Determination of citrinin in food by liquid chromatography tandem mass spectrometry (LC-MS/MS)

This document describes a procedure for the determination of the citrinin content in food (cereals, red yeast rice (RYR)), herbs and food supplements by liquid chromatography tandem mass spectrometry (LC MS/MS).
This method has been validated for citrinin in red yeast rice and in the formulated food supplements in the range of 2,5 µg/kg to 3000 µg/kg and in wheat flour in the range of 2,5 µg/kg to 100 µg/kg.
Laboratory experiences have shown that this method is also applicable to white rice, herbs such as a powder of ginkgo biloba leaves and the formulated food supplements in the range of 2,5 µg/kg to 50 µg/kg.

Lebensmittel - Bestimmung von Citrinin in Lebensmitteln mit Flüssigchromatographie und Tandem-Massenspektrometrie (LC-MS/MS)

Diese Europäische Norm beschreibt ein Verfahren zur Bestimmung des Citriningehalts in Lebensmitteln (Getreide, rotem Reis [RYR, en: red yeast rice)], Kräutern und Nahrungsergänzungsmitteln mit Flüssigchromatographie und Tandem-Massenspektrometrie (LC-MS/MS).
Dieses Verfahren wurde für Citrinin in rotem Reis und in entsprechend zusammengesetzten Nahrungs-ergänzungsmitteln im Bereich von 2,5 μg/kg bis 3000 μg/kg sowie für Citrinin in Weizenmehl im Bereich von 2,5 μg/kg bis 100 μg/kg validiert.
Laborerfahrungen haben gezeigt, dass dieses Verfahren auch auf weißen Reis, auf Kräuter wie Ginkgo-Biloba-Blätter in Pulverform und entsprechend zusammengesetzte Nahrungsergänzungsmittel im Bereich von 2,5 μg/kg bis 50 μg/kg anwendbar ist.

Produits alimentaires - Dosage de la citrinine dans les produits alimentaires par chromatographie liquide couplée à une spectrométrie de masse en tandem (CL-SM/SM)

Le présent document décrit un mode opératoire de détermination de la teneur en citrinine dans les aliments [céréales, levure de riz rouge (LRR)], les herbes aromatiques et les compléments alimentaires par chromatographie liquide couplée à une spectrométrie de masse en tandem (CL‐SM/SM). Cette méthode a été validée pour la citrinine dans la levure de riz rouge et dans les compléments
alimentaires à base de levure de riz rouge dans la gamme de concentration de 2,5 μg/kg à 3 000 μg/kg et dans la farine de blé dans la gamme de concentration de 2,5 μg/kg à 100 μg/kg. Les expériences en laboratoire ont montré que cette méthode est également applicable au riz blanc, aux herbes aromatiques telles que les feuilles de Ginkgo biloba en poudre et aux compléments alimentaires
formulés dans la gamme de concentration de 2,5 μg/kg à 50 μg/kg.

Živila - Določevanje citrinina v živilih s tekočinsko kromatografijo s tandemsko masno spektrometrijo (LC-MS/MS)

Ta evropski standard opisuje postopek za določevanje vsebnosti citrinina v živilih (žito, rdeči riž), zeliščih in prehranskih dopolnilih s tekočinsko kromatografijo s tandemsko masno spektrometrijo (LC-MS/MS).
Ta metoda je potrjena za rdeči kvasni riž v razponu od 2,5 do 3000 μg/kg in pšenično moko v razponu od 2,5 do 100 μg/kg.
Laboratorijske izkušnje kažejo, da se metoda uporablja tudi za beli riž, zelišča, kot so listi dvokrpega ginka (Ginkgo biloba) v prahu, in že pripravljena prehranska dopolnila.

General Information

Status
Withdrawn
Publication Date
18-Dec-2018
Withdrawal Date
04-May-2021
Current Stage
9960 - Withdrawal effective - Withdrawal
Completion Date
05-May-2021

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittel - Bestimmung von Citrinin in Lebensmitteln mit Flüssigchromatographie und Tandem-Massenspektrometrie (LC-MS/MS)Produits alimentaires - Dosage de la citrinine dans les produits alimentaires par chromatographie liquide couplée à une spectrométrie de masse en tandem (CL-SM/SM)Foodstuffs - Determination of citrinin in food by liquid chromatography tandem mass spectrometry (LC-MS/MS)67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 17203:2018SIST EN 17203:2019en,fr,de01-marec-2019SIST EN 17203:2019SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 17203
December
t r s z ICS
x yä r w r English Version
Foodstuffs æ Determination of citrinin in food by liquid Produits alimentaires æ Dosage de la citrinine dans les produits alimentaires par chromatographie liquide
Lebensmittel æ Bestimmung von Citrinin in Lebensmitteln mit Flüssigchromatographie und TandemæMassenspektroThis European Standard was approved by CEN on
{ November
t r s zä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Rue de la Science 23,
B-1040 Brussels
t r s z CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s y t r uã t r s z ESIST EN 17203:2019

Page
European foreword . 3 Introduction . 4 1 Scope . 5 2 Normative references . 5 3 Terms and definitions . 5 4 Principle . 5 5 Reagents . 5 6 Apparatus and equipment . 8 7 Procedure. 9 7.1 Preparation of the test sample . 9 7.2 Extraction of citrinin . 9 7.3 Spiking procedure . 10 7.4 Preparation of sample test solutions . 10 7.5 LC-MS/MS analysis . 10 7.6 Identification . 12 8 Calculation . 12 8.1 General . 12 8.2 Calculation with the internal standard citrinin (ISTD) . 12 9 Precision . 14 9.1 General . 14 9.2 Repeatability . 14 9.3 Reproducibility . 14 10 Test report . 15 Annex A (informative)
Example conditions for suitable LC-MS/MS systems . 16 A.1 Settings for chromatography for WATERS Acquity H-class coupled to a Xevo® TQ-S . 16 A.2 Mass spectrometric detection settings . 17 Annex B (informative)
Typical chromatograms . 18 Annex C (informative)
Precision data . 21 Bibliography . 24
IEC Electropedia: available at http://www.electropedia.org/
ISO Online browsing platform: available at http://www.iso.org/obp 4 Principle A test portion is humidified with a hydrochloric acid aqueous solution and extracted with ethyl acetate/acetonitrile/glacial acetic acid mixture for 60 min. Magnesium sulfate and sodium chloride are added to the extract, agitated and centrifuged in order to expel water and allow phase separation from the mixture. An aliquot of supernatant is collected, filtered, isotopic labelled internal standard (ISTD) solution is added and analysed by reversed phase LC-MS/MS. Quantification is based on matching citrinin/citrinin-13C ratios and citrinin concentrations. 5 Reagents Use only reagents of recognized analytical grade and water complying with grade 1 of EN ISO 3696, unless otherwise specified. Commercially available solutions with equivalent properties to those listed may also be used. 5.1 Ethyl acetate, analytical grade or higher. 5.2 Acetonitrile, LC-MS grade. . 5.3 Glacial acetic acid (CH3COOH), analytical grade or higher. 5.4 Glacial acetic acid (CH3COOH), LC-MS grade. 5.5 Magnesium sulfate; anhydrous (MgSO4), analytical grade or higher. SIST EN 17203:2019

« s z °C. 5.16 Mobile phase A: ammonium acetate/glacial acetic acid in water, c = 5 mmol/l. Add 1 ml of ammonium acetate/glacial acetic acid in water (5.15) to 999 ml of water (5.9) and mix thoroughly. 5.17 Mobile phase B: ammonium acetate/glacial acetic acid in methanol, c = 5 mmol/l. Add 1 ml of ammonium acetate/glacial acetic acid in water (5.15) to 999 ml of methanol (5.10) and mix thoroughly. 5.18 Citrinin, analytical standard > 99 %, e.g. crystalline or as certified standard solution. 5.19 Citrinin stock solution, mass concentration
= 500 µg/ml. Weigh 5 mg of crystalline citrinin to the nearest 0,1 mg into a 10 ml volumetric flask and dissolve with acetonitrile (5.2) by filling up to the mark. The mass concentration of this stock solution shall be checked. This can be achieved via LC-MS/MS analysis against the certified standard solution (5.18) or by a photometric determination of concentration using the molar extinction coefficient [8]. The certified standard solution (5.18) can alternatively be used as stock solution. SIST EN 17203:2019

= 100 µg/ml. Pipette 1 ml of the stock solution (5.19) into 4 ml of the dilution solution (5.14) and homogenize the mixture. A correction factor (see 5.19) shall be determined and used to correct the exact concentration of this working solution (mass concentration
= 100 µg/ml). This step may be omitted when using the ce
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