Animal feeding stuff: Methods of sampling and analysis - Determination of intact glucosinolates in feed materials and compound feed by LC-MS/MS

This document describes a method for the determination of individual intact glucosinolates in rapeseed
by high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry
(MS/MS). Progoitrin, gluconapin, glucobrassicanapin, glucobrassicin, nasturtiin, neoglucobrassicin and
4-methoxyglucobrassicin are quantitatively determined. Other glucosinolates such as
4-hydroxyglucobrassicin, glucnapoliferin, glucoalysin, can only be qualitatively detected when
analytical standards become commercially available.
The method has been in-house validated for rapeseeds in the range 0.05-60 mmol/kg for individual
glucosinolates.

Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von intakten Glucosinolaten in Futtermittel-Ausgangserzeugnissen und Mischfuttermitteln mittels LC-MS/MS

Dieses Dokument legt ein Verfahren zur Bestimmung der einzelnen Glucosinolate in Ölsaaten, Ölsaaten- erzeugnissen und Alleinfuttermitteln durch Hochleistungsflüssigkeitschromatographie(HPLC) in Verbindung mit Tandem-Massenspektrometrie(MS/MS) fest.
Das in diesem Dokument beschriebene Verfahren wurde im Rahmen eines Ringversuchs mit den folgenden Matrices erfolgreich validiert: Rapssamen, Leindottersamen, Brassica-oleracea-Samen, gemischte Ölsaaten, Rapssamenflocken, Mischfuttermittel für Rinder, Schweine und Geflügel.
Das Verfahren ist anwendbar für die quantitative Bestimmung von Epiprogroitrin, Glucoalyssin, Glu
coarabin, Glucobrassicanapin, Glucobrassicin, Glucocamelinin, Glucoerucin, Glucoiberin, Gluconapin, Gluconapoleiferin, Gluconasturtiin, Glucoraphanin, Glucoraphenin, Glucotropaeolin, Homoglucocamelinin, 4-Hydroxyglucobrassicin, 4-Methoxyglucobrassicin, Neoglucobrassicin, Progoitrin, Sinalbin und Sinigrin.
Die im Ringversuch geprüften Konzentrationsbereiche für jedes einzelne Glucosinolat und für den Gesamt- gehalt an Glucosinolaten sind in Tabelle1 zusammengefasst.

Alimentation animale : Méthodes d’échantillonnage et d’analyse - Dosage des glucosinolates intacts dans les matières premières pour l’alimentation animale et les aliments composés par CLHP MS/MS

Le présent document spécifie une méthode pour le dosage de différents glucosinolates intacts dans les graines oléagineuses, les produits oléagineux et les aliments composés par chromatographie liquide haute performance (CLHP) couplée à la spectrométrie de masse en tandem (SM/SM).
La méthode décrite dans le présent document a été validée par un essai interlaboratoires avec les matrices suivantes : graines de colza, graines de cameline, graines de Brassica oleracea, mélange de graines oléagineuses, flocons de graines de colza, aliments composés pour bovins, porcins et volaille.
La méthode est applicable pour la détermination quantitative de l’épiprogroitrine, la glucoalyssine, la glucoarabine, la glucobrassicanapine, la glucobrassicine, la glucocamélinine, la glucoérucine, la glucoibérine, la gluconapine, la gluconapoléiférine, la gluconasturtiine, la glucoraphanine, la glucoraphénine, la glucotropaéoline, l’homoglucocamélinine, la 4-hydroxyglucobrassicine, la 4-méthoxyglucobrassicine, la néoglucobrassicine, la progoitrine, la sinalbine et la sinigrine.
Les plages de concentration soumises à essai dans le cadre de l’essai interlaboratoires pour déterminer la teneur des différents glucosinolates et des glucosinolates totaux sont présentées dans le Tableau 1.

Krma: metode vzorčenja in analize - Ugotavljanje nepoškodovanih glukozinolatov v sestavinah krme in krmni mešanici z LC-MS/MS

Ta dokument opisuje metodo za določevanje posameznih nepoškodovanih glukozinatov v ogrščici s
tekočinsko kromatografijo visoke ločljivosti (HPLC) v kombinaciji s tandemsko masno spektrometrijo (MS/MS). Progoitrin, glukonapin, glukobrasikanapin, glukobrasicin, nasturtiin, neoglukobrasicin in 4-metoksiglukobrasicin se določajo kvantitativno. Druge glukozinate, kot so 4-hidroksiglukobrasicin, gluknapoliferin in glukoalisin, bo mogoče kvantitativno določiti šele, ko bodo analitični standardi komercialno dostopni.
Ta metoda je bila interno potrjena za semena ogrščice v območju 0,05–60 mmol/kg za posamezne glukozinate.

General Information

Status
Published
Public Enquiry End Date
30-Jul-2022
Publication Date
20-Aug-2023
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
20-Jun-2023
Due Date
25-Aug-2023
Completion Date
21-Aug-2023

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Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN 17853:2023
01-september-2023
Krma: metode vzorčenja in analize - Ugotavljanje nepoškodovanih glukozinolatov
v sestavinah krme in krmni mešanici z LC-MS/MS
Animal feeding stuff: Methods of sampling and analysis - Determination of intact
glucosinolates in feed materials and compound feed by LC-MS/MS
Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von intakten
Glucosinolaten in Futtermittel-Ausgangserzeugnissen und Mischfuttermitteln mittels LC-
MS/MS
Alimentation animale : Méthodes d’échantillonnage et d’analyse - Dosage des
glucosinolates intacts dans les matières premières pour l’alimentation animale et les
aliments composés par CLHP MS/MS
Ta slovenski standard je istoveten z: EN 17853:2023
ICS:
65.120 Krmila Animal feeding stuffs
SIST EN 17853:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN 17853:2023

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SIST EN 17853:2023


EN 17853
EUROPEAN STANDARD

NORME EUROPÉENNE

April 2023
EUROPÄISCHE NORM
ICS 65.120
English Version

Animal feeding stuff: Methods of sampling and analysis -
Determination of intact glucosinolates in feed materials
and compound feed by LC-MS/MS
Alimentation animale : Méthodes d'échantillonnage et Futtermittel - Probenahme- und
d'analyse - Dosage des glucosinolates intacts dans les Untersuchungsverfahren - Bestimmung von intakten
matières premières pour l'alimentation animale et les Glucosinolaten in Futtermittel-Ausgangserzeugnissen
aliments composés par CLHP MS/MS und Mischfuttermitteln mittels LC-MS/MS
This European Standard was approved by CEN on 3 March 2023.

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
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17853:2023 E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------
SIST EN 17853:2023
EN 17853:2023 (E)
Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 7
3 Terms and definitions . 7
4 Principle . 7
5 Reagents . 7
5.1 Analytical standards . 7
5.2 Chemicals . 8
5.3 Standard solutions . 8
5.4 Reagents .
...

SLOVENSKI STANDARD
oSIST prEN 17853:2022
01-julij-2022
Krma: metode vzorčenja in analize - Ugotavljanje nepoškodovanih glukozinolatov
v oljni ogrščici z LC-MS/MS
Animal feeding stuffs: Methods of sampling and analysis - Determination of intact
glucosinolates in rapeseed by LC-MS/MS
Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von intakten
Glucosinolaten in Rapssaat mittels LC-MS/MS
Aliments pour animaux - Méthodes d’échantillonnage et d’analyse - Dosage des
glucosinolates intacts dans les matières premières pour aliments des animaux et les
aliments composés par CL-SM/SM
Ta slovenski standard je istoveten z: prEN 17853
ICS:
65.120 Krmila Animal feeding stuffs
oSIST prEN 17853:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN 17853:2022

---------------------- Page: 2 ----------------------
oSIST prEN 17853:2022


DRAFT
EUROPEAN STANDARD
prEN 17853
NORME EUROPÉENNE

EUROPÄISCHE NORM

May 2022
ICS 65.120
English Version

Animal feeding stuffs: Methods of sampling and analysis -
Determination of intact glucosinolates in rapeseed by LC-
MS/MS
Aliments pour animaux - Méthodes d'échantillonnage Futtermittel - Probenahme- und
et d'analyse - Dosage des glucosinolates intacts dans Untersuchungsverfahren - Bestimmung von intakten
les matières premières pour aliments des animaux et Glucosinolaten in Rapssaat mittels LC-MS/MS
les aliments composés par CL-SM/SM
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 327.

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
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17853:2022 E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------
oSIST prEN 17853:2022
prEN 17853:2022 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 6
3 Terms and definitions . 6
4 Principle . 6
5 Reagents . 6
6 Apparatus . 11
7 Procedure . 12
8 LC-MS/MS analysis .
...

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