Total Amino Acid Composition - dla-lvu.de Reports 2015/Report DLA 42-2015 Total Amino... · From 11...
Transcript of Total Amino Acid Composition - dla-lvu.de Reports 2015/Report DLA 42-2015 Total Amino... · From 11...
May 2016 DLA 42/2015 - Total Amino Acid Composition
DLADienstleistung
LebensmittelAnalytik GbR
Evaluation Reportproficiency test
DLA 42/2015
Total Amino Acid Composition
in Infant Food
Dienstleistung Lebensmittel Analytik GbRWaldemar-Bonsels-Weg 17022926 Ahrensburg, Germany
[email protected] www.dla-lvu.de
Coordinator of this PT: Dr. Matthias Besler
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Inhalt / Content1. Introduction.........................................................32. Realisation..........................................................3
2.1 Test material...................................................32.1.1 Homogeneity....................................................42.2 Test.............................................................42.3 Submission of results............................................4
3. Evaluation...........................................................53.1 Assigned value...................................................53.2 Standard deviation...............................................53.3 Outliers.........................................................53.4 Target standard deviation........................................53.4.1 General model (Horwitz)........................................63.4.2 Value by precision experiment..................................63.4.3 Value by perception............................................83.5 z-Score..........................................................83.6 z'-Score.........................................................83.7 Quotient ........................................................93.8 Standard uncertainty.............................................9
4. Results.............................................................104.1 L-Alanine in g/100g.............................................114.2 L-Arginine in g/100g............................................134.3 L-Aspartic Acid in g/100g.......................................154.4 L-Cyst(e)ine in g/100g..........................................174.5 L-Glutaminic Acid in g/100g.....................................194.6 Glycine in g/100g...............................................214.7 L-Histidine in g/100g...........................................234.8 L-Isoleucine in g/100g..........................................254.9 L-Leucine in g/100g.............................................274.10 L-Lysine in g/100g.............................................294.11 L-Methionine in g/100g.........................................314.12 L-Phenylalanine in g/100g......................................334.13 L-Proline in g/100g............................................354.14 L-Serine in g/100g.............................................374.15 L-Threonine in g/100g..........................................394.16 L-Tryptophan in g/100g.........................................414.17 L-Tyrosine in g/100g...........................................434.18 L-Valine in g/100g.............................................45
5. Documentation.......................................................475.1 Primary data....................................................475.2 Homogeneity.....................................................525.3 Analytical Methods..............................................53
6. Index of participant laboratories...................................607. Index of references.................................................61
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1. Introduction
The participation in proficiency testing schemes is an essential elementof the quality-management-system of every laboratory testing food andfeed, cosmetics and food contact materials. The implementation ofproficiency tests enables the participating laboratories to prove theirown analytical competence under realistic conditions. At the same timethey receive valuable data regarding the validity of the particulartesting method. The purpose of DLA is to offer proficiency tests for selected parametersin concentrations with practical relevance.Realisation and evaluation of the present proficiency test follows thetechnical requirements of DIN EN ISO/IEC 17043 (2010) and DIN ISO13528:2009 (6).
2. Realisation
2.1 Test material
The test material is a common in commerce infant food formula based onwhey proteins with < 20% protein content from a EU supplier. The powderwas mixed and homogenized. Afterwards the samples were packagedlightproof in portions to approximately 10 g. The portions were numberedchronologically.
The composition (list of ingredients) of the samples is given in table 1.
Table 1: Composition of DLA-Samples
Infant Food Milk Formula
Ingredients: Demineralized whey powder, vegetable oils, lactose, skimmed milk powder, galacto-oligosaccharides (from milk), whey protein concentrate, fructo-oligosaccharides, calcium carbonate, potassium citrate, potassium chloride, fish oil, magnesium chloride, calcium phosphate, vitamin C, soylecithin, cholin chloride, taurine, nucleotides (uridine-, cytidine-, adenosine-, inosin-, guanosin-5-monophosphate),iron sulfate, vitamin E, zinc sulfate, inositol, niacin, L-tryptophan, L-carni-tin, calcium-D-pantothenate, folic acid, copper sulfate, vitamin A, biotin, vit-amin B12, vitamin B1, vitamin D3, vitamin B6, manganese sulfate, potassium iodi-de, vitamin K1, sodium selenite
Nutrients per 100 g: protein 9,7 g, carbohydrates 54 g thereof sugar 53 g, fat 25 g
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2.1.1 Homogeneity
Homogeneity of the test material was checked by 5fold determination ofmagnesium by ICP-OES. With a repeatability standard deviation of 2,3 %the homogeneity of the test material was considered acceptable. The re-sults are given in the documentation.
The calculation of the repeatability standard deviation of the partici-pants was also used as an indicator of homogeneity. For L-lysine it was2,6 % and for L-threonine 2,4 % and in the range of common relative re-peatability standard deviations of methods for amino acid determination(13-16). The repeatability standard deviation of the participants forboth parameters is given in the documentation.
Additionally in the documentation the portion numbers are graphically as-signed to the results of L-alanine. There is no trend recognizable in theresults which could suggest inhomogeneity.
2.2 Test
Two portions of test material were sent to every participating laboratoryin the 40th week of 2015. The testing method was optional. The testsshould be finished at 13th November 2015.
2.3 Submission of results
The participants submitted their results in provided standard forms byemail.The final concentration of the parameters as mean of both numberedsamples (as far as available) was used for each statistical evaluation. Queried and documented were single results, recovery and the testingmethods used. From 11 participants of the PTs total amino acid composition (DLA42/2015) and free amino acids (DLA 43/2015) 7 and 9 participantssubmitted results, respectively. One participant submitted no results.All other participants submitted their results in time.
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3. Evaluation
3.1 Assigned value
Because the analysed material was no certified reference material therobust mean of the submitted results was used as assigned value X (6).The distribution of submitted results showed no hint for bimodaldistribution or other reasons for a higher variability.The statistical evaluation is performed when there are at least 7 resultsfor a parameter.This was the case for all parameters except for cysteine/cystine andtryptophan. Therefore for the parameters cysteine/cystine and tryptophanno statistical evaluation was done.Single results giving values outside the measuring range of theparticipating laboratory were considered for statistical evaluation (e.g.results given as > 25 mg/kg and < 2,5 mg/kg, respectively) when a resultindicating „>“ is above and a result indicating „<“ is below the targetrange.
3.2 Standard deviation
For comparison to the target standard deviation a robust standard devi-ation (Sx) was calculated (6).
3.3 Outliers
Statistical outliers were determined by Mandel´s-H-Statistic for 95%significance niveau (5). Detected outliers were stated for informationonly, when z-score was < -2 or > 2.
3.4 Target standard deviation
The target standard deviation of the assigned value is determinedaccording to the following methods.
In general the Horwitz target standard deviation is suitable for thestatistical evaluation of interlaboratory tests where differentanalytical methods are applied. The standard deviation from precisionexperiments are derived from proficiency tests where a specificanalytical method is mandatory. For information the z-scores from bothmodels were given in the result tables, if available.
For the valuation of the following parameters the target standard devia-tion according to the general model of horwitz was applied (3.4.1): L-alanine, L-arginine, glycine, L-isoleucine, L-leucine, L-lysine, L-phe-nylalanine, L-serine, L-threonine and L-valine.
For the valuation of the following parameters the target standard devia-tion from precision experiments (s. 3.4.2) (German official ASU §64 me-
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thod: 14) was applied: L-aspartic acid, L-glutaminic acid, L-histidine,L-methionine, L-proline and L-tyrosine.
Additionally the standard uncertainty was considered for L-arginine andL-serine and for L-histidine and L-tyrosine, respectively, by valuatingwith z'-score (see 3.6).
For L-cysteine/L-cystine and L-tryptophan there were < 7 quantitativeresults, thus no statistical evaluation could be done
3.4.1 General model (Horwitz)
The relative target standard deviation in % of the assigned value isderived from following equation (Horwitz)
σ (%) = 2(1-0,5logX)
From the result the target standard deviation is calculated
σ = X * σ (%) / 100.
3.4.2 Value by precision experiment
Using the reproducibility standard deviation σR and the repeatabilitystandard deviation σr of a precision experiment the between-laboratoriesstandard deviation can be calculated σL :
L= R2− r
2 .
And then, using the number of replicate measurements n, each participantis to perform, the target standard deviation for proficiency assessmentis calculated :
= L2 r
2/n .
The target standard deviations given in table 2 were calculated from theprecision data of the respective methods.
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Table 2: Relative target standard deviations (RSD) according to precisionexperiments (14, 15, 16)
Parameter Matrix RSD σ Method / Literature
L-Alanine Dietetic food 4,7 % 1 ASU §64 L 49.07-2 (14)
L-Arginine Dietetic food 6,6 % 1 ASU §64 L 49.07-2 (14)
L-Aspartic acid Dietetic food 7,3 % 1 ASU §64 L 49.07-2 (14)
L-Cyst(e)ine Dietetic foodProtein concentrate
14,2 % 1
12,1 %ASU §64 L 49.07-2 (14)VO 152/2009/EG (16)
L-Glutaminic acid Dietetic food 4,8 % 1 ASU §64 L 49.07-2 (14)
Glycine Dietetic food 6,5 % 1 ASU §64 L 49.07-2 (14)
L-Histidine Dietetic food 10,6 % 1 ASU §64 L 49.07-2 (14)
L-Isoleucine Dietetic food 4,9 % 1 ASU §64 L 49.07-2 (14)
L-Methionine Dietetic foodProtein concentrate
6,1 % 1
12,9 %ASU §64 L 49.07-2 (14)VO 152/2009/EG (16)
L-Leucine Dietetic food 5,3 % 1 ASU §64 L 49.07-2 (14)
L-Lysine Dietetic foodProtein concentrate
8,8 % 1
2,2 %ASU §64 L 49.07-2 (14)VO 152/2009/EG (16)
L-Phenylalanine Dietetic food - ASU §64 L 49.07-2 (14)
L-Proline Dietetic food 7,7 % 1 ASU §64 L 49.07-2 (14)
L-Serine Dietetic food 4,2 % 1 ASU §64 L 49.07-2 (14)
L-Threonine Dietetic foodProtein concentrate
5,5 % 1
3,0 %ASU §64 L 49.07-2 (14)VO 152/2009/EG (16)
L-Tryptophan Dietetic food 6,8 % 1 ASU §64 L 49.07-3 (15)
L-Tyrosine Dietetic food 6,5 % 1 ASU §64 L 49.07-2 (14)
L-Valine Dietetic food 5,8 % 1 ASU §64 L 49.07-2 (14)1 values given/applied in the evaluation (s. chapter 4)
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3.4.3 Value by perception
The target standard deviation for proficiency assessment can be set at avalue that corresponds to the level of performance that the coordinatorwould wish laboratories to be able to achieve (6).
For the present evaluation of results the target standard deviation ac-cording to Horwitz was applied for L-alanine, L-arginine, glycine, L-i-soleucine, L-leucine, L-lysine, L-phenylalanine, L-serine, L-threonine and L-valine (3.4.1) and the target standard deviation from precision experiments was applied for L-aspartic acid, L-glutaminic acid, L-histi-dine, L-methionine, L-proline and L-tyrosine (3.4.2).
Additionally the standard uncertainty was considered for L-arginine andL-serine and for L-histidine and L-tyrosine, respectively, by valuatingwith z'-score (see 3.6).
3.5 z-Score
To assess the results of the participants the z-score is used. Itindicates about which multiple of the target standard deviation ( σ )the result (x) of the participant is deviating from the assigned value(X) (6).Participants’ z-scores were derived as:
z = (x – X) / σ ;
the requirements for the analytical performance are generally consideredas fulfilled if
-2 ≤ z ≤ 2 .
3.6 z'-Score
The z'-score can be used for the valuation of the results of theparticipants, in cases the standard uncertainty has to be considered (s.3.8). The z'-score represents the relation of the deviation of the result(x) of the participant from the respective assigned value (X) to thesquare root of quadrat sum of the target standard deviation ( σ̂ ) andthe standard uncertainty (Ux) (6).
Participants’ z'-scores are derived as:
In the following we define the denominator as the target standarddeviation σ '.
The requirements for the analytical performance are generally considered
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as fulfilled if
-2 ≤ z' ≤ 2 .
The z'-Score was used for the analytes L-arginine, L-serine, L-histidineand L-tyrosine by valuating with z'-score (see also 3.7 and 3.8).
3.7 Quotient S x /
Following the Horrat-value the results of a proficiency-test (PT) can beconsidered convincing, if the quotient of robust standard deviation andtarget standard deviation does not exceed the value of 2.A value > 2 means an insufficient precision, i.e. the analytical methodis too variable, or the variation between the test participants is higherthan estimated. Thus the comparability of the results is not given (11).In the present proficiency tests the quotients Sx/ σ̂ were
In the present proficiency test the quotient Sx/ σ̂ of all parametersexcept L-arginine, L-serine, L-histidine and L-tyrosine was below 2,0.For L-arginine, L-serine, L-histidine and L-tyrosine the quotients Sx/ σ̂were clearly above 2,0. Therefore evaluation of these parameters wasdone according to 3.6 by z'-Scores. The resulting quotients Sx/ σ̂ ' werebelow 2,0 then.
3.8 Standard uncertainty
The assigned value X has a standard uncertainty u X that depends on theanalytical method, differences between the analytical methods used, thetest material, the number of participant laboratories and perhaps onother factors. The standard uncertainty u X for this PT is calculatedas follows (6).
u X=1,25∗S x / p
If u X ≤ 0,3∗ the standard uncertainty of the assigned value needsnot to be included in the interpretation of the results of the PT (6).Values exceeding 0,3 imply, that the target standard deviation could betoo low with respect to the standard uncertainty of the assigned value.
In the present proficiency tests the quotients Ux/ σ̂ were for allparameters except L-arginine, L-serine, L-histidine and L-tyrosinebetween 0,26 and 0,74. For L-arginine, L-serine, L-histidine and L-tyrosine the quotients were between 1,2 and 1,5. At the same time thequotients Sx/ σ̂ were > 2,0 for L-arginine, L-serine, L-histidine and L-tyrosine. Therefore the target range for these parameters was extendedaccording 3.6 z'-score considering the standard uncertainty.
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4. Results
All following tables are anonymized. With the delivering of theevaluation-report the participants are informed about their individualevaluation-number. In the first table the characteristics are listed:
Statistic Data
Number of results
Number of outliers
Mean
Median
Robust mean (X)
Robust standard deviation (Sx)
Target range:
Target standard deviation σ̂ or σ̂ '
Target standard deviation for information
lower limit of target range (X - 2 σ̂ ) or (X - 2 σ ') *
upper limit of target range (X + 2 σ ) or (X + 2 σ ') *
Quotient Sx/ σ '
Standard uncertainty uX
Quotient u X / '
Number of results in the target range
* Target range is calculated with z-score or z'-score
In the second table the individual results of the participatinglaboratories are listed:
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z-Score Hinweis
Remark
Auswerte- nummer Parameter
[Einheit / Unit]
Abweichung [Einheit / Unit]
z-Score (Info)
Evaluation number
Deviation [Einheit / Unit]
σ̂
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.1 L-Alanine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 1: Ergebnisse L-AlaninFig. 1: Results L-Alanine
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Statistic DataNumber of results 7Number of outliers 1Mean 0,436Median 0,430Robust Mean (X) 0,432
0,0150Target range:Target standard deviation 0,0196
0,0203
lower limit of target range 0,393upper limit of target range 0,472
0,77
0,00711
0,36
Results in the target range 6Percent in the target range 86
Robust standard deviation (Sx)
Target standard deviation ASU (for Information)
Quotient Sx/ Standard uncertainty ux
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Alanin / L-Alanine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 2: Z-Scores L-AlaninFig. 2: Z-Scores L-Alanine
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4 7 2 5 1 3 6-3
-2
-1
0
1
2
3
z-Score
Auswertenummer / evaluation number
z-Score Hinweis
Remark
1 0,432 -0,0004 0,0 0,02 0,43 -0,0024 -0,1 -0,13 0,4425 0,0101 0,5 0,54 0,413 -0,0194 -1,0 -1,05 0,43 -0,0024 -0,1 -0,16 0,48 0,0476 2,4 2,3 Ausreisser / Outlier
7 0,4245 -0,0079 -0,4 -0,4
Auswerte- nummer
L-Alanin / L-Alanin [g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
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4.2 L-Arginine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 3: Ergebnisse L-ArgininFig. 3: Results L-Arginine
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Statistic DataNumber of results 7Number of outliers 0Mean 0,282Median 0,290Robust Mean (X) 0,282
0,0384Target range:Target standard deviation ' 0,0227
0,0186
lower limit of target range 0,236upper limit of target range 0,327
1,69
0,0181
0,80
Results in the target range 5Percent in the target range 71
Robust standard deviation (Sx)
Target standard deviation ASU (for Information)
Quotient Sx/ 'Standard uncertainty ux
Quotient ux / '
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Arginin / L-Arginine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 4: Z'-Scores L-ArgininFig. 4: Z'-Scores L-Arginine
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z'-Score Hinweis
Remark
1 0,266 -0,0159 -0,7 -0,92 0,33 0,0481 2,1 2,63 0,23 -0,0519 -2,3 -2,84 0,256 -0,0259 -1,1 -1,45 0,29 0,0081 0,4 0,46 0,31 0,0281 1,2 1,57 0,291 0,0091 0,4 0,5
Auswerte- nummer
L-Arginin / L-Arginine
[g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
3 4 1 5 7 6 2-3
-2
-1
0
1
2
3
z'-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.3 L-Aspartic Acid in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 5: Ergebnisse L-AsparaginsäureFig. 5: Results L-Aspartic Acid
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Statistic DataNumber of results 7Number of outliers 0Mean 0,921Median 0,910Robust Mean (X) 0,915
0,0369Target range:Target standard deviation 0,0665
0,0371
lower limit of target range 0,782upper limit of target range 1,05
0,55
0,0174
0,26
Results in the target range 7Percent in the target range 100
Robust standard deviation (Sx)
Target standard deviation Horwitz (for Information)
Quotient Sx/ Standard uncertainty ux
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,20
0,40
0,60
0,80
1,00
1,20
1,40
Ergebnisse / Results
L-Asparagin-säure / L-Aspartic Acid [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 6: Z-Scores L-AsparaginsäureFig. 6: Z-Scores L-Aspartic Acid
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z-Score Hinweis
Remark
1 0,929 0,0137 0,2 0,42 0,91 -0,0053 -0,1 -0,13 0,88 -0,0353 -0,5 -1,04 0,876 -0,0393 -0,6 -1,15 0,91 -0,0053 -0,1 -0,16 1,01 0,0947 1,4 2,67 0,9315 0,0162 0,2 0,4
Auswerte- nummer
L-Asparaginsäure / L-Aspartic Acid
[g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
4 3 5 2 1 7 6-3
-2
-1
0
1
2
3
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.4 L-Cyst(e)ine in g/100g
Vergleichsuntersuchung / Proficiency Test
Due to the low number of results <7 no statistical evaluation was done.
Abb. 7: Ergebnisse L-CystinFig. 7: Results L-Cystine
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1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Cystin / L-Cystine [g/100g]
Median
Auswertenummer / evaluation number
Statistic DataNumber of results 4Number of outliers 0Mean 0,180Median 0,180Robust Mean (X) 0,180
0,0410Target range:Target standard deviation lower limit of target rangeupper limit of target range
Results in the target rangePercent in the target range
Robust standard deviation (Sx)
Quotient Sx/ Standard uncertainty ux
Quotient ux /
σ̂
σ̂
σ̂
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
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z-Score Hinweis
Remark
12 0,16 -0,020334 0,141 -0,03935 0,2 0,01986 0,22 0,03987
Auswerte- nummer
L-Cystin / L-Cystine [g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.5 L-Glutaminic Acid in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 8: Ergebnisse L-GlutaminsäureFig. 8: Results L-Glutaminic Acid
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1 2 3 4 5 6 7
0,00
0,50
1,00
1,50
2,00
2,50
Ergebnisse / Results
L-Glutamin-säure / L-Glutaminic Acid [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
Statistic DataNumber of results 7Number of outliers 0Mean 1,91Median 1,91Robust Mean (X) 1,91
0,124Target range:Target standard deviation 0,0915
0,0692
lower limit of target range 1,72upper limit of target range 2,09
1,4
0,0587
0,64
Results in the target range 7Percent in the target range 100
Robust standard deviation (Sx)
Target standard deviation Horwitz (for Information)
Quotient Sx/ Standard uncertainty ux
Quotient ux /
σ̂
σ̂
σ̂
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 9: Z-Scores L-GlutaminsäureFig. 9: Z-Scores L-Glutaminic Acid
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z-Score Hinweis
Remark
1 1,977 0,0711 0,8 1,02 1,88 -0,0259 -0,3 -0,43 1,75 -0,156 -1,7 -2,34 1,804 -0,102 -1,1 -1,55 1,94 0,0341 0,4 0,56 2,08 0,174 1,9 2,57 1,91 0,0041 0,0 0,1
Auswerte- nummer
L-Glutaminsäure / L-Glutaminic Acid
[g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
3 4 2 7 5 1 6-3
-2
-1
0
1
2
3
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.6 Glycine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 10: Ergebnisse GlycinFig. 10: Results Glycine
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Statistic DataNumber of results 7Number of outliers 1Mean 0,194Median 0,190Robust Mean (X) 0,191
0,0116Target range:Target standard deviation 0,00979
0,0125
lower limit of target range 0,171upper limit of target range 0,210
1,2
0,00548
0,56
Results in the target range 6Percent in the target range 86
Robust standard deviation (Sx)
Target standard deviation ASU (for Information)
Quotient Sx/ Standard uncertainty u
x
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,05
0,10
0,15
0,20
0,25
0,30
0,35
0,40
Ergebnisse / Results
Glycin / Glycine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 11: Z-Scores GlycinFig. 11: Z-Scores Glycine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 22 of 61
z-Score Hinweis
Remark
1 0,199 0,0082 0,8 0,72 0,19 -0,0008 -0,1 -0,13 0,177 -0,0138 -1,4 -1,14 0,183 -0,0078 -0,8 -0,65 0,19 -0,0008 -0,1 -0,16 0,23 0,0392 4,0 3,1 Ausreisser / Outlier
7 0,1885 -0,0023 -0,2 -0,2
Auswerte- nummer
Glycin / Glycine [g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
3 4 7 2 5 1 6-3
-2
-1
0
1
2
3
4
5
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.7 L-Histidine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 12: Ergebnisse L-HistidinFig. 12: Results L-Histidine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 23 of 61
Statistic DataNumber of results 7Number of outliers 0Mean 0,250Median 0,220Robust Mean (X) 0,246
0,0662Target range:Target standard deviation ' 0,0408
0,0122
lower limit of target range 0,165upper limit of target range 0,328
1,6
0,0313
0,77
Results in the target range 6Percent in the target range 86
Robust standard deviation (Sx)
Target standard deviation Horwitz (for Information)
Quotient Sx/ 'Standard uncertainty u
x
Quotient ux / '
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,05
0,10
0,15
0,20
0,25
0,30
0,35
0,40
Ergebnisse / Results
L-Histidin / L-Histidine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 13: Z'-Scores L-HistidinFig. 13: Z'-Scores L-Histidine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 24 of 61
z'-Score Hinweis
Remark
1 0,326 0,0797 2,0 6,62 0,2 -0,0463 -1,1 -3,83 0,205 -0,0413 -1,0 -3,44 0,212 -0,0343 -0,8 -2,85 0,22 -0,0263 -0,6 -2,26 0,36 0,1137 2,8 9,37 0,2255 -0,0208 -0,5 -1,7
Auswerte- nummer
L-Histidin / L-Histidine [g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
2 3 4 5 7 1 6-3
-2
-1
0
1
2
3
z'-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.8 L-Isoleucine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 14: Ergebnisse L-IsoleucinFig. 14: Results L-Isoleucine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 25 of 61
Statistic DataNumber of results 7Number of outliers 0Mean 0,540Median 0,540Robust Mean (X) 0,540
0,0276Target range:Target standard deviation 0,0237
0,0266
lower limit of target range 0,493upper limit of target range 0,588
1,2
0,0130
0,55
Results in the target range 7Percent in the target range 100
Robust standard deviation (Sx)
Target standard deviation ASU (for Information)
Quotient Sx/ Standard uncertainty u
x
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Isoleucin / L-Isoleucine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 15: Z-Scores L-IsoleucinFig. 15: Z-Scores L-Isoleucine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 26 of 61
z-Score Hinweis
Remark
1 0,574 0,0337 1,4 1,32 0,52 -0,0203 -0,9 -0,83 0,515 -0,0253 -1,1 -1,04 0,571 0,0307 1,3 1,25 0,52 -0,0203 -0,9 -0,86 0,54 -0,0003 0,0 0,07 0,542 0,0017 0,1 0,1
Auswerte- nummer
L-Isoleucin / L-Isoleucine
[g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
3 2 5 6 7 4 1-3
-2
-1
0
1
2
3
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.9 L-Leucine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 16: Ergebnisse L-LeucinFig. 16: Results L-Leucine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 27 of 61
Statistic DataNumber of results 7Number of outliers 0Mean 1,021Median 1,032Robust Mean (X) 1,021
0,0388Target range:Target standard deviation 0,0407
0,0543
lower limit of target range 0,940upper limit of target range 1,103
0,95
0,0184
0,45
Results in the target range 7Percent in the target range 100
Robust standard deviation (Sx)
Target standard deviation ASU (for Information)
Quotient Sx/ Standard uncertainty u
x
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,20
0,40
0,60
0,80
1,00
1,20
1,40
Ergebnisse / Results
L-Leucin / L-Leucine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 17: Z-Scores L-LeucinFig. 17: Z-Scores L-Leucine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 28 of 61
z-Score Hinweis
Remark
1 1,032 0,0109 0,3 0,22 0,99 -0,0311 -0,8 -0,63 0,965 -0,0561 -1,4 -1,04 1,011 -0,0101 -0,2 -0,25 1,05 0,0289 0,7 0,56 1,06 0,0389 1,0 0,77 1,04 0,0189 0,5 0,3
Auswerte- nummer
L-Leucin / L-Leucine [g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
3 2 4 1 7 5 6-3
-2
-1
0
1
2
3
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.10 L-Lysine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 18: Ergebnisse L-LysinFig. 18: Results L-Lysine
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Statistic DataNumber of results 7Number of outliers 0Mean 0,817Median 0,830Robust Mean (X) 0,817
0,0529Target range:Target standard deviation 0,0337
0,0718
lower limit of target range 0,749upper limit of target range 0,884
1,6
0,0250
0,74
Results in the target range 7Percent in the target range 100
Robust standard deviation (Sx)
Target standard deviation ASU (for Information)
Quotient Sx/ Standard uncertainty ux
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,20
0,40
0,60
0,80
1,00
1,20
1,40
Ergebnisse / Results
L-Lysin / L-Lysine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 19: Z-Scores L-LysinFig. 19: Z-Scores L-Lysine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 30 of 61
z-Score Hinweis
Remark
1 0,875 0,0581 1,7 0,82 0,86 0,0431 1,3 0,63 0,785 -0,0319 -0,9 -0,44 0,765 -0,0519 -1,5 -0,75 0,83 0,0131 0,4 0,26 0,76 -0,0569 -1,7 -0,87 0,843 0,0261 0,8 0,4
Auswerte- nummer
L-Lysin / L-Lysine [g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
6 4 3 5 7 2 1-3
-2
-1
0
1
2
3
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.11 L-Methionine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 20: Ergebnisse L-MethioninFig. 20: Results L-Methionine
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Statistic DataNumber of results 6Number of outliers 0Mean 0,214Median 0,218Robust Mean (X) 0,215
0,0123Target range:Target standard deviation 0,0132
0,0109
lower limit of target range 0,189upper limit of target range 0,242
0,9
0,00630
0,48
Results in the target range 6Percent in the target range 100
Robust standard deviation (Sx)
Target standard deviation Horwitz (for Information)
Quotient Sx/ Standard uncertainty ux
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,05
0,10
0,15
0,20
0,25
0,30
0,35
0,40
Ergebnisse / Results
L-Methionin / L-Methionine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 21: Z-Scores L-MethioninFig. 21: Z-Scores L-Methionine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 32 of 61
z-Score Hinweis
Remark
12 0,21 -0,0053 -0,4 -0,53 0,215 -0,0003 0,0 0,04 0,222 0,0067 0,5 0,65 0,22 0,0047 0,4 0,46 0,19 -0,0253 -1,9 -2,37 0,228 0,0127 1,0 1,2
Auswerte- nummer
L-Methionin / L-Methionine
[g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
6 2 3 5 4 7-3
-2
-1
0
1
2
3
4
5
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.12 L-Phenylalanine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 22: Ergebnisse L-PhenylalaninFig. 22: Results L-Phenylalanine
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Statistic DataNumber of results 7Number of outliers 0Mean 0,408Median 0,409Robust Mean (X) 0,408
0,0201Target range:Target standard deviation 0,0187lower limit of target range 0,370upper limit of target range 0,445
1,1
0,0095
0,51
Results in the target range 7Percent in the target range 100
Robust standard deviation (Sx)
Quotient Sx/ Standard uncertainty u
x
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Phenylalanin / L-Phenyl-alanine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 23: Z-Scores L-PhenylalaninFig. 23: Z-Scores L-Phenylalanine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 34 of 61
z-Score Hinweis
Remark
1 0,392 -0,0158 -0,82 0,42 0,0122 0,73 0,379 -0,0288 -1,54 0,405 -0,0028 -0,15 0,43 0,0222 1,26 0,42 0,0122 0,77 0,4085 0,0007 0,0
Auswerte- nummer
L-Phenylalanin / L-Phenylalanine
[g/100g]
Abweichung [g/100g]
Evaluation number
Deviation [g/100g]
σ̂
3 1 4 7 2 6 5-3
-2
-1
0
1
2
3
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.13 L-Proline in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 24: Ergebnisse L-ProlinFig. 24: Results L-Proline
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Statistic DataNumber of results 7Number of outliers 0Mean 0,740Median 0,750Robust Mean (X) 0,744
0,0329Target range:Target standard deviation 0,0575
0,0311
lower limit of target range 0,629upper limit of target range 0,859
0,57
0,0156
0,27
Results in the target range 7Percent in the target range 100
Robust standard deviation (Sx)
Target standard deviation Horwitz (for Information)
Quotient Sx/ Standard uncertainty u
x
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,20
0,40
0,60
0,80
1,00
1,20
1,40
Ergebnisse / Results
L-Prolin / L-Proline [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 25: Z-Scores L-ProlinFig. 25: Z-Scores L-Proline
Reprint, also in part, only with written permission from DLA-AhrensburgPage 36 of 61
z-Score Hinweis
Remark
1 0,733 -0,0113 -0,2 -0,42 0,77 0,0257 0,4 0,83 0,725 -0,0193 -0,3 -0,64 0,662 -0,0823 -1,4 -2,65 0,75 0,0057 0,1 0,26 0,78 0,0357 0,6 1,17 0,757 0,0127 0,2 0,4
Auswerte- nummer
L-Prolin / L-Proline
[g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
4 3 1 5 7 2 6-3
-2
-1
0
1
2
3
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.14 L-Serine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 26: Ergebnisse L-SerinFig. 26: Results L-Serine
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Statistic DataNumber of results 7Number of outliers 0Mean 0,538Median 0,525Robust Mean (X) 0,538
0,0762Target range:Target standard deviation ' 0,0431
0,0229
lower limit of target range 0,452upper limit of target range 0,624
1,8
0,0360
0,84
Results in the target range 5Percent in the target range 71
Robust standard deviation (Sx)
Target standard deviation ASU (for Information)
Quotient Sx/ 'Standard uncertainty u
x
Quotient ux / '
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Serin / L-Serine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 27: Z'-Scores L-SerinFig. 27: Z'-Scores L-Serine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 38 of 61
4 1 3 7 5 2 6-3
-2
-1
0
1
2
3
z'-Score
Auswertenummer / evaluation number
z'-Score Hinweis
Remark
1 0,512 -0,0263 -0,6 -1,12 0,58 0,0417 1,0 1,83 0,52 -0,0183 -0,4 -0,84 0,431 -0,107 -2,5 -4,75 0,55 0,0117 0,3 0,56 0,65 0,112 2,6 4,97 0,525 -0,0133 -0,3 -0,6
Auswerte- nummer
L-Serin / L-Serine [g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.15 L-Threonine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 28: Ergebnisse L-ThreoninFig. 28: Results L-Threonine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 39 of 61
Statistic DataNumber of results 7Number of outliers 1Mean 0,547Median 0,540Robust Mean (X) 0,535
0,0203Target range:Target standard deviation 0,0235
0,0296
lower limit of target range 0,488upper limit of target range 0,582
0,86
0,0096
0,41
Results in the target range 6Percent in the target range 86
Robust standard deviation (Sx)
Target standard deviation ASU (for Information)
Quotient Sx/ Standard uncertainty u
x
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Threonin / L-Threonine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 29: Z-Scores L-ThreoninFig. 29: Z-Scores L-Threonine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 40 of 61
z-Score Hinweis
Remark
1 0,532 -0,0034 -0,1 -0,12 0,54 0,0046 0,2 0,23 0,525 -0,0104 -0,4 -0,44 0,493 -0,0424 -1,8 -1,45 0,54 0,0046 0,2 0,26 0,66 0,125 5,3 4,2 Ausreisser / Outlier
7 0,54 0,0046 0,2 0,2
Auswerte- nummer
L-Threonin / L-Threonine
[g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
4 3 1 2 5 7 6-3
-2
-1
0
1
2
3>
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.16 L-Tryptophan in g/100g
Vergleichsuntersuchung / Proficiency Test
Due to the low number of results <7 no statistical evaluation was done.
Abb. 30: Ergebnisse L-TryptophanFig. 30: Results L-Tryptophan
Reprint, also in part, only with written permission from DLA-AhrensburgPage 41 of 61
Statistic DataNumber of results 4Number of outliers 0Mean 0,244Median 0,169Robust Mean (X) 0,191
0,0656Target range:Target standard deviation lower limit of target rangeupper limit of target range
Results in the target rangePercent in the target range
Robust standard deviation (Sx)
Quotient Sx/ Standard uncertainty u
x
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Tryptophan [g/100g]
Median
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Reprint, also in part, only with written permission from DLA-AhrensburgPage 42 of 61
z-Score Hinweis
Remark
1234 0,49 0,299 no method indicated
5 0,15 -0,0409 VDLUFA
6 0,176 -0,015 EU VO 152/2009
7 0,162 -0,0294 no method indicated
Auswerte- nummer
L-Tryptophan [g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.17 L-Tyrosine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 31: Ergebnisse L-TyrosinFig. 31: Results L-Tyrosine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 43 of 61
Statistic DataNumber of results 7Number of outliers 1Mean 0,318Median 0,320Robust Mean (X) 0,314
0,0560Target range:Target standard deviation ' 0,0334
0,0150
lower limit of target range 0,248upper limit of target range 0,381
1,7
0,0265
0,79
Results in the target range 6Percent in the target range 86
Robust standard deviation (Sx)
Target standard deviation Horwitz (for Information)
Quotient Sx/ 'Standard uncertainty u
x
Quotient ux / '
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Tyrosin / L-Tyrosine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 32: Z'-Scores L-TyrosinFig. 32: Z'-Scores L-Tyrosine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 44 of 61
z'-Score Hinweis
Remark
1 0,263 -0,0514 -1,5 -3,42 0,32 0,0056 0,2 0,43 0,255 -0,0594 -1,8 -4,04 0,293 -0,0214 -0,6 -1,45 0,34 0,0256 0,8 1,76 0,42 0,106 3,2 7,1 Ausreisser / Outlier
7 0,3315 0,0171 0,5 1,1
Auswerte- nummer
L-Tyrosin / L-Tyrosine
[g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
3 1 4 2 7 5 6-3
-2
-1
0
1
2
3
4
z'-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
4.18 L-Valine in g/100g
Vergleichsuntersuchung / Proficiency Test
Abb. 33: Ergebnisse L-ValinFig. 33: Results L-Valine
Reprint, also in part, only with written permission from DLA-AhrensburgPage 45 of 61
Statistic DataNumber of results 7Number of outliers 1Mean 0,611Median 0,601Robust Mean (X) 0,598
0,0335Target range:Target standard deviation 0,0258
0,0346
lower limit of target range 0,546upper limit of target range 0,650
1,3
0,0158
0,61
Results in the target range 6Percent in the target range 86
Robust standard deviation (Sx)
Target standard deviation ASU (for Information)
Quotient Sx/ Standard uncertainty ux
Quotient ux /
σ̂
σ̂
σ̂
1 2 3 4 5 6 7
0,00
0,10
0,20
0,30
0,40
0,50
0,60
0,70
0,80
Ergebnisse / Results
L-Valin / L-Valine [g/100g]
obere Grenze upper limit
rob. Mittelwert robust mean
untere Grenze lower limit
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
Ergebnisse der teilnehmenden Institute:Results of Participants:
Abb. 34: Z-Scores L-ValinFig. 34: Z-Scores L-Valine
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z-Score Hinweis
Remark
1 0,613 0,0152 0,6 0,42 0,57 -0,0278 -1,1 -0,83 0,585 -0,0128 -0,5 -0,44 0,608 0,0102 0,4 0,35 0,56 -0,0378 -1,5 -1,16 0,74 0,142 5,5 4,1 Ausreisser / Outlier
7 0,601 0,0032 0,1 0,1
Auswerte- nummer
L-Valin / L-Valine [g/100g]
Abweichung [g/100g]
z-Score (Info)
Evaluation number
Deviation [g/100g]
σ̂
5 2 3 7 4 1 6-3
-2
-1
0
1
2
3>
z-Score
Auswertenummer / evaluation number
May 2016 DLA 42/2015 - Total Amino Acid Composition
5. Documentation
5.1 Primary data
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Parameter Teilnehmer Einheit Proben-Nr. A Proben-Nr. B Ergebnis (Mittel) Ergebnis A Ergebnis B inkl. WFAnalyte Participant Unit Sample No. A Sample No. B Result (Mean) Result A Result B incl. RR
1 g/100g 20 35 0,432 0,435 0,428 no2 g/100g 4 37 0,43 0,43 0,42 no no3 g/100g 8 25 0,4425 0,441 0,4444 g/100g 1 17 0,413 0,419 0,4075 g/100g 16 38 0,43 0,43 0,42 no6 g/100g 7 18 0,48 0,48 0,48 no7 g/100g 45 13 0,4245 0,424 0,425
1 g/100g 20 35 0,266 0,28 0,251 no2 g/100g 4 37 0,33 0,33 0,32 no no3 g/100g 8 25 0,23 0,22 0,244 g/100g 1 17 0,256 0,264 0,2495 g/100g 16 38 0,29 0,29 0,28 no6 g/100g 7 18 0,31 0,31 0,31 no7 g/100g 45 13 0,291 0,286 0,296
1 g/100g 20 35 0,929 0,943 0,915 no2 g/100g 4 37 0,91 0,92 0,9 no no3 g/100g 8 25 0,88 0,87 0,894 g/100g 1 17 0,876 0,880 0,8725 g/100g 16 38 0,91 0,9 0,91 no6 g/100g 7 18 1,01 1,01 1,01 no7 g/100g 45 13 0,9315 0,931 0,932
Wiederfindungsrate [%]Recovery rate [%]
L-Alanin / L-Alanine
L-Arginin / L-Arginine
L-Asparaginsäure / L-Aspartic Acid
May 2016 DLA 42/2015 - Total Amino Acid Composition
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Parameter Teilnehmer Einheit Proben-Nr. A Proben-Nr. B Ergebnis (Mittel) Ergebnis A Ergebnis B inkl. WFAnalyte Participant Unit Sample No. A Sample No. B Result (Mean) Result A Result B incl. RR
1 g/100g 20 352 g/100g 4 37 0,16 0,15 0,16 no no3 g/100g 8 254 g/100g 1 17 0,141 0,144 0,1395 g/100g 16 38 0,2 0,2 0,2 no6 g/100g 7 18 0,22 0,22 0,22 no7 g/100g 45 13
1 g/100g 20 35 1,977 2,032 1,922 no2 g/100g 4 37 1,88 1,89 1,86 no no3 g/100g 8 25 1,75 1,77 1,734 g/100g 1 17 1,804 1,804 1,8045 g/100g 16 38 1,94 1,93 1,94 no6 g/100g 7 18 2,08 2,08 2,08 no7 g/100g 45 13 1,91 1,91 1,91
Glycin / Glycine
1 g/100g 20 35 0,199 0,203 0,195 no2 g/100g 4 37 0,19 0,19 0,19 no no3 g/100g 8 25 0,177 0,176 0,1784 g/100g 1 17 0,183 0,188 0,1795 g/100g 16 38 0,19 0,19 0,19 no6 g/100g 7 18 0,23 0,23 0,23 no7 g/100g 45 13 0,1885 0,187 0,19
Wiederfindungsrate [%]Recovery rate [%]
L-Cystin / L-Cystine
L-Glutaminsäure / L-Glutaminic Acid
May 2016 DLA 42/2015 - Total Amino Acid Composition
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Parameter Teilnehmer Einheit Proben-Nr. A Proben-Nr. B Ergebnis (Mittel) Ergebnis A Ergebnis B inkl. WFAnalyte Participant Unit Sample No. A Sample No. B Result (Mean) Result A Result B incl. RR
1 g/100g 20 35 0,326 0,334 0,317 no2 g/100g 4 37 0,2 0,2 0,2 no no3 g/100g 8 25 0,205 0,2 0,214 g/100g 1 17 0,212 0,214 0,2095 g/100g 16 38 0,22 0,21 0,22 no6 g/100g 7 18 0,36 0,36 0,36 no7 g/100g 45 13 0,2255 0,225 0,226
1 g/100g 20 35 0,574 0,583 0,566 no2 g/100g 4 37 0,52 0,53 0,51 no no3 g/100g 8 25 0,515 0,51 0,524 g/100g 1 17 0,571 0,569 0,5735 g/100g 16 38 0,52 0,52 0,51 no6 g/100g 7 18 0,54 0,54 0,54 no7 g/100g 45 13 0,542 0,542 0,542
1 g/100g 20 35 1,032 1,045 1,02 no2 g/100g 4 37 0,99 1 0,98 no no3 g/100g 8 25 0,965 0,96 0,974 g/100g 1 17 1,011 1,015 1,0075 g/100g 16 38 1,05 1,05 1,04 no6 g/100g 7 18 1,06 1,06 1,06 no7 g/100g 45 13 1,04 1,04 1,04
Wiederfindungsrate [%]Recovery rate [%]
L-Histidin / L-Histidine
L-Isoleucin / L-Isoleucine
L-Leucin / L-Leucine
May 2016 DLA 42/2015 - Total Amino Acid Composition
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Parameter Teilnehmer Einheit Proben-Nr. A Proben-Nr. B Ergebnis (Mittel) Ergebnis A Ergebnis B inkl. WFAnalyte Participant Unit Sample No. A Sample No. B Result (Mean) Result A Result B incl. RR
1 g/100g 20 35 0,875 0,871 0,88 no2 g/100g 4 37 0,86 0,85 0,86 no no3 g/100g 8 25 0,785 0,78 0,794 g/100g 1 17 0,765 0,739 0,7915 g/100g 16 38 0,83 0,83 0,82 no6 g/100g 7 18 0,76 0,76 0,76 no7 g/100g 45 13 0,843 0,842 0,844
1 g/100g 20 352 g/100g 4 37 0,21 0,22 0,2 no no3 g/100g 8 25 0,22 0,21 0,224 g/100g 1 17 0,222 0,225 0,2195 g/100g 16 38 0,22 0,21 0,22 no6 g/100g 7 18 0,19 0,19 0,19 no7 g/100g 45 13 0,228 0,243 0,213
1 g/100g 20 35 0,392 0,398 0,387 no2 g/100g 4 37 0,42 0,42 0,41 no no3 g/100g 8 25 0,379 0,377 0,3814 g/100g 1 17 0,405 0,406 0,4035 g/100g 16 38 0,43 0,43 0,43 no6 g/100g 7 18 0,42 0,42 0,42 no7 g/100g 45 13 0,4085 0,407 0,41
Wiederfindungsrate [%]Recovery rate [%]
L-Lysin / L-Lysine
L-Methionin / L-Methionine
L-Phenylalanin / L-Phenylalanine
May 2016 DLA 42/2015 - Total Amino Acid Composition
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Parameter Teilnehmer Einheit Proben-Nr. A Proben-Nr. B Ergebnis (Mittel) Ergebnis A Ergebnis B inkl. WFAnalyte Participant Unit Sample No. A Sample No. B Result (Mean) Result A Result B incl. RR
1 g/100g 20 35 0,733 0,733 0,733 no2 g/100g 4 37 0,77 0,78 0,75 no no3 g/100g 8 25 0,725 0,73 0,724 g/100g 1 17 0,662 0,617 0,7075 g/100g 16 38 0,75 0,74 0,75 no6 g/100g 7 18 0,78 0,78 0,78 no7 g/100g 45 13 0,757 0,754 0,76
1 g/100g 20 35 0,512 0,507 0,517 no2 g/100g 4 37 0,58 0,58 0,57 no no3 g/100g 8 25 0,52 0,51 0,534 g/100g 1 17 0,431 0,428 0,4335 g/100g 16 38 0,55 0,54 0,55 no6 g/100g 7 18 0,65 0,65 0,65 no7 g/100g 45 13 0,525 0,522 0,528
1 g/100g 20 35 0,532 0,532 0,531 no2 g/100g 4 37 0,54 0,54 0,53 no no3 g/100g 8 25 0,525 0,51 0,544 g/100g 1 17 0,493 0,498 0,4885 g/100g 16 38 0,54 0,54 0,54 no6 g/100g 7 18 0,66 0,66 0,66 no7 g/100g 45 13 0,54 0,537 0,543
Wiederfindungsrate [%]Recovery rate [%]
L-Prolin / L-Proline
L-Serin / L-Serine
L-Threonin / L-Threonine
May 2016 DLA 42/2015 - Total Amino Acid Composition
5.2 Homogeneity
5.2.1 Homogeneity test before the PT
Homogeneity test for magnesium by ICP-OES:
5.2.2 Repeatability standard deviation of duplicate tests of the participants
The repeatability standard deviations were calculated with the data documented in 5.1.It is 0,0209 g/100g = 2,56 % of X for L-lysine.And it is 0,0127 g/100g = 2,38 % of X for L-threonine.
5.2.3 Comparison of sample number / test results
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Independant samples mg/100g
1 31,02 31,53 32,04 30,25 30,6
Mean 31,1Repeatability Standard Deviation 0,704 2,3%
0
10
20
30
40
50
60
70
80
90
100
Homgenität / homogeneity
L-Alanin / L-Alanine
DLA-Nr. / No.
Ergebnis *100
May 2016 DLA 42/2015 - Total Amino Acid Composition
5.3 Analytical Methods
Details by the participants
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Parameter Teilnehmer Methodenbeschreibung Einwaage
1 200 - 500 mg Ninhydrin
2 0,5
3 1 g Ninhydrin
4
5 ca. 0,5 g HCl (6 mol/L)
6 REG (EG) 152/2009 0,25g -
7
WF mit gleicher Matrix
Homoge-nisierung
Aufschluss-methode
Derivatisie-rung
Referenzma-terial
Kalibrierver-fahren
Methode ist akkredi-
tiert
Sonstige Hinweise
Analyte ParticipantRecovery with same
matrixMethod description
Homoge-nization
Sample weight
Hydrolization DerivatisationReference material
CalibrationMethod
accreditedFurther remarks
L-Alanin / L-Alanine
Total amino acids af ter acidic hydroly-sis w ith amino acid analyzer (w ith post-column derivatization)
mortaracidic hydrolysis w ith 6 M HCl, 24 h at 110°C
milk proteinexternal standard, linear regression
yes
no Alanine (total)No- as re-ceived
Yes Yes individual standard Yes Yes
amino acid analyzer acidic hydrolysis infant food one point yes
Amino acids after hydrolysis (accor-ding to REG (EG) 152/2009)
feed (internal RM)internal std., 1-point-calibration
yes
grinding acidic hydrolysis
amino acid stan-dard for protein hydrolysates Sig-ma A2908-5ML
one-point calibrati-on w ith internal standard (norleu-cin)
no
yes
May 2016 DLA 42/2015 - Total Amino Acid Composition
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Parameter Teilnehmer Methodenbeschreibung Einwaage
1
2 Arginine (total) 0,5
34567
1
2 0,5
34567
1
2 0,5
345 Oxidation
67
WF mit gleicher Matrix
Homoge-nisierung
Aufschluss-methode
Derivatisie-rung
Referenzma-terial
Kalibrierver-fahren
Methode ist akkredi-
tiert
Sonstige Hinweise
Analyte ParticipantRecovery with same
matrixMethod description
Homoge-nization
Sample weight
Hydrolization DerivatisationReference material
CalibrationMethod
accreditedFurther remarks
L-Arginin / L-Arginine
noNo- as
receivedYes Yes individual standard Yes Yes
yes
L-Asparaginsäure
/ L-Aspartic Acid
no Aspartic acid (total)No- as
receivedYes Yes individual standard Yes Yes
yes
L-Cystin / L-Cystine
no Cystine (total)No- as
receivedYes Yes individual standard Yes Yes
May 2016 DLA 42/2015 - Total Amino Acid Composition
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Parameter Teilnehmer Methodenbeschreibung Einwaage
1
2 0,5
34567
1
2 Glycine (total) 0,5
34567
1
2 Histidine (total) 0,5
34567
WF mit gleicher Matrix
Homoge-nisierung
Aufschluss-methode
Derivatisie-rung
Referenzma-terial
Kalibrierver-fahren
Methode ist akkredi-
tiert
Sonstige Hinweise
Analyte ParticipantRecovery with same
matrixMethod description
Homoge-nization
Sample weight
Hydrolization DerivatisationReference material
CalibrationMethod
accreditedFurther remarks
L-Glutaminsäure /
L-Glutaminic Acid
no Glutaminc acid (total)No- as
receivedYes Yes individual standard Yes Yes
yes
Glycin / Glycine
noNo- as
receivedYes Yes individual standard Yes Yes
yes
L-Histidin / L-Histidine
noNo- as
receivedYes Yes individual standard Yes Yes
yes
May 2016 DLA 42/2015 - Total Amino Acid Composition
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Parameter Teilnehmer Methodenbeschreibung Einwaage
Analyte Participant Method description Hydrolization Derivatisation Calibration
1
2 no Isoleucine (Total) 0,5 Yes Yes individual standard Yes Yes
34567 yes
1
2 no Leucine (total) 0,5 Yes Yes individual standard Yes Yes
34567 yes
1
2 no Lysine (total) 0,5 Yes Yes individual standard Yes Yes
345 Oxidation
67 yes
WF mit gleicher Matrix
Homoge-nisierung
Aufschluss-methode
Derivatisie-rung
Referenzma-terial
Kalibrierver-fahren
Methode ist akkredi-
tiert
Sonstige Hinweise
Recovery with same
matrix
Homoge-nization
Sample weight
Reference material
Method accredited
Further remarks
L-Isoleucin / L-Isoleucine
No- as received
L-Leucin / L-Leucine
No- as received
L-Lysin / L-Lysine
No- as received
May 2016 DLA 42/2015 - Total Amino Acid Composition
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Parameter Teilnehmer Methodenbeschreibung Einwaage
Analyte Participant Method description Hydrolization Derivatisation Calibration
1
2 no Methionine (total) 0,5 Yes Yes individual standard Yes Yes
345 Oxidation
67 yes
1
2 no Phenylalanine (total) 0,5 Yes Yes individual standard Yes Yes
34567 yes
1
2 no Proline (total) 0,5 Yes Yes individual standard Yes Yes
34567 yes
WF mit gleicher Matrix
Homoge-nisierung
Aufschluss-methode
Derivatisie-rung
Referenzma-terial
Kalibrierver-fahren
Methode ist akkredi-
tiert
Sonstige Hinweise
Recovery with same
matrix
Homoge-nization
Sample weight
Reference material
Method accredited
Further remarks
L-Methionin / L-Methionine
No- as received
L-Phenylalanin /
L-Phenylalanine
No- as received
L-Prolin / L-Proline
No- as received
May 2016 DLA 42/2015 - Total Amino Acid Composition
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Parameter Teilnehmer Methodenbeschreibung Einwaage
Analyte Participant Method description Hydrolization Derivatisation Calibration
1
2 no Serine (total) 0,5 Yes Yes individual standard Yes Yes
34567 yes
1
2 no Threonine (total) 0,5 Yes Yes individual standard Yes Yes
345 Oxidation
67 yes
L-Tryptophan
12 n/a n/a n/a n/a n/a n/a n/a n/a n/a34
5 3-point-calibration ja
67 yes
WF mit gleicher Matrix
Homoge-nisierung
Aufschluss-methode
Derivatisie-rung
Referenzma-terial
Kalibrierver-fahren
Methode ist akkredi-
tiert
Sonstige Hinweise
Recovery with same
matrix
Homoge-nization
Sample weight
Reference material
Method accredited
Further remarks
L-Serin / L-Serine
No- as received
L-Threonin / L-Threonine
No- as received
HPLC (according to No. 4.11.2 VDLUFA methods III, 2. amendment
1988)
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Parameter Teilnehmer Methodenbeschreibung Einwaage
1
2 Tyrosine (total) 0,5
34567
1
2 Valine (total) 0,5
34567
WF mit gleicher Matrix
Homoge-nisierung
Aufschluss-methode
Derivatisie-rung
Referenzma-terial
Kalibrierver-fahren
Methode ist akkredi-
tiert
Sonstige Hinweise
Analyte ParticipantRecovery with same
matrixMethod description
Homoge-nization
Sample weight
Hydrolization DerivatisationReference material
CalibrationMethod
accreditedFurther remarks
L-Tyrosin / L-Tyrosine
noNo- as
receivedYes Yes individual standard Yes Yes
yes
L-Valin / L-Valine
noNo- as
receivedYes Yes individual standard Yes Yes
yes
May 2016 DLA 42/2015 - Total Amino Acid Composition
6. Index of participant laboratories in alphabetical order
List of participants of PTs DLA 42-2015 and DLA 43-2015:
[Die Adressdaten der Teilnehmer wurden für die allgemeine Veröffentlichung des Auswerte-Berichts nicht angege-ben.]
[The address data of the participants were deleted for publication of the evaluation report.]
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ENGLAND
ITALY
DENMARK
SPAIN
NETHERLANDS
Teilnehmer / Participant Ort / Town Land / Country
Germany
Germany
Germany
Germany
Germany
Germany
May 2016 DLA 42/2015 - Total Amino Acid Composition
7. Index of references
1. DIN EN ISO/IEC 17043:2010; Konformitätsbewertung – Allgemeine Anforderun-gen an Eignungsprüfungen / Conformity assessment – General requirements for proficiency testing
2. Verordnung / Regulation 882/2004/EU; Verordnung über amtliche Kontrollen /Regulation on official controls
3. DIN EN ISO/IEC 17025:2005; Allgemeine Anforderungen an die Kompetenz von Prüf- und Kalibrierlaboratorien / General requirements for the competence of testing and calibration laboratories
4. Richtlinie / Directive 1993/99/EU; über zusätzliche Maßnahmen im Bereich der amtlichen Lebensmittelüberwachung / on additional measures concerning the official control of foodstuffs
5. ASU §64 LFGB: Planung und statistische Auswertung von Ringversuchen zur Methodenvalidierung
6. DIN ISO 13528:2009; Statistische Verfahren für Eignungsprüfungen durch Ringversuche / Statistical methods for use in proficiency testing by in-terlaboratory comparisons
7. The International Harmonised Protocol for the Proficiency Testing of Anan-lytical Laboratories ; J.AOAC Int., 76(4), 926 – 940 (1993)
8. The International Harmonised Protocol for the Proficiency Testing of Anan-lytical Chemistry Laboratories ; Pure Appl Chem, 78, 145 – 196 (2006)
9. Evaluation of analytical methods used for regulation of food and drugs;W. Horwitz; Analytical Chemistry, 54, 67-76 (1982)
10.A Horwitz-like funktion describes precision in proficiency test; M. Thomp-son, P.J. Lowthian; Analyst, 120, 271-272 (1995)
11.Protocol for the design, conduct and interpretation of method performance studies; W. Horwitz; Pure & Applied Chemistry, 67, 331-343 (1995)
12.Recent trends in inter-laboratory precision at ppb and sub-ppb concentra-tions in relation to fitness for purpose criteria in proficiency testing; M. Thompson; Analyst, 125, 385-386 (2000)
13.ASU §64 LFGB: L49.07-1; Bestimmung der Aminosäuren in Aminosäurengemi-schen.
14.ASU §64 LFGB: L49.07-2; Bestimmung der Aminosäuren in diätetischen Lebens-mitteln auf Basis von Proteinhydrolysaten
15.ASU §64 LFGB: L49.07-3; Bestimmung des Tryptophangehaltes in diätetischen Lebensmitteln auf Basis von Proteinhydrolysaten
16.Verordnung 152/2009/EG zur Festlegung der Probenahmeverfahren und Analyse-methoden für die amtliche Untersuchung von Futtermitteln / Regulation 152/2009/EC laying down the methods of sampling and analysis for the offi-cial control of feed
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