,028 2,360 2,20 0,191 2,148

5 2,48 0,834 1,890 2,00 0,283 1,673

6 7,62 0,042 7,650 7,11 0,445 7,497

7 3,34 0,042 3,370 3,15 0,021 3,169

8 4,23 0,021 4,215 4,18 0,085 4,024

9 6,51 0,382 6,240 5,69 0,431 6,071

10 7,62 0,134 7,525 7,67 0,127 7,371

11 6,70 0,028 6,680 6,45 0,262 6,516

12 1,78 0,156 1,890 1,81 0,191 1,673

13 4,87 0,134 4,775 4,70 0,205 4,590

14 5,56 0,057 5,520 5,36 0,057 5,343

15 5,79 0,064 5,745 5,61 0,014 5,571

16 4,83 0,057 4,790 4,89 0,092 4,605

17 7,54 0,057 7,500 7,28 0,000 7,345

Sx= 2,248 Sy= 2,285

SD(Mxi) = 2,283 SD(Myi) = 2,314

M(x) = 4,408 M(y) = 4,219

MED(x) = 4,775 MED(y) = 4,555


q (doses)= 17

p (replicates)= 2

v (df)= 15

SDwy/SDwx SDwx/Sdwy

rob. 3,00 0,333

OLS2 regression

r(Mx, My) = 0,9949 SD t:H p(t:H) H Critical T

Res.SD(My) = 0,234 = RSD b= 1,0112 0,026 0,436 0,669 1

RSD * SQRT(p) = Res.SD(y) = 0,331 =sr(y) a= -0,2384 0,127 1,883 0,079 0


vd (df DEN)= 17

vn (df NUM)= 15

rob. F= 0,328

p(rob.F)= 98%

2,13145

SDyi

Rep.1

Rep.2

MyiRep.1

Rep.2

Mxi

SDxi




All products Bi-dimensional graphic

0,00

1,00

2,00

3,00

4,00

5,00

6,00

7,00

8,00

9,00

10,00

0,00 1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00 9,00 10,00

log

(Alt

ern

ati

ve

me

tho

d)


All products

Naturally contaminated samples



y = 1,0261x - 0,0741

0,00

1,00

2,00

3,00

4,00

5,00

6,00

7,00

8,00

9,00

10,00

0,00 1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00 9,00 10,00

Alt

ern

ati

ve

Reference

All products-GMFR regression





Bias D 0,150


1 2,28 2,270 2,64 2,585 0,315

2 3,40 3,350 3,61 3,640 0,290

3 4,41 4,355 4,54 4,555 0,200

4 5,34 5,320 5,49 5,530 0,210

5 6,28 6,330 6,64 6,715 0,385

6 7,32 7,360 7,67 7,770 0,410

7 4,79 4,760 4,79 4,770 0,010

8 3,58 3,570 1,70 1,480 -2,090 1254 Half creamed pasteurized milk

9 2,83 2,720 2,97 3,005 0,285

10 3,26 3,290 3,88 4,275 0,985 1371 Half creamed pasteurized milk

11 3,04 3,120 3,51 3,565 0,445

12 2,30 2,450 2,68 2,825 0,375

13 2,08 1,890 1,78 1,890 0,000

14 2,18 1,980 2,00 2,040 0,060

15 4,65 4,690 5,11 4,970 0,280

16 7,74 7,805 8,09 8,170 0,365

17 4,15 4,115 4,46 4,415 0,300

18 3,97 4,040 4,23 4,215 0,175

19 4,45 4,430 4,59 4,535 0,105

20 4,81 4,775 5,00 4,890 0,115

21 7,48 7,480 7,67 7,630 0,150

22 5,04 5,040 5,26 5,220 0,180

23 4,08 4,080 4,08 4,080 0,000

24 5,61 5,635 5,17 5,461 -0,175

25 3,45 3,415 3,20 3,175 -0,240

26 3,34 3,370 3,41 3,450 0,080

27 5,20 5,155 5,61 5,505 0,350

28 3,79 3,820 3,75 3,875 0,055

29 5,08 5,080 5,08 5,140 0,060

30 5,23 5,190 4,43 4,385 -0,805 1180 Steak

31 5,48 5,400 5,28 5,205 -0,195

32 4,98 5,065 5,00 4,960 -0,105

33 8,58 8,570 7,45 7,225 -1,345 1246 Dry sausage

34 2,32 2,300 2,81 2,810 0,510

35 3,26 3,270 3,48 3,525 0,255

36 4,30 4,290 4,43 4,440 0,150

37 5,32 5,320 5,54 5,565 0,245

38 6,32 6,275 6,61 6,560 0,285

39 6,76 6,745 6,95 6,900 0,155

40 2,40 2,240 2,56 2,320 0,080

41 3,60 3,600 1,30 1,750 -1,850 1138 Frozen artichoke hearts

42 8,28 8,195 8,45 8,465 0,270

43 5,89 5,985 6,15 6,245 0,260

44 4,69 4,690 4,00 3,950 -0,740

45 4,20 4,190 3,75 3,675 -0,515

46 2,89 2,875 2,68 2,565 -0,310

47 4,60 4,515 3,62 3,535 -0,980 1370 Guacamole

48 0,70 0,940 1,30 1,540 0,600

49 1,30 1,450 1,30 1,450 0,000

50 1,65 1,525 2,00 1,800 0,275

51 1,93 2,065 2,34 2,360 0,295

52 1,60 1,800 1,30 1,890 0,090

53 7,74 7,425 7,68 7,650 0,225

54 3,18 3,165 3,40 3,370 0,205

55 4,30 4,240 4,20 4,215 -0,025

56 6,30 5,995 5,97 6,240 0,245

57 7,49 7,580 7,43 7,525 -0,055

58 6,08 6,265 6,66 6,680 0,415

59 1,54 1,675 2,00 1,890 0,215

60 4,41 4,555 4,68 4,775 0,220

61 5,28 5,320 5,48 5,520 0,200

62 5,63 5,620 5,70 5,745 0,125

63 4,76 4,825 4,75 4,790 -0,035

64 7,28 7,280 7,46 7,500 0,220

65 2,46 2,530 2,73 2,495 -0,035

66 2,40 2,600 2,75 2,850 0,250

67 3,00 2,950 3,00 2,875 -0,075

68 3,18 3,090 3,45 3,200 0,110

69 2,86 3,020 3,08 3,270 0,250

70 4,97 4,780 4,79 4,690 -0,090

71 3,18 3,305 3,23 2,990 -0,315

72 5,64 6,025 6,04 6,375 0,350

73 2,94 3,025 2,88 3,055 0,030

74 3,11 3,145 2,75 2,840 -0,305

75 2,04 1,870 1,90 1,900 0,030

76 2,62 2,500 2,58 2,780 0,280

77 3,11 3,025 3,04 2,980 -0,045

78 3,97 3,870 3,87 3,640 -0,230

79 7,26 7,290 7,79 7,830 0,540

Rep.1 Mxi

Seafo

od p

roducts

Bakery

and o

ther p

roducts

MyiRep.1

Milk

pro

ducts

Meat p

roducts

Fru

it and v

egeta

ble

s




Reference method Alternative method

1 2,26 0,014 2,53 0,078

2 3,30 0,071 3,67 0,042

3 4,30 0,078 4,57 0,021

4 5,30 0,028 5,57 0,057

5 6,38 0,071 6,79 0,106

6 7,40 0,057 7,87 0,141

7 4,73 0,042 4,75 0,028

8 3,56 0,014 1,26 0,311

9 2,61 0,156 3,04 0,049

10 3,32 0,042 4,67 0,559

11 3,20 0,113 3,62 0,078

12 2,60 0,212 2,97 0,205

13 1,70 0,269 2,00 0,156

14 1,78 0,283 2,08 0,057

15 4,73 0,057 4,83 0,198

16 7,87 0,092 8,25 0,113

17 4,08 0,049 4,37 0,064

18 4,11 0,099 4,20 0,021

19 4,41 0,028 4,48 0,078

20 4,74 0,049 4,78 0,156

21 7,48 0,000 7,59 0,057

22 5,04 0,000 5,18 0,057

23 4,08 0,000 4,08 0,000

24 5,66 0,035 5,75 0,409

25 3,38 0,049 3,15 0,035

26 3,40 0,042 3,49 0,057

27 5,11 0,064 5,40 0,148

28 3,85 0,042 4,00 0,177

29 5,08 0,000 5,20 0,085

30 5,15 0,057 4,34 0,064

31 5,32 0,113 5,13 0,106

32 5,15 0,120 4,92 0,057

33 8,56 0,014 7,00 0,318

34 2,28 0,028 2,81 0,000

35 3,28 0,014 3,57 0,064

36 4,28 0,014 4,45 0,014

37 5,32 0,000 5,59 0,035

38 6,23 0,064 6,51 0,071

39 6,73 0,021 6,85 0,071

40 2,08 0,226 2,08 0,339

41 3,60 0,000 2,20 0,636

42 8,11 0,120 8,48 0,021

43 6,08 0,134 6,34 0,134

44 4,69 0,000 3,90 0,071

45 4,18 0,014 3,60 0,106

46 2,86 0,021 2,45 0,163

47 4,43 0,120 3,45 0,120

48 1,18 0,339 1,78 0,339

49 1,60 0,212 1,60 0,212

50 1,40 0,177 1,60 0,283

51 2,20 0,191 2,38 0,028

52 2,00 0,283 2,48 0,834

53 7,11 0,445 7,62 0,042

54 3,15 0,021 3,34 0,042

55 4,18 0,085 4,23 0,021

56 5,69 0,431 6,51 0,382

57 7,67 0,127 7,62 0,134

58 6,45 0,262 6,70 0,028

59 1,81 0,191 1,78 0,156

60 4,70 0,205 4,87 0,134

61 5,36 0,057 5,56 0,057

62 5,61 0,014 5,79 0,064

63 4,89 0,092 4,83 0,057

64 7,28 0,000 7,54 0,057

65 2,60 0,099 2,26 0,332

66 2,80 0,283 2,95 0,141

67 2,90 0,071 2,75 0,177

68 3,00 0,127 2,95 0,354

69 3,18 0,226 3,46 0,269

70 4,59 0,269 4,59 0,141

71 3,43 0,177 2,75 0,339

72 6,41 0,544 6,71 0,474

73 3,11 0,120 3,23 0,247

74 3,18 0,049 2,93 0,127

75 1,70 0,240 1,90 0,000

76 2,38 0,170 2,98 0,283

77 2,94 0,120 2,92 0,085

78 3,77 0,141 3,41 0,325

79 7,32 0,042 7,87 0,057

SDyiRep.2 SDxi Rep.2

0,105 0,157

1,50

OLS 2

GMFR

OLS 1 Alternative

rob.SDwx= rob.SDwy=

SDwy/SDwx =

x-axis y-axis

ReferenceSDwy/SDwx<0,5

Alternative0,5<SDwy/SDwx<2

SDwy/SDwx>2 Référence

Alternative

Reference





1 2,28 2,270 2,270 2,64 2,585 2,585 2,26 0,330

2 3,40 3,350 3,350 3,61 3,640 3,640 3,36 0,277

3 4,41 4,355 4,355 4,54 4,555 4,555 4,39 0,160

4 5,34 5,320 5,320 5,49 5,530 5,530 5,38 0,145

5 6,28 6,330 6,330 6,64 6,715 6,715 6,42 0,294

6 7,32 7,360 7,360 7,67 7,770 7,770 7,48 0,292

7 4,79 4,760 4,760 4,79 4,770 4,770 4,81 -0,040

8 3,58 3,570 3,570 1,70 1,480 1,480 3,59 -2,109

9 2,83 2,720 2,720 2,97 3,005 3,005 2,72 0,288

10 3,26 3,290 3,290 3,88 4,275 4,275 3,30 0,973

11 3,04 3,120 3,120 3,51 3,565 3,565 3,13 0,438

12 2,30 2,450 2,450 2,68 2,825 2,825 2,44 0,385

13 2,08 1,890 1,890 1,78 1,890 1,890 1,87 0,025

14 2,18 1,980 1,980 2,00 2,040 2,040 1,96 0,082

15 4,65 4,690 4,690 5,11 4,970 4,970 4,74 0,232

16 7,74 7,805 7,805 8,09 8,170 8,170 7,93 0,235

17 4,15 4,115 4,115 4,46 4,415 4,415 4,15 0,267

18 3,97 4,040 4,040 4,23 4,215 4,215 4,07 0,144

19 4,45 4,430 4,430 4,59 4,535 4,535 4,47 0,063

20 4,81 4,775 4,775 5,00 4,890 4,890 4,83 0,064

21 7,48 7,480 7,480 7,67 7,630 7,630 7,60 0,029

22 5,04 5,040 5,040 5,26 5,220 5,220 5,10 0,122

23 4,08 4,080 4,080 4,08 4,080 4,080 4,11 -0,032

24 5,61 5,635 5,635 5,17 5,461 5,461 5,71 -0,248

25 3,45 3,415 3,415 3,20 3,175 3,175 3,43 -0,255

26 3,34 3,370 3,370 3,41 3,450 3,450 3,38 0,066

27 5,20 5,155 5,155 5,61 5,505 5,505 5,22 0,289

28 3,79 3,820 3,820 3,75 3,875 3,875 3,85 0,029

29 5,08 5,080 5,080 5,08 5,140 5,140 5,14 0,001

30 5,23 5,190 5,190 4,43 4,385 4,385 5,25 -0,866

31 5,48 5,400 5,400 5,28 5,205 5,205 5,47 -0,262

32 4,98 5,065 5,065 5,00 4,960 4,960 5,12 -0,163

33 8,58 8,570 8,570 7,45 7,225 7,225 8,72 -1,495

34 2,32 2,300 2,300 2,81 2,810 2,810 2,29 0,524

35 3,26 3,270 3,270 3,48 3,525 3,525 3,28 0,244

36 4,30 4,290 4,290 4,43 4,440 4,440 4,33 0,112

37 5,32 5,320 5,320 5,54 5,565 5,565 5,38 0,180

38 6,32 6,275 6,275 6,61 6,560 6,560 6,36 0,195

39 6,76 6,745 6,745 6,95 6,900 6,900 6,85 0,053

40 2,40 2,240 2,240 2,56 2,320 2,320 2,22 0,096

41 3,60 3,600 3,600 1,30 1,750 1,750 3,62 -1,870

42 8,28 8,195 8,195 8,45 8,465 8,465 8,33 0,130

43 5,89 5,985 5,985 6,15 6,245 6,245 6,07 0,178

44 4,69 4,690 4,690 4,00 3,950 3,950 4,74 -0,788

45 4,20 4,190 4,190 3,75 3,675 3,675 4,23 -0,550

46 2,89 2,875 2,875 2,68 2,565 2,565 2,88 -0,311

47 4,60 4,515 4,515 3,62 3,535 3,535 4,56 -1,024

48 0,70 0,940 0,940 1,30 1,540 1,540 0,89 0,650

49 1,30 1,450 1,450 1,30 1,450 1,450 1,41 0,036

50 1,65 1,525 1,525 2,00 1,800 1,800 1,49 0,309

51 1,93 2,065 2,065 2,34 2,360 2,360 2,04 0,315

52 1,60 1,800 1,800 1,30 1,890 1,890 1,77 0,117

53 7,74 7,425 7,425 7,68 7,650 7,650 7,54 0,105

54 3,18 3,165 3,165 3,40 3,370 3,370 3,17 0,196

55 4,30 4,240 4,240 4,20 4,215 4,215 4,28 -0,062

56 6,30 5,995 5,995 5,97 6,240 6,240 6,08 0,162

57 7,49 7,580 7,580 7,43 7,525 7,525 7,70 -0,179

58 6,08 6,265 6,265 6,66 6,680 6,680 6,35 0,325

59 1,54 1,675 1,675 2,00 1,890 1,890 1,64 0,245

60 4,41 4,555 4,555 4,68 4,775 4,775 4,60 0,175

61 5,28 5,320 5,320 5,48 5,520 5,520 5,38 0,135

62 5,63 5,620 5,620 5,70 5,745 5,745 5,69 0,052

63 4,76 4,825 4,825 4,75 4,790 4,790 4,88 -0,087

64 7,28 7,280 7,280 7,46 7,500 7,500 7,40 0,104

65 2,46 2,530 2,530 2,73 2,495 2,495 2,52 -0,027

66 2,40 2,600 2,600 2,75 2,850 2,850 2,59 0,256

67 3,00 2,950 2,950 3,00 2,875 2,875 2,95 -0,078

68 3,18 3,090 3,090 3,45 3,200 3,200 3,10 0,103

69 2,86 3,020 3,020 3,08 3,270 3,270 3,02 0,245

70 4,97 4,780 4,780 4,79 4,690 4,690 4,83 -0,141

71 3,18 3,305 3,305 3,23 2,990 2,990 3,32 -0,327

72 5,64 6,025 6,025 6,04 6,375 6,375 6,11 0,267

73 2,94 3,025 3,025 2,88 3,055 3,055 3,03 0,025

74 3,11 3,145 3,145 2,75 2,840 2,840 3,15 -0,313

75 2,04 1,870 1,870 1,90 1,900 1,900 1,84 0,055

76 2,62 2,500 2,500 2,58 2,780 2,780 2,49 0,289

77 3,11 3,025 3,025 3,04 2,980 2,980 3,03 -0,050

78 3,97 3,870 3,870 3,87 3,640 3,640 3,90 -0,257

79 7,26 7,290 7,290 7,79 7,830 7,830 7,41 0,424

Rep.1Mxi MyiRep.1




Reference method Alternative method

1 2,26 0,014 2,53 0,078 Sum = 0,000

2 3,30 0,071 3,67 0,042 RSD' = 0,477

3 4,30 0,078 4,57 0,021

4 5,30 0,028 5,57 0,057

5 6,38 0,071 6,79 0,106

6 7,40 0,057 7,87 0,141

7 4,73 0,042 4,75 0,028

8 3,56 0,014 1,26 0,311

9 2,61 0,156 3,04 0,049

10 3,32 0,042 4,67 0,559

11 3,20 0,113 3,62 0,078

12 2,60 0,212 2,97 0,205

13 1,70 0,269 2,00 0,156

14 1,78 0,283 2,08 0,057

15 4,73 0,057 4,83 0,198

16 7,87 0,092 8,25 0,113

17 4,08 0,049 4,37 0,064

18 4,11 0,099 4,20 0,021

19 4,41 0,028 4,48 0,078

20 4,74 0,049 4,78 0,156

21 7,48 0,000 7,59 0,057

22 5,04 0,000 5,18 0,057

23 4,08 0,000 4,08 0,000

24 5,66 0,035 5,75 0,409

25 3,38 0,049 3,15 0,035

26 3,40 0,042 3,49 0,057

27 5,11 0,064 5,40 0,148

28 3,85 0,042 4,00 0,177

29 5,08 0,000 5,20 0,085

30 5,15 0,057 4,34 0,064

31 5,32 0,113 5,13 0,106

32 5,15 0,120 4,92 0,057

33 8,56 0,014 7,00 0,318

34 2,28 0,028 2,81 0,000

35 3,28 0,014 3,57 0,064

36 4,28 0,014 4,45 0,014

37 5,32 0,000 5,59 0,035

38 6,23 0,064 6,51 0,071

39 6,73 0,021 6,85 0,071

40 2,08 0,226 2,08 0,339

41 3,60 0,000 2,20 0,636

42 8,11 0,120 8,48 0,021

43 6,08 0,134 6,34 0,134

44 4,69 0,000 3,90 0,071

45 4,18 0,014 3,60 0,106

46 2,86 0,021 2,45 0,163

47 4,43 0,120 3,45 0,120

48 1,18 0,339 1,78 0,339

49 1,60 0,212 1,60 0,212

50 1,40 0,177 1,60 0,283

51 2,20 0,191 2,38 0,028

52 2,00 0,283 2,48 0,834

53 7,11 0,445 7,62 0,042

54 3,15 0,021 3,34 0,042

55 4,18 0,085 4,23 0,021

56 5,69 0,431 6,51 0,382

57 7,67 0,127 7,62 0,134

58 6,45 0,262 6,70 0,028

59 1,81 0,191 1,78 0,156

60 4,70 0,205 4,87 0,134

61 5,36 0,057 5,56 0,057

62 5,61 0,014 5,79 0,064

63 4,89 0,092 4,83 0,057

64 7,28 0,000 7,54 0,057

65 2,60 0,099 2,26 0,332

66 2,80 0,283 2,95 0,141

67 2,90 0,071 2,75 0,177

68 3,00 0,127 2,95 0,354

69 3,18 0,226 3,46 0,269

70 4,59 0,269 4,59 0,141

71 3,43 0,177 2,75 0,339

72 6,41 0,544 6,71 0,474

73 3,11 0,120 3,23 0,247

74 3,18 0,049 2,93 0,127

75 1,70 0,240 1,90 0,000

76 2,38 0,170 2,98 0,283

77 2,94 0,120 2,92 0,085

78 3,77 0,141 3,41 0,325

17 7,32 0,042 7,87 0,057

SDyiRep.2 Rep.2SDxi




Sx= 1,804 Sy= 1,851

SD(Mxi) = 1,804 SD(Myi) = 1,851

M(x) = 4,293 M(y) = 4,331

MED(x) = 4,190 MED(y) = 4,215


q (doses)= 79

p (replicates)= 2

v (df)= 77

SDwy/SDwx SDwx/Sdwy

rob. 1,50 0,667



Res.SD(My) = 0,477 = RSD' b= 1,0261 0,030 0,872 0,386 1



vd (df DEN)= 79

vn (df NUM)= 77

rob. F= 36,321

p(rob.F)= 0%

1,99125




Annex 6 - Detection and quantification limits




Inoculation level

Inoculum (cfu/ml)

Replicate

1 2 3 4 5 6

0 0 <1 <1 <1 <1 <1 <1

0,5 0,5 2 2 <1 <1 <1 <1

1 0,8 <1 <1 <1 4 2 2

5 4,3 10 14 6 10 4 4

10 9,5 22 12 18 22 24 18

50 50,4 70 50 94 116 84 68

Inoculation level

Number of positive samples

Standard deviation (S0)

Bias X0

(médiane des Xoi)

0 0 / /

0,5 2 0,000 2

1 3 1,155 2

5 6 4,000 8

10 6 4,320 20

50 6 23,028 77

MICROVAL ISO 16140:2003 Validation of SimPlate Total … TPC-CI MicroVal... · The results are...

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