EN ISO 9167:2019
(Main)Rapeseed and rapeseed meals - Determination of glucosinolates content - Method using high-performance liquid chromatography (ISO 9167:2019)
Rapeseed and rapeseed meals - Determination of glucosinolates content - Method using high-performance liquid chromatography (ISO 9167:2019)
This document specifies a method for the determination of the individual glucosinolates content in rapeseeds and rapeseed meals using high-performance liquid chromatography with gradient elution.
This method was tested on rapeseeds and rapeseed meals (Brassica rapa, Brassica napus and Brassica juncea) but is applicable to other plant materials, on the condition that the occurring glucosinolates previously identified are described in this document. On the contrary, the quantitative analysis of the concerned glucosinolate(s) is not carried out.
NOTE This method does not determine glucosinolates that are substituted on the glucose molecule, but these compounds are of little importance in commercial rapeseed and rapeseed meal.
Annex A presents the results of the interlaboratory trials for the gradient elution HPLC method. Annex B presents how to check the titre of the prepared internal standard solution. Annex C presents how to prepare and test the purified sulfatase solution and how to check the desulphation step on the ion exchange column. Annex D presents the HPLC and column performance criteria qualification.
The analysis of glucosinolates content in rapeseed can also be done using an isocratic elution mode. This requires some modifications of the method (internal, standard, HPLC column and HPLC buffers), as described in Annex E.
Rapssamen und Rapsschrot - Bestimmung des Glucosinolatgehaltes - Verfahren mittels Hochleistungsflüssigchromatographie (ISO 9167:2019)
Dieses Dokument legt ein Verfahren zur Bestimmung der einzelnen Glucosinolate in Rapssamen und Rapsschrot mittels Hochleistungsflüssigkeitschromatographie mit Gradientenelution fest.
Dieses Verfahren wurde an Rapssamen und Rapsschrot (Brassica rapa, Brassica napus und Brassica juncea) geprüft, ist jedoch auf andere Pflanzenmaterialien unter der Bedingung anwendbar, dass die vorkommenden Glucosinolate zuvor identifiziert wurden und in diesem Dokument beschrieben sind. Die quantitative Bestimmung des (der) betreffenden Glucosinolats (Glucosinolate) wird nicht durchgeführt.
ANMERKUNG Glucosinolate, die am Glucosemolekül substituiert sind, werden mit diesem Verfahren nicht erfasst, sind für handelsübliche Rapssamen und Rapsschrot jedoch auch von untergeordneter Bedeutung.
Anhang A enthält die Ergebnisse der Ringversuche für das HPLC Verfahren mit Gradientenelution. Anhang B stellt dar, wie der Titer der hergestellten internen Standardlösung überprüft wird. Anhang C stellt dar, wie die gereinigte Sulfatase Lösung hergestellt und geprüft wird und wie der Desulfatierungsschritt an der Ionenaustauschersäule überprüft wird. Anhang D stellt die Qualifikation der HPLC- und Säulenleistungs¬kriterien dar.
Die Analyse des Glucosinolatgehalts in Rapssamen kann auch unter Anwendung eines isokratischen Elutionsmodus erfolgen. Das erfordert einige Modifikationen des Verfahrens (interner Standard, HPLC Säule und HPLC Pufferlösungen), wie in Anhang E beschrieben.
Graines et tourteaux de colza - Dosage des glucosinolates - Méthode par chromatographie liquide à haute performance (ISO 9167:2019)
Le présent document spécifie une méthode de dosage des glucosinolates individuels dans les graines et tourteaux de colza par chromatographie en phase liquide à haute performance avec élution par gradient.
Cette méthode a été soumise à essai sur les graines et tourteaux de colza (Brassica rapa, Brassica napus et Brassica juncea), mais elle est applicable à d'autres matériaux végétaux, à condition que les glucosinolates identifiés précédemment soient décrits dans le présent document. Sinon, l'analyse quantitative du ou des glucosinolates concernés n'est pas effectuée.
NOTE Cette méthode ne dose pas les glucosinolates ayant des substituants sur la partie glucose, mais ces composés sont peu importants dans les graines et tourteaux de colza commercialisés.
L'Annexe A présente les résultats des essais interlaboratoires pour la méthode de CLHP avec élution par gradient. L'Annexe B présente comment vérifier le titre de la solution préparée d'étalon interne. L'Annexe C présente comment préparer et analyser la solution purifiée de sulfatase et contrôler l'étape de désulfatation sur la colonne échangeuse d'ions. L'Annexe D présente la qualification du système de CLHP et des critères de performance de la colonne.
Les glucosinolates des graines de colza peuvent également être dosés en utilisant un mode d'élution isocratique. Cela nécessite un certain nombre de modifications de la méthode (étalon interne, colonne de CLHP et solutions tampons pour CLHP), comme décrit dans l'Annexe E.
Seme in obroki oljne repice - Določevanje glukozinolatov - Metoda s tekočinsko kromatografijo visoke ločljivosti (ISO 9167:2019)
Ta dokument določa metodo za določevanje vsebnosti posameznih glukozinolatov v semenu in obrokih oljne repice s pomočjo tekočinske kromatografije visoke ločljivosti z gradientnim eluiranjem. Ta metoda je bila preskušena na semenu in obrokih oljne repice (Brassica rapa, Brassica napus in Brassica juncea), vendar se uporablja tudi za druge rastlinske materiale pod pogojem, da so v tem dokumentu opisani obstoječi glukozinolati, ki so bili predhodno prepoznani. Nasprotno se ne opravi kvantitativna analiza zadevnega glukozinolata oziroma glukozinolatov.
OPOMBA: Ta metoda ne določa glukozinolatov, ki so v molekuli glukoze nadomeščeni, vendar te spojine v okviru obroka komercialne oljne repice in oljne repice nimajo velikega pomena. V dodatku A so predstavljeni rezultati medlaboratorijskih preskusov za gradientno eluiranje po metodi HPLC. V dodatku B je predstavljeno, kako je mogoče preveriti porabo pripravljene raztopine iz internega standarda. V dodatku C je predstavljeno, kako pripraviti in preskusiti prečiščeno raztopino sulfataze ter kako preveriti korak desulfatizacije v koloni za ionsko izmenjavo. V dodatku D sta predstavljeni metoda HPLC in uvrstitev merila uspešnosti kolone. Analiza vsebnosti glukozinolatov v oljni repici je mogoča tudi z načinom izokratskega eluiranja. Za to je potrebnih nekaj prilagoditev metode (notranje, standardne, kolona HPLC in puferske raztopine za HPLC), kot je opisano v dodatku E.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2019
Nadomešča:
SIST EN ISO 9167-1:1998
SIST EN ISO 9167-1:1998/A1:2013
Seme in obroki oljne repice - Določevanje glukozinolatov - Metoda s tekočinsko
kromatografijo visoke ločljivosti (ISO 9167:2019)
Rapeseed and rapeseed meals - Determination of glucosinolates content - Method using
high-performance liquid chromatography (ISO 9167:2019)
Rapssamen und Rapsschrot - Bestimmung des Glucosinolatgehaltes - Verfahren mittels
Hochleistungsflüssigchromatographie (ISO 9167:2019)
Graines et tourteaux de colza - Dosage des glucosinolates - Méthode par
chromatographie liquide à haute performance (ISO 9167:2019)
Ta slovenski standard je istoveten z: EN ISO 9167:2019
ICS:
67.200.20 Oljnice Oilseeds
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 9167
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2019
EUROPÄISCHE NORM
ICS 67.200.20
English Version
Rapeseed and rapeseed meals - Determination of
glucosinolates content - Method using high-performance
liquid chromatography (ISO 9167:2019)
Graines et tourteaux de colza - Dosage des Rapssamen und Rapsschrot - Bestimmung des
glucosinolates - Méthode par chromatographie liquide Glucosinolatgehaltes - Verfahren mittels
à haute performance (ISO 9167:2019) Hochleistungsflüssigchromatographie (ISO 9167:2019)
This European Standard was approved by CEN on 4 May 2019.
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
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COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 9167:2019 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
This document (EN ISO 9167:2019) has been prepared by Technical Committee ISO/TC 34 "Food
products" in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats
and oils and their by-products - Methods of sampling and analysis” the secretariat of which is held by
AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by December 2019, and conflicting national standards
shall be withdrawn at the latest by December 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 9167-1:1995.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: 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 the
United Kingdom.
Endorsement notice
The text of ISO 9167:2019 has been approved by CEN as EN ISO 9167:2019 without any modification.
INTERNATIONAL ISO
STANDARD 9167
First edition
2019-05
Rapeseed and rapeseed meals —
Determination of glucosinolates
content — Method using high-
performance liquid chromatography
Graines et tourteaux de colza — Dosage des glucosinolates —
Méthode par chromatographie liquide à haute performance
Reference number
ISO 9167:2019(E)
©
ISO 2019
ISO 9167:2019(E)
© ISO 2019
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ISO 9167:2019(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
6 Apparatus . 4
7 Sampling . 5
8 Preparation of the test sample . 6
9 Procedure. 6
9.1 Test portion . 6
9.2 Extraction of glucosinolates . 6
9.3 Blank test . 7
9.4 Preparation of ion-exchange columns . 7
9.5 Purification and desulfatation . 7
9.6 Chromatography with gradient elution . 7
9.6.1 General. 7
9.6.2 Adjustment of the apparatus . 8
10 Expression of results . 9
10.1 Calculation of the content of each glucosinolate . 9
10.2 Relative proportionality factors . 9
10.3 Calculation of the total glucosinolate content .10
11 Precision .10
11.1 Interlaboratory test.10
11.2 Repeatability .10
11.3 Reproducibility .10
12 Test report .11
Annex A (informative) Results of interlaboratory trials — Gradient elution HPLC method .12
Annex B (normative) Checking of the titre of the prepared internal standard solution.14
Annex C (normative) Preparation and test of purified sulfatase solution and checking of the
desulphation step on ion-exchange columns .15
Annex D (informative) HPLC system and column performance criteria qualification .20
Annex E (informative) Elution in the isocratic mode .22
Bibliography .28
ISO 9167:2019(E)
Foreword
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