Foodstuffs - Multimethod for the determination of aflatoxins, deoxynivalenol, fumonisins, ochratoxin A, T-2 toxin, HT-2 toxin and zearalenone by LC-MS/MS

This document describes a method using isotopically labelled standards for the quantitative determination of aflatoxins B1, B2, G1, G2 and M1 (AFB1, AFB2, AFG1, AFG2 and AFM1), ochratoxin A (OTA), deoxynivalenol (DON), zearalenone (ZEN), T-2 and HT-2 toxins (T-2 and HT-2) and fumonisins B1 and B2 (FB1 and FB2) in foods by liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS).
A specific immunoaffinity column (IAC) clean-up is needed for aflatoxins (AFs) and OTA in food intended for infants and young children (e.g. infant cereals, milk-based powders), in spices, in dried fruits and in nuts.
The method has been validated through an intercollaborative study on different commodity groups: cereals and cereal-based products including food for infant and young children, nuts, spices, dried fruits and milk powder. The measuring range of each mycotoxin in these naturally contaminated and/or spiked food samples were:
- AFB1: 0,085 7 µg/kg - 11,4 µg/kg;
- AFB2: 0,079 2 µg/kg - 12,5 µg/kg;
- AFG1: 0,062 8 µg/kg - 20,9 µg/kg;
- AFG2: 0,052 0 µg/kg - 15,0 µg/kg;
- AFM1: 0,034 2 µg/kg - 0,110 µg/kg;
- OTA: 0,448 µg/kg - 17,2 µg/kg;
- DON: 45,2 µg/kg - 743 µg/kg;
- ZEN: 9,57 µg/kg - 131 µg/kg;
- T-2: 10,3 µg/kg - 57,9 µg/kg;
- HT-2: 9,50 µg/kg - 81,8 µg/kg;
- FB1: 31,1 µg/kg - 4 260 µg/kg;
- FB2: 44,2 µg/kg - 1 300 µg/kg.
The measuring ranges of the method for each mycotoxin/matrix combination are given in Table 8.

Lebensmittel - Multiverfahren für die Bestimmung von Aflatoxinen, Deoxynivalenol, Fumonisinen, Ochratoxin A, T-2-Toxin, HT-2-Toxin und Zearalenon mittels LC-MS/MS

Dieses Dokument beschreibt ein Verfahren, das isotopenmarkierte Standards verwendet für die quantitative Bestimmung der Aflatoxine B1, B2, G1, G2 und M1 (AFB1, AFB2, AFG1, AFG2 und AFM1), Ochratoxin A (OTA), Deoxynivalenol (DON), Zearalenon (ZEN), T 2 und HT 2-Toxine (T 2 und HT 2) und Fumonisine B1 und B2 (FB1 und FB2) in Lebensmitteln durch Flüssigchromatographie (LC, en.: liquid chromatography), gekoppelt mit Tandem-Massenspektrometrie (MS/MS).
Für Aflatoxine (AF) und OTA in für Säuglinge und Kleinkinder bestimmter Nahrung (z. B. Zerealien für Kleinkinder, Pulver auf Milchbasis), in Gewürzen, in Trockenfrüchten und in Nüssen ist eine spezifische Immunaffinitätssäulen (IAC, en.: immunoaffinity column)-Reinigung erforderlich.
Das Verfahren wurde durch eine Ringversuchstudie zu verschiedenen Lebensmittelgruppen validiert: Getreide und Produkte auf Getreidebasis einschließlich Nahrung für Säuglinge und Kleinkinder, Nüsse, Gewürze, Trockenfrüchte und Milchpulver. Die Messbereiche der einzelnen Mykotoxine in diesen natürlich kontaminierten und/oder aufgestockten Lebensmittelproben waren:
—   AFB1:   0,085 7 µg/kg – 11,4 µg/kg;
—   AFB2:   0,079 2 µg/kg – 12,5 µg/kg;
—   AFG1:   0,062 8 µg/kg – 20,9 µg/kg;
—   AFG2:   0,052 0 µg/kg – 15,0 µg/kg;
—   AFM1:   0,034 2 µg/kg – 0,110 µg/kg;
—   OTA:   0,448 µg/kg – 17,2 µg/kg;
—   DON:   45,2 µg/kg – 743 µg/kg;
—   ZEN:   9,57 µg/kg – 131 µg/kg;
—   T 2:   10,3 µg/kg – 57,9 µg/kg;
—   HT 2:   9,50 µg/kg – 81,8 µg/kg;
—   FB1:   31,1 µg/kg – 4 260 µg/kg;
—   FB2:   44,2 µg/kg – 1 300 µg/kg.
Die Messbereiche der Verfahren für jede Mykotoxin-/Matrix-Kombination sind in Tabelle 8 angegeben.

Produits alimentaires - Multiméthode de détermination de la teneur en aflatoxines, déoxynivalénol, fumonisines, ochratoxine A, toxine T-2, toxine HT-2 et zéaralénone par CL-SM/SM

Le présent document décrit une méthode utilisant des étalons marqués aux isotopes pour la détermination quantitative des teneurs en aflatoxines B1, B2, G1, G2 et M1 (AFB1, AFB2, AFG1, AFG2 et AFM1), ochratoxine A (OTA), déoxynivalénol (DON), zéaralénone (ZEN), toxines T-2 et HT-2 (T-2 et HT 2) et fumonisines B1 et B2 (FB1 et FB2) dans les aliments par chromatographie liquide (CL) couplée à une spectrométrie de masse en tandem (SM/SM).
Une purification spécifique sur colonne d’immuno-affinité (CIA) est nécessaire pour les aflatoxines (AF) et l’OTA présentes dans les aliments pour nourrissons et enfants en bas âge (par exemple, céréales infantiles, lait en poudre), les épices, les fruits secs et les fruits à coques.
La méthode a été validée lors d’un essai interlaboratoires portant sur différents groupes de denrées : céréales et produits à base de céréales, y compris aliments pour nourrissons et enfants en bas âge, fruits à coques, épices, fruits secs et lait en poudre. Les gammes de mesure de chaque mycotoxine dans ces échantillons d’aliments naturellement contaminés et/ou dopés étaient les suivantes :
- AFB1 : 0,085 7 µg/kg - 11,4 µg/kg ;
- AFB2 : 0,079 2 µg/kg - 12,5 µg/kg ;
- AFG1 : 0,062 8 µg/kg - 20,9 µg/kg ;
- AFG2 : 0,052 0 µg/kg - 15,0 µg/kg ;
- AFM1 : 0,034 2 µg/kg - 0 110 µg/kg ;
- OTA : 0,448 µg/kg - 17,2 µg/kg ;
- DON : 45,2 µg/kg - 743 µg/kg ;
- ZEN : 9,57 µg/kg - 131 µg/kg ;
- T-2 : 10,3 µg/kg - 57,9 µg/kg ;
- HT-2 : 9,50 µg/kg - 81,8 µg/kg ;
- FB1 : 31,1 µg/kg - 4 260 µg/kg ;
- FB2 : 44,2 µg/kg - 1 300 µg/kg.
Les gammes de mesure de la méthode pour chaque combinaison mycotoxine/matrice sont indiquées dans le Tableau 8.

Živila - Hkratna metoda za določevanje aflatoksina, deoksinivalenola, fumonizinov, ohratoksina A, toksinov T-2 in HT-2 ter zearalenona z LC-MS/MS

Ta dokument opisuje metodo redčenja izotopov za kvantitativno določanje aflatoksinov B1, B2, G1, G2 in M1 (AFB1, AFB2, AFG1, AFG2 in AFM1), okratoksina A (OTA), deoksinivalenola (DON), zearalenona (ZEN), toksinov T-2 in HT-2 (T-2 in HT-2) ter fumonizinov B1 in B2 (FB1 in FB2) v živilih z visokozmogljivo tekočinsko kromatografijo (LC) v povezavi s tandemsko masno spektrometrijo (MS/MS).
Za aflatoksine (AF) in OTA v hrani za dojenčke (npr. kosmiči za dojenčke, praški na osnovi mleka), v začimbah, suhem sadju in oreščkih je potrebno posebno čiščenje imunoafinitetne kolone (IAC).
Metoda je bila potrjena z medstrokovno študijo o različnih skupinah živil: žita in proizvodi na osnovi žit, vključno s hrano za dojenčke in majhne otroke, oreščki, začimbami, suhim sadjem in mlekom v prahu. Območja koncentracij vsakega mikotoksina v teh naravno kontaminiranih vzorcih hrane in/ali vzorcih hrane z dodatki so bila:
–   aflatoksin B1:   od 0,0857 µg/kg do 11,4 µg/kg;
–   aflatoksin B2:   od 0,0792 µg/kg do 12,5 µg/kg;
–   aflatoksin G1:   od 0,0628 µg/kg do 20,9 µg/kg;
–   aflatoksin G2:   od 0,0520 µg/kg do 15,0 µg/kg;
–   aflatoksin M1:   od 0,0342 µg/kg do 0,110 µg/kg;
–   ohratoksin A:   od 0,448 µg/kg do 17,2 µg/kg;
–   deoksinivalenol:   od 45,2 µg/kg do 743 µg/kg;
–   zearalenon:   od 9,57 µg/kg do 131 µg/kg;
–   toksin T-2:      od 10,3 µg/kg do 57,9 µg/kg;
–   toksin HT-2:   od 9,50 µg/kg do 81,8 µg/kg;
–   fumonizin B1:   od 31,1 µg/kg do 4262 µg/kg;
–   fumonizin B2:   od 44,2 µg/kg do 1299 µg/kg.
Merilna območja metode za vsako kombinacijo mikotoksin/matrika so navedena v preglednici 7.

General Information

Status
Published
Publication Date
06-Sep-2022
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
07-Sep-2022
Due Date
21-Jul-2022
Completion Date
07-Sep-2022

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SLOVENSKI STANDARD
SIST EN 17641:2022
01-november-2022
Živila - Hkratna metoda za določevanje aflatoksina, deoksinivalenola, fumonizinov,
ohratoksina A, toksinov T-2 in HT-2 ter zearalenona z LC-MS/MS
Foodstuffs - Multimethod for the determination of aflatoxins, deoxynivalenol, fumonisins,
ochratoxin A, T-2 toxin, HT-2 toxin and zearalenone by LC-MS/MS
Lebensmittel - Multimethode für die Bestimmung von Aflatoxinen, Deoxynivalenol,
Fumonisinen, Ochratoxin A, T-2-Toxin, HT-2-Toxin und Zearalenon mittels LC-MS/MS
Produits alimentaires - Multiméthode de détermination de la teneur en aflatoxines,
déoxynivalénol, fumonisines, ochratoxine A, toxine T-2, toxine HT-2 et zéaralénone par
CL-SM/SM
Ta slovenski standard je istoveten z: EN 17641:2022
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
SIST EN 17641:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN 17641:2022

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SIST EN 17641:2022


EN 17641
EUROPEAN STANDARD

NORME EUROPÉENNE

September 2022
EUROPÄISCHE NORM
ICS 67.050
English Version

Foodstuffs - Multimethod for the determination of
aflatoxins, deoxynivalenol, fumonisins, ochratoxin A, T-2
toxin, HT-2 toxin and zearalenone by LC-MS/MS
Produits alimentaires - Multiméthode de Lebensmittel - Multimethode für die Bestimmung von
détermination de la teneur en aflatoxines, Aflatoxinen, Deoxynivalenol, Fumonisinen, Ochratoxin
déoxynivalénol, fumonisines, ochratoxine A, toxine T-2, A, T-2-Toxin, HT-2-Toxin und Zearalenon mittels LC-
toxine HT-2 et zéaralénone par CL-SM/SM MS/MS
This European Standard was approved by CEN on 24 July 2022.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17641:2022 E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------
SIST EN 17641:2022
EN 17641:2022 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principles . 6
5 Reagents . 6
6 Apparatus and equipment .12
7 Procedure.14
7.1 Preparation of the laboratory sample .14
7.2 Test portions weighing .
...

SLOVENSKI STANDARD
oSIST prEN 17641:2021
01-marec-2021
Živila - Večelementna metoda za določevanje aflatoksina, deoksinivalenola,
fumonizinov, ohratoksina A, toksinov T-2 in HT-2 ter zearalenona z LC-MS/MS
Foodstuffs - Multimethod for the determination of aflatoxins, deoxynivalenol, fumonisins,
ochratoxin A, T-2 toxin, HT-2 toxin and zearalenone by LC-MS/MS
Lebensmittel — Multimethode für die Bestimmung von Aflatoxinen, Deoxynivalenol,
Fumonisinen, Ochratoxin A, T 2 Toxin, HT 2 Toxin und Zearalenon mittels LC MS/MS
Produits alimentaires — Multiméthode de détermination de la teneur en aflatoxines,
déoxynivalénol, fumonisines, ochratoxine A, toxine T-2, toxine HT-2 et zéaralénone par
CL-SM/SM
Ta slovenski standard je istoveten z: prEN 17641
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
oSIST prEN 17641:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN 17641:2021

---------------------- Page: 2 ----------------------
oSIST prEN 17641:2021


DRAFT
EUROPEAN STANDARD
prEN 17641
NORME EUROPÉENNE

EUROPÄISCHE NORM

January 2021
ICS 67.050
English Version

Foodstuffs - Multimethod for the determination of
aflatoxins, deoxynivalenol, fumonisins, ochratoxin A, T-2
toxin, HT-2 toxin and zearalenone by LC-MS/MS
Produits alimentaires - Multiméthode de Lebensmittel - Multimethode für die Bestimmung von
détermination de la teneur en aflatoxines, Aflatoxinen, Deoxynivalenol, Fumonisinen, Ochratoxin
déoxynivalénol, fumonisines, ochratoxine A, toxine T-2, A, T 2 Toxin, HT 2 Toxin und Zearalenon mittels LC
toxine HT-2 et zéaralénone par CL-SM/SM MS/MS
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 275.

If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations
which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.

This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC
Management Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.


EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17641:2021 E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------
oSIST prEN 17641:2021
prEN 17641:2021 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principles . 6
5 Reagents . 6
6 Apparatus and equipment .
...

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