Foodstuffs - Determination of zearalenone in edible vegetable oils by LC-FLD or LC-MS/MS

This European Standard describes a procedure for the determination of the zearalenone content in edible vegetable oils specifically maize germ oil by either of the following techniques: High performance liquid chromatography with fluorescence detection (LC-FLD) or high performance liquid chromatography with tandem mass spectrometry (LC-MS/MS) after basic extraction of the diluted oil.
The method has been validated for zearalenone in naturally contaminated maize germ oil at levels of 61,2 µg/kg to 515 µg/kg [5].
Laboratory experiences [6] have shown that this method is also applicable to other vegetable oils such as wheat germ oil (n = 4), sunflower oil (n = 5), pumpkin seed oil (n = 1), soybean oil (n = 5), hemp seed oil (n = 5), rape seed oil (n = 11), and mixed oils including maize germ oil (n = 3). However occasionally, samples can result in interferences in the FLD-chromatograms. In this case, the detection with MS/MS is recommended.

Lebensmittel - Bestimmung von Zearalenon in pflanzlichen Speiseölen mit LC-FLD oder LC-MS/MS

Diese Europäische Norm beschreibt ein Verfahren für die Bestimmung des Zearalenongehalts in pflanzlichen Speiseölen, insbesondere in Maiskeimöl, mit einem der beiden folgenden Verfahren: Hochleistungsflüssig¬chromatographie mit Fluoreszenzdetektion (LC FLD) oder Hochleistungsflüssigchromatographie mit Tandem-Massenspektrometrie (LC MS/MS) nach basischer Extraktion des verdünnten Öles.
Das Verfahren wurde für Zearalenon in natürlich kontaminiertem Maiskeimöl bei Konzentrationen von 61,2 µg/kg bis 515 µg/kg validiert [5].
Laboruntersuchungen [6] haben gezeigt, dass das Verfahren auch für andere pflanzliche Öle, wie z. B. Weizenkeimöl (n = 4), Sonnenblumenöl (n = 5), Kürbiskernöl (n = 1), Sojaöl (n = 5), Hanfsamenöl (n = 5), Rapsöl (n = 11) sowie Pflanzenölmischungen (n = 3), die Maiskeimöl enthalten, anwendbar ist. Jedoch können Proben gelegentlich zu Interferenzen in den FLD Chromatogrammen führen. In diesem Fall wird die Detektion mit MS/MS empfohlen.

Produits alimentaires - Dosage de la zéaralénone dans les huiles végétales alimentaires par CL-DF ou CL-SM/SM

La présente Norme européenne décrit un mode opératoire de détermination de la teneur en zéaralénone dans les huiles végétales alimentaires, notamment l’huile de germes de maïs, par l’une des techniques suivantes : chromatographie liquide à haute performance avec détection de fluorescence (CL-DF) ou chromatographie liquide à haute performance couplée à une spectrométrie de masse en tandem (CL-SM/SM) après extraction basique de l’huile diluée.
La méthode a été validée pour la zéaralénone présente dans l’huile de germes de maïs naturellement contaminée à des niveaux de 61,2 µg/kg à 515 µg/kg [5].
Les expériences menées en laboratoire [6] sans doute ont démontré que cette méthode est également applicable à d’autres huiles végétales telles que l’huile de germes de blé (n = 4), l’huile de tournesol (n = 5), l’huile de pépins de courge (n = 1), l’huile de soja (n = 5), l’huile de chanvre (n = 5), l’huile de colza (n = 11) et les mélanges d’huiles tels que l’huile de germes de maïs (n = 3). Toutefois, les échantillons peuvent parfois provoquer des interférences dans les chromatogrammes issus de la détection par fluorescence (DF). Dans ce cas, il est recommandé d’utiliser la détection par SM/SM.

Živila - Določevanje zearalenona v jedilnih rastlinskih oljih z LC-FLD ali LC-MS/MS

Ta evropski standard opisuje postopek za določanje vsebnosti zearalenona v jedilnih rastlinskih oljih, zlasti v olju iz koruznih kalčkov, z eno od naslednjih tehnik: tekočinska kromatografija visoke ločljivosti s fluorescenčno detekcijo (LC-FLD) ali tekočinska kromatografija visoke ločljivosti s tandemsko masno spektrometrijo (LC-MS/MS) po osnovni ekstrakciji razredčenega olja.
Ta metoda je bila potrjena za zearalenon v naravno kontaminiranem olju iz koruznih kalčkov pri koncentracijah 61,2–515 μg/kg [5].
Laboratorijske izkušnje [6] kažejo, da se ta metoda uporablja tudi za rastlinska olja, kot so olje pšeničnih kalčkov (n = 4), sončnično olje (n = 5), bučno olje (n = 1), sojino olje (n = 5), konopljino olje (n = 5), olje oljne ogrščice (n = 11) in mešana olja, vključno z olji iz koruznih kalčkov (n = 3). Vendar pa vzorci lahko občasno povzročijo motnje v kromatogramih FLD. V tem primeru je priporočena detekcija z MS/MS.

General Information

Status
Published
Publication Date
23-May-2017
Withdrawal Date
29-Nov-2017
Current Stage
9093 - Decision to confirm - Review Enquiry
Completion Date
01-Mar-2023

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Lebensmittel - Bestimmung von Zearalenon in pflanzlichen Speiseölen mit LC-FLD oder LC-MS/MSDenrées alimentaires - Dosage de la zéaralénone dans les huiles végétales alimentaires par CL-FLD ou CL-SM/SMFoodstuffs - Determination of zearalenone in edible vegetable oils by LC-FLD or LC-MS/MS67.200.10Animal and vegetable fats and oilsICS:Ta slovenski standard je istoveten z:EN 16924:2017SIST EN 16924:2017en,fr,de01-september-2017SIST EN 16924:2017SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16924
May
t r s y ICS
x yä t r rä s r English Version
Foodstuffs æ Determination of zearalenone in edible Produits alimentaires æ Dosage de la zéaralénone dans les huiles végétales alimentaires par CLæFLD ou CLæ Lebensmittel æ Bestimmung von Zearalenon in This European Standard was approved by CEN on
t y February
t r s yä
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:
Avenue Marnix 17,
B-1000 Brussels
t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x { t vã t r s y ESIST EN 16924:2017

Typical chromatograms . 16 Annex B (informative)
Example conditions for suitable LC-MS/MS systems . 22 Annex C (informative)
Precision data . 27 Bibliography . 30
= 10 g/l. Weigh in 1 g of ammonium hydrogen carbonate (4.4) into a 100 ml volumetric flask and fill up to the mark with water. Prepare a fresh solution each day of analysis. SIST EN 16924:2017

= 100 µg/ml. Weigh in 10 mg of crystalline zearalenone (4.7) to the nearest 0,1 mg into a 100 ml volumetric flask and fill up to the mark with acetonitrile (4.3). The stock solution is stable for at least 4 weeks to 12 weeks if stored at <
°C [7]. This step can be omitted when using the certified standard solution. The certified standard solution then serves as stock solution. 4.9 Standard solution of zearalenone,
= 10 µg/ml. Pipette 1 ml of the stock solution of zearalenone (4.8) into a 10 ml volumetric flask and fill up to the mark with acetonitrile (4.3). Determine the exact concentration of zearalenone in this standard solution spectrometrically. For this purpose, record the absorption curve of the standard solution from 190 nm to 350 nm against acetonitrile. Calculate the mass concentration of zearalenone in the standard solution st in µg/ml according to Formula (1): max100stEMρδε⋅⋅=⋅=(1)=where=Emax is the maximum extinction value determined from the absorption curve (here: 274 nm); M is the molar mass of zearalenone = 318,4 g/mol;
is the layer thickness of the cuvette in cm;
is the molar extinction coefficient in acetonitrile: 1262 m2/mol. 4.10 Reagents, mobile phases and calibration solutions for LC-FLD analysis: 4.10.1 Glacial acetic acid for LC-FLD, volume fraction
(CH3COOH) approximately 99 %. 4.10.2 Mobile phase A for LC-FLD: Acetonitrile/water/glacial acetic acid (47+52+1, v+v+v). Mix 47 volumes of acetonitrile (4.3) with 52 volumes of water and 1 volume of glacial acetic acid (4.10.1). For the stability of the chromatographic separation it is necessary to acidify the mobile phase. 4.10.3 Mobile phase B for LC-FLD: Acetonitrile (100 %) (4.3). 4.10.4 Calibration solutions of zearalenone for LC-FLD. Prepare a series of calibration solutions from the standard solution (4.9) of zearalenone. According to the pipetting scheme in Table 1, pipette the corresponding volumes of standard solution of zearalenone into volumetric flasks, evaporate the solvent with nitrogen at approximately 40 °C to dryness and dissolve the residue in mobile phase A (4.10.2). Dissolve by means of laboratory shaker (5.4) or ultrasonic bath (5.3) at room temperature. Then fill up to the mark. The calibration range shall be SIST EN 16924:2017

µl Mass concentration of calibration solution
ng/ml 1 10 25 25 2 10 50 50 3 10 100 100 4 10 150 150 5 10 200 200 6 10 250 250 4.11 Reagents, mobile phases, and additional standards and standard solutions for LC-MS/MS analysis: 4.11.1 Methanol, LC quality. 4.11.2 Ammonium hydrogen carbonate (NH4HCO3), for LC-MS, molecular weight: 79 g/mol. 4.11.3 Mobile phase A for LC-MS/MS: 1 mmol/l NH4HCO3 in water/methanol (95+5, v+v). Dissolve 79 mg of ammonium hydrogen carbonate (4.11.2) in 950 ml of water and mix with 50 ml of methanol (4.11.1). 4.11.4 Mobile phase B for LC-MS/MS: 1 mmol/l NH4HCO3 in water/methanol (5+95, v+v). Dissolve 79 mg of ammonium hydrogen carbonate (4.11.2) in 50 ml of water and mix with 950 ml of methanol (4.11.1). 4.11.5 Working solution of zearalenone for calibration,
= 200 ng/ml. Transfer 0,5 ml of the standard solution (4.9) into a 25 ml volumetric flask and fill up to the calibration mark with methanol (4.11.1). 4.11.6 Zearalanone, internal standard (ISTD 1) for LC-MS/MS, e.g. crystalline or as certified standard solution with 10 µg/ml. 4.11.7 Zearalenone, isotopic labelled internal Standard (ISTD 2) for LC-MS/MS, as optional internal standard, e.g. zearalenone [13C18]-labelled. 4.11.8 Stock solution of zearalanone (ISTD 1),
= 100 µg/ml. Weigh in 10 mg of zearalanone (ISTD 1) (4.11.6) to the nearest 0,1 mg into a 100 ml volumetric flask and fill up to the mark with acetonitrile (4.3). The ISTD 1 stock solution is stable for at least 4 weeks to 12 weeks if stored at <
°C [7]. If the certified standard solution is used, the preparation of this stock solution of zearalanone (ISTD 1) is not necessary. SIST EN 16924:2017

= 10 µg/ml. Transfer 1 ml of the stock solution of zearalanone (4.11.8) into a 10 ml volumetric flask and fill up to the calibration mark with methanol (4.11.1). This step can be omitted when using the certified standard solution of zearalanone. The certified standard solution then serves as the internal standard solution of zearalanone (ISTD 1). 4.11.10 Working solution of internal standard zearalanone (ISTD 1) for calibration,
= 200 ng/ml. Transfer 0,5 ml of the internal standard solution of z
...

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