Evaluation Report proficiency test. DLA 19/ Aflatoxins and OTA in spice mixture. Waldemar-Bonsels-Weg Ahrensburg, Germany

Transcription

1 DLA Dienstleistung Lebensmittel Analytik GbR Evaluation Report proficiency test DLA 19/2015 Aflatoxins and OTA in spice mixture Dienstleistung Lebensmittel Analytik GbR Waldemar-Bonsels-Weg Ahrensburg, Germany Coordinator: Dr. G. Wichmann Page 1 of 24

2 Inhalt / Content 1. Introduction Realisation Test material Homogeneity Test Results Evaluation Assigned value Standard deviation Outliers Target standard deviation General model (Horwitz) Precision experiment Value by perception z-score z'-score Quotient Standard uncertainty Results Aflatoxin B1 in µg/kg Total aflatoxins in µg/kg Ochratoxin A in µg/kg Documentation Primary data Aflatoxin B Aflatoxin B2 in µg/kg Aflatoxin G1 in µg/kg Aflatoxin G2 in µg/kg Total aflatoxins in µg/kg Ochratoxin A Homogeneity Homogeneity testing before PT Repeatability standard deviation of participants Comparison of sample number/test result Analytical methods Aflatoxine Ochratoxin A Index of participant laboratories Index of literature...24 Page 2 of 24

3 1. Introduction The participation in proficiency testing schemes is an essential element of the quality-management-system of every laboratory testing food and feed, cosmetics and food contact materials. The implementation of proficiency tests enables the participating laboratories to prove their own analytical competence under realistic conditions. At the same time they receive valuable data regarding the validity of the particular testing method. The purpose of DLA is to offer proficiency tests for selected parameters in concentrations with practical relevance. Realisation and evaluation of the present proficiency test follows the technical requirements of DIN EN ISO/IEC (2010) and DIN ISO 13528: Realisation 2.1 Test material The test material with a natural content of aflatoxins and ochratoxin A is a spice mixture (Paprika, Curry) with additional cornmeal (3%) and fructose for testing the homogeneity. 3,5 kg of the material were homogenized and then packaged lightproof in portions to approximately 50 g. The portions were numbered chronologically. The material was checked for homogeneity Homogeneity The calculation of the repeatability standard deviation of the participants for total aflatoxins and ochratoxin A was used as an indicator of homogeneity. The result is similar to the repeatability standard deviation of the official method ASU 64 LFGB (corresponds to EN 14123) and ASU L (13, 14). The repeatability standard deviation of the participants is given in the documentation (see 5.2.1). To verify the homogeneity of the test material fructose was added before homogenisation. The homogeneity was examined by titrimetric determination (according Luff-Schorl), see The homogeneity is considered verified with a standard deviation of 1,9%, see in the documentation. In the documentation the portion numbers are graphically assigned to the results of ochratoxin A. There is no trend recognizable in the results which could suggest inhomogeneity. Page 3 of 24

4 2.2 Test Two portions of test material were sent to every participating laboratory in the 47 th week of The testing method was optional. The tests should be finished at 8 th January 2016 the latest. 2.3 Results The participants submitted their results in standard forms, which have been handed out with the samples (by ). The finally calculated concentrations of aflatoxin B1, total aflatoxins and ochratoxin A as average of duplicate determinations of both numbered samples was used for the statistical evaluation. Queried and documented were single results, recovery and the used testing method for aflatoxin B1, B2, G1 and G2 and ochratoxin A. From the 12 participants two participants have not delivered a result, all other participants submitted at least one result. Page 4 of 24

5 3. Evaluation 3.1 Assigned value Because the analysed material was no certified reference material the robust mean of the submitted results was used as assigned value X. The distribution of submitted results showed no hint for bimodal distribution or other reasons for a higher variability. 3.2 Standard deviation For comparison to the target standard deviation a robust standard deviation (Sx) was calculated (6). 3.3 Outliers Statistical outliers were determined by Mandel s-h-statistic (significance level: 5%) (5). Detected outliers were stated for information only, when z-score simultaneously was < -2 or > Target standard deviation The target standard deviation of the assigned value is determined according to the following methods General model (Horwitz) The relative target standard deviation in % of the assigned value is calculated according to the following equation. σ (%) = 2 (1-0,5logX) Out of this is calculated the target standard deviation in µg/kg σ = X * σ (%) / 100. For analytes with a content below 120 µg/kg after the evaluation of a lot of mycotoxin-proficiency testing schemes after 1997 Thompson suggested for the target standard deviation a steady value of 22 % (11), analogical σ = 0,22 C / mr with σ = Target standard deviation for contents < 120 µg/kg C = measured value, expressed as a dimensionless mass ratio mr = dimensionless mass ratio. The target standard deviation according to Horwitz/Thompson (11/17/18) was used. Page 5 of 24

6 3.4.2 Precision experiment Using the reproducibility standard deviation σ R and the repeatability standard deviation σ r of a precision experiment the between-laboratories standard deviation ( σ L ) can be calculated: L = R 2 r 2. And then, using the number of replicate measurements n, each participant is to perform, the standard deviation for proficiency assessment is calculated: = L 2 r 2 /n. The precision data of the method ASU 64 LFGB (corresponds to EN 14123) for a comparable aflatoxin content/paprika powder (13) result in a relative target standard deviation of 14,6 % for aflatoxin B1 and of the method ASU 64 LFGB for a high ochratoxin A-content/ sultanas result in a relative target deviation of 13,5% for ochratoxin A. This target standard deviation is given for information in the evaluation. Because the method for this LVU was optional the target standard deviation according to Horwitz/Thompson (11/17/18) was used Value by perception The target standard deviation for proficiency assessment can be set at a value that corresponds to the level of performance that the coordinator would wish laboratories to be able to achieve (6). For the present evaluation of results the target standard deviation according to Horwitz/ Thompson was applied for aflatoxin B1, total aflatoxins and ochratoxin A and evaluated with z -score (see 3.6). 3.5 z-score To assess the results of the participants the z-score is used. It indicates 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 considered as fulfilled if -2 z 2. Page 6 of 24

7 In accordance with the norm DIN ISO 13528:2009 (6) it is recommended that a result that gives rise to a z-score above 3,0 or below 3,0, shall be considered to give an action signal. Likewise, a z-score above 2,0 or below 2,0 shall be considered to give a warning signal. A single action signal, or warning signals in two successive PT-rounds, shall be taken as evidence that an anomaly has occurred which requires investigation. For example a fault isolation or a root cause analysis through the examination of transmission error or an error in the calculation, in the trueness and precision must be performed and if necessary appropriate corrective measures should be applied. 3.6 z'-score The z'-score can be used for the valuation of the results of the participants, 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 the square root of quadrat sum of the target standard deviation ( σ ) and the standard uncertainty (Ux) (6). Participants z'-scores are derived as: In the following we define the denominator deviation σ '. as the target standard The requirements for the analytical performance are generally considered as fulfilled if -2 z' 2. aflatoxin B1, total aflatoxins and ochratoxin A were evaluated with z score (see 3.7 and 3.8). Page 7 of 24

8 3.7 Quotient S x / Following the Horrat-value the results of a proficiency-test (PT) can be considered convincing, if the quotient of robust standard deviation and target standard deviation does not exceed the value of 2. A value > 2 means an insufficient precision, i.e. the analytical method is too variable, or the variation between the test participants is higher than estimated. Thus the comparability of the results is not given (11). In the present proficiency test the quotient S x / σ for Aflatoxin B1, total Aflatoxins and ochratoxin A were clearly above 2,0. Therefore evaluation of these parameters was done according to 3.6 by z'-scores. The resulting quotients S x / σ ' were in the range of 1,6 to 2,0 then. 3.8 Standard uncertainty The assigned value X has a standard uncertainty u X that depends on the analytical method, differences between the analytical methods used, the test material, the number of participant laboratories and perhaps on other factors. The standard uncertainty ( u X ) for this PT is calculated as follows (6). u X =1,25 S x / p If u X 0,3 the standard uncertainty of the assigned value needs not to be included in the interpretation of the results of the PT (6). The quotient u X / is reported in the characteristics of the test. In the present proficiency tests the quotients U x / σ were between 1,0 and 1,3 for Aflatoxin B1, total aflatoxins and ochratoxin A. At the same time the quotients S x / σ were > 2,0 for these parameters. Therefore the target range for these parameters was extended according 3.6 z'-score considering the standard uncertainty. Page 8 of 24

9 4. Results All following tables are anonymized. With the delivering of the evaluation-report the participants are informed about their individual evaluation-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 (S x ) Target range: Target standard deviation σ or σ ' Target standard deviation for information lower limit of target range (X - 2 σ ) or (X - 2 σ ') * upper limit of target range (X + 2 σ ) or (X + 2 σ ') * Quotient S x / σ ' Standard uncertainty u X 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 participating laboratories are listed: Auswertenummer Parameter Evaluation [Einheit / Unit] number Abweichung z-score z-score Hinweis σ (Info) Deviation Remark Page 9 of 24

10 4.1 Aflatoxin B 1 in µg/kg Vergleichsuntersuchung / Proficiency Test Statistic Data Number of results 8* Number of outliers 0 Mean 1,76 Median 1,92 Robust Mean (X) 1,76 Robust standard deviation (S x ) 0,914 Target range: Target standard deviation (Horwitz/Thompson) σ Target standard deviation ASU (for Information) 0,559 0,257 lower limit of target range 0,640 upper limit of target range 2,88 Quotient S x / σ ' 1,6 Standard uncertainty u x 0,404 Quotient u x / σ ' 0,72 Results in the target range 7 Percent in the target range 88 * without result of participant 3 3,5 Ergebnisse / Results 3,0 2,5 2,0 1,5 1,0 0,5 0, Auswertenummer / evaluation number Aflatoxin B1 (µg/kg) obere Grenze upper limit rob. Mittelwert robust mean untere Grenze lower limit Abb. 1: Ergebnisse Aflatoxin B1 Fig. 1: Results aflatoxin B1 Page 10 of 24

11 Ergebnisse der teilnehmenden Institute: Results of Participants: Auswertenumme r Evaluation Aflatoxin B1 (µg/kg) Abweichung [µg/kg] Deviation z -Score σ z-score (Info) number [µg/kg] 1 1,70-0,06-0,1-0,2 2 0,70-1,06-1,9-4,1 3 0 (-1,76) 4 2,18 0,42 0,7 1,6 5 2,76 1,00 1,8 3,9 6 1,70-0,06-0,1-0,2 7 0,47-1,29-2,3-5,0 8 2,14 0,38 0,7 1, ,42 0,66 1,2 2,6 Hinweis Remark 3 z -Score Auswertenummer / evaluation number Abb. 2: Fig. 2: Z-Scores Aflatoxin B1 Z-Scores aflatoxin B1 Page 11 of 24

12 4.2 Total aflatoxins in µg/kg Statistic Data Number of results 8* Number of outliers 1 Mean 2,49 Median 1,98 Robust Mean (X) 2,01 Robust standard deviation (S x ) 1,21 Target range: Target standard deviation 0,695 (Horwitz/Thompson) σ Target standard deviation ASU 0,294 (for Information) lower limit of target range 0,617 upper limit of target range 3,40 Quotient S x / σ ' 1,7 Standard uncertainty u x 0,537 Quotient u x / σ ' 0,77 Results in the target range 6 Percent in the target range 75 * without result of participant 3 8,0 Ergebnisse / Results 7,0 6,0 5,0 4,0 3,0 2,0 1,0 0, Auswertenummer / evaluation number Gesamt- Aflatoxin (µg/kg) obere Grenze upper limit rob. Mittelwert robust mean untere Grenze lower limit Abb. 3: Ergebnisse Gesamt-Aflatoxin Fig. 3: Results total aflatoxins Page 12 of 24

13 Ergebnisse der teilnehmenden Institute: Results of Participants: Auswertenummer Evaluation Gesamt-Aflatoxin (µg/kg) Abweichung [µg/kg] Deviation z -Score σ z-score (Info) Hinweis Remark number [µg/kg] 1 1,79-0,22-0,3-0,7 2 0,80-1,21-1,7-4,1 3 0 (-2,01) 4 2,18 0,17 0,2 0,6 5 2,88 0,87 1,3 3,0 6 1,70-0,31-0,4-1,0 7 0,53-1,48-2,1-5,0 8 2,36 0,35 0,5 1,2 9 7,70 5,69 8,2 19,4 Ausreisser / Outlier z -Score Auswertenummer / evaluation number Abb. 4: Fig. 4: Z-Scores Gesamt-Aflatoxin Z-Scores total aflatoxins Page 13 of 24

14 4.3 Ochratoxin A in µg/kg Statistic Data Number of results 10 Number of outliers 1 Mean 52,7 Median 53,0 Robust Mean (X) 45,6 Robust standard deviation (S x ) 31,9 Target range: Target standard deviation 16,1 (Horwitz/Thompson) σ Target standard deviation ASU 6,13 (for Information) lower limit of target range 13,4 upper limit of target range 77,8 Quotient S x / 2,0 σ ' Standard uncertainty u x 12,6 Quotient u x / σ ' 0,78 Results in the target range 7 Percent in the target range Ergebnisse / Results Auswertenummer / evaluation number Ochratoxin A (µg/kg) obere Grenze upper limit rob. Mittelwert robust mean untere Grenze lower limit Abb. 5: Ergebnisse Ochratoxin A Fig. 5: Results ochratoxin A Page 14 of 24

15 Ergebnisse der teilnehmenden Institute: Results of Participants: Auswertenummer Evaluation Ochratoxin A (µg/kg) Abweichung [µg/kg] Deviation z -Score σ z-score (Info) Hinweis Remark number [µg/kg] ,42 0,3 0,7 2 54,1 8,52 0,5 1, , ,4 19,4 Ausreisser / Outlier 4 22,8-22,8-1,4-3,7 5 4,12-41,5-2,6-6,8 6 61,90 16,3 1,0 2,7 7 51,85 6,27 0,4 1,0 8 56,6 11,0 0,7 1, ,6-2,7-7, ,4 0,8 2,2 8 z -Score Auswertenummer / evaluation number Abb. 6: Fig. 6: Z -Scores Ochratoxin A Z -Scores Ochratoxin A Page 15 of 24

16 5. Documentation 5.1 Primary data Aflatoxin B 1 inkl. Ergebnis Ergebnis DLA- DLA- Wiederfindungfindung/ Wieder- Teilnehmer/ Ergebnis/ Probe A/ Probe B/ Nr A/ Nr B/ Participant result Result Result no. A no. B included recovery sample A sample B recovery µg/kg µg/kg µg/kg ja / nein in % 1 1, ,6 1, , ,8 0,6 no no - 4 2, ,16 2,19 69,9 5 2, ,18 2,33 no / 6 1, ,84 1, , ,48 0,46 89,9 8 2, , , Aflatoxin B 2 in µg/kg inkl. Ergebnis Ergebnis Wiederfindungfindung/ Wieder- Teilnehmer/ DLA-Nr A/ DLA-Nr B/ Probe A/ Probe B/ participant no. A no. B Result Result included recovery sample A sample B recovery µg/kg µg/kg ja / nein in % ,1 0, ,1 <0.1 no no < 0.4 < , ,13 0,12 no / ,06 0,05 79, ,24 0,2 99, Page 16 of 24

17 5.1.3 Aflatoxin G 1 in µg/kg inkl. Teilneh Ergebnis Ergebnis Wiederfindungfindung/ Wieder- mer/ DLA-Nr A/ DLA-Nr B/ Probe A/ Probe B/ partici no. A no. B Result Result included recovery pant sample A sample B recovery µg/kg µg/kg ja / nein in % <0.1 < <0.1 <0.1 no no N.N N.N N.N N.N no / < 0,1 < 0,1 93, Aflatoxin G 2 in µg/kg inkl. Ergebnis Ergebnis Wiederfindungfindung/ Wieder- Teilnehmer/ DLA-Nr A/ DLA-Nr B/ Probe A/ Probe B/ participant no. A no. B Result Result included recovery sample A sample B recovery µg/kg µg/kg ja / nein in % <0.1 < <0.1 <0.1 no no N.N N.N N.N N.N no / < 0,1 < 0,1 54, Page 17 of 24

18 5.1.5 Total aflatoxins in µg/kg inkl. Ergebnis Ergebnis DLA- DLA- Wiederfindung/ Probe A/ Probe B/ Nr A/ Nr B/ Result Result no. A no. B included sample A sample B recovery µg/kg µg/kg µg/kg ja / nein in % 1 1, ,7 1, , ,9 0,6 no no - 4 2, ,16 2,19 5 2, ,31 2,45 no / 6 1, ,84 1,56 7 0, ,54 0, , ,51 2,2 9 7, Teilnehmer/ Ergebnis/ Participant result Wiederfindung/ recovery Ochratoxin A inkl. Ergebnis Ergebnis DLA- DLA- Wiederfindungfindung/ Wieder- Teilnehmer/ Ergebnis/ Probe A/ Probe B/ Nr A/ Nr B/ Participant result Result Result no. A no. B included recovery sample A sample B recovery µg/kg µg/kg µg/kg ja / nein in % , ,5 52,7 no , ,5 243,15 no , n.a. 5 4, ,21 4,04 no / 6 61, ,4 62,4 no , ,7 106,7 8 56, ,7 56,4 95, Page 18 of 24

19 5.2 Homogeneity Homogeneity testing before PT To verify the homogeneity of the test material the content of reducing sugar was determined in a 5-fold determination by Luff-Schorl (titration). Sample no. Sugar (red.) a 8,89 g/100g b 9,05 g/100g c 9,07 g/100g d 9,27 g/100g e 9,30 g/100g Mean 9,1 Standard deviation 0,17 1,9 % Repeatability standard deviation of participants The repeatability standard deviations were calculated with the data documented in chapter 5.1. It is 0,33 µg/kg = 18,5 % of X (Aflatoxin B1) and 1,4 µg/kg = 3,1 % of X (ochratoxin A/ without outlier). In the ASU L the relative repeatability standard deviation of 10 % (Aflatoxin B 1 ) for a aflatoxin content x = 1,4 µg/kg was determined for paprika powder (13) and in the ASU L the relative repeatability standard deviations of 5,6 % (ochratoxin A) for a ochratoxin A content x = 11,4 µg/kg was determined for sultanas (14). Page 19 of 24

20 5.2.3 Comparison of sample number/test result The comparison of the increasing sample-numbers and measured ochratoxin A-results shows a sufficient homogeneity. Homognität/ homogeneity DLA-Nr./DLA-No. Ochratoxin A (µg/kg) Page 20 of 24

21 5.3 Analytical methods To the participants: Aflatoxine Teilnehmer/ paticipant 1 2 no HPLC 3 no HPLC 4 Wiederfindung mit gleicher Matrix/ recovery with the same matrix /no Methode/ method Extraction by SLMB 1374: 50.0 g sample + 5 g NaCl, extraction with 300 ml MeOH/aqua (80+20 v/v). Mix 3 min (Polytron ). Filter extract.5 ml sample extract in 100 ml measuring cylinder and dilute with 60 ml TWEEN-20 10% solution. Than IAC cleaning of the total 25 ml ( ca. 1-2 drops/s). Elution of the toxins with methanol in a 5.0 ml volumetric flask. Complete the total methanol eluate with distilled aqua to 5.0 ml and filter the solution (0.2 μm) into HPLC vial. Quantitative determination by RP- HPLC/ fluorescence detection (Ex 362 nm, Em 440 nm) after electrochemical post-column derivatisation (COBRA-Cell). Extraction with acetone/h 2 O (85/15). Extract cleaning with IAC. Quantification of the aflatoxins with a fluorescence detector in the eluate of the RP-HPLC after photochemical derivatisation. 5 no IAC, HPLC, Fluorescence detector, Coring Cell Akkreditiert/ accredided /no no no Sonstige Hinweise/ remarks Mandatory final result incl. recovery; LOQ (B2)= 0,4µg/kg, LOD (G1, G2)= 0,1µg/kg, 6 Determination of mycotoxins in food with LC-MS/MS. ASU L ( ), mod. Matrix calibration with standard addition 7 PV 2.019/ LFGB, HPLC with FLD and UVE 10 *IAC = Immuno Affinity Column Page 21 of 24

22 5.3.2 Ochratoxin A Teilnehmer/ Participant 1 2 no HPLC 3 no HPLC Wiederfindung mit gleicher Matrix/ recovery with the same matrix /no Methode/ method Extraction according to SLMB 1387: 25.0 g sample add with 200 ml extraction solution (MeOH/3%Sodiumhydrogencarbonate solution v/v). Extract mix 3 min. with Polytron mixer and filter with glass fiber filter (alternatively centrifugation). Wash 10 ml filtrate with CH2Cl2. Than transfer 5 ml aqueous phase in a 100 ml measuring cylinder and dilute with PBS buffer sulition to 100 ml. Than IAC (flow ca. 1 drops/s). Than elution with methanol, dry with Rotavapor. Dissolve residue in ml mobile phase. The quantitative determination by RP-HPLC/ fluorescence detection (Ex 330 nm, Em 470 nm). ELISA Ridascreen Ochratoxin A 30/15 (R1311) with OCHRAPREP IAC (RBRP14 / P14B) Akkreditiert/ accedided /no no no IAC, HPLC, fluorescence detector no Determination of mycotoxins in food with LC-MS/MS. ASU L ( ), mod. 7 PV 2.019/ LFGB, HPLC with FLD ELISA from Fa. R-biopharm no Sonstige Hinweise/ remarks *IAC = Immuno Affinity Column Page 22 of 24

23 6. Index of participant laboratories Teilnehmer/ Participant Ort/ Town Land/ Country Switzerland Switzerland Germany Germany Germany Denmark Switzerland Germany Germany Austria Germany Germany [Die Adressdaten der Teilnehmer wurden für die allgemeine Veröffentlichung des Auswerte-Berichts nicht angegeben.] [The address data of the participants were deleted for publication of the evaluation report.] Page 23 of 24

24 7. Index of literature 1. DIN EN ISO/IEC 17043:2010; Konformitätsbewertung Allgemeine Anforderungen 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 interlaboratory comparisons 7. The International Harmonised Protocol for the Proficiency Testing of Ananlytical Laboratories ; J.AOAC Int., 76(4), (1993) 8. The International Harmonised Protocol for the Proficiency Testing of Ananlytical Chemistry Laboratories ; Pure Appl Chem, 78, (2006) 9. Evaluation of analytical methods used for regulation of food and drugs;w. Horwitz; Analytical Chemistry, 54, (1982) 10.A Horwitz-like funktion describes precision in proficiency test; M. Thompson, P.J. Lowthian; Analyst, 120, (1995) 11.Protocol for the design, conduct and interpretation of method performance studies; W. Horwitz; Pure & Applied Chemistry, 67, (1995) 12.Recent trends in inter-laboratory precision at ppb and sub-ppb concentrations in relation to fitness for purpose criteria in proficiency testing; M. Thompson; Analyst, 125, (2000) 13.ASU 64 LFGB (Jan. 2012): Bestimmung von Aflatoxin B 1 und der Summe von Aflatoxin B 1, B 2, G 1 und G 2 in Erdnüssen, Pistazien, Feigen und Paprikapulver (: EN 14123:2007, Foodstuffs. Determination of aflatoxin B1 and the sum of aflatoxin B1, B2, G1 and G2 in hazelnuts, peanuts, pistachios, figs, and paprika powder. High performance liquid chromatographic method with post-column derivatisation and immunoaffinity column cleanup 14.ASU 64 LFGB : Bestimmung von Ochratoxin A in Korinthen, Rosinen, Sultaninen, gemischtem Trockenobst und getrockneten Feigen (Jan. 2011) 15.ASU 64 LFGB : Bestimmung von Ochratoxin A in Gerste (Jan. 2010) 16.Report on the 2007 Proficiency Test for the Determination of Ochratoxin A in Capsicum ssp (Paprika Powder), J.Stroka et al., JRC Scientific and Technical Reports, European Commission EUR EN, European Communities, EG-VO zur Festlegung der Probenahmeverfahren und Analysemethoden für die amtliche Kontrolle des Mykotoxingehalts von Lebensmitteln (COMMISSION REGULATION (EC) No 401/2006 laying down the methods of sampling and analysis for the official control of the levels of mycotoxins in foodstuffs) 18.EU-VO 519/2014 zur Änderung der Verordnung (EG) Nr. 401/2006 hinsichtlich der Probenahmeverfahren für große Partien, Gewürze und Nahrungsergänzungsmittel, der Leistungskriterien für die Bestimmung von T-2-Toxin, HT-2-Toxin und Citrinin sowie der Screening-Methoden für die Analyse (v. 16. Mai 2014) (COMMISSION REGULATION (EU) No 519/2014 amending Regulation (EC) No 401/2006 as regards methods of sampling of large lots, spices and food supplements, performance criteria for T-2, HT-2 toxin and citrinin and screening methods of analysis) Page 24 of 24