EN 15054:2006

Non fatty foods - Determination of chlormequat and mepiquat - LC-MS method

This draft European Standard specifies a method using high performance liquid chromatography/mass spectrometry (LC-MS) for the determination of the growth regulators chlormequat and mepiquat in non fatty foods as chlormequat and mepiquat cation, respectively.
The method is applicable to all kinds of fruits, vegetables and cereal products. It has been collaboratively studied on mushrooms, pears, wheat flour and fruit puree, see [1].

Fettarme Lebensmittel - Bestimmung von Chlormequat und Mepiquat - LC-MS-Verfahren

Aliments non gras - Détermination du chlorméquat et du mépiquat - Méthode CL-SM

La présente Norme européenne spécifie une méthode utilisant la Chromatographie liquide à haute
performance/Spectrométrie de masse (CL-SM) pour la détermination des substances ou régulateurs de
croissance chlorméquat et mépiquat dans des aliments non gras respectivement sous la forme de cation
chlorméquat et de cation mépiquat.
La méthode s'applique à toutes les sortes de fruits, légumes et produits céréaliers. Elle a fait l'objet d'études
réalisées en collaboration sur des champignons, des poires, de la farine de blé et de la purée de fruit (voir [1]).

Nemastna živila – Določevanje klormekvata in mepikvata – Metoda LC-MS

General Information

• Status: Published
• Publication Date: 16-May-2006
• Withdrawal Date: 29-Nov-2006
• ICS: 67.060 - Cereals, pulses and derived products
• ICS: 67.080.01 - Fruits, vegetables and derived products in general
• Technical Committee: CEN/TC 275 - Food analysis - Horizontal methods
• Drafting Committee: CEN/TC 275/WG 3 - Pesticides and PCB's in foods of animal origin
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Completion Date: 05-Jun-2023
• Ref Project: SIST EN 15054:2006 - Non fatty foods - Determination of chlormequat and mepiquat - LC-MS method

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Non fatty foods - Determination of chlormequat and mepiquat - LC-MS method&06Aliments non gras - Détermination du chlorméquat et du mépiquat - Méthode CL-SMFettarme Lebensmittel - Bestimmung von Chlormequat und Mepiquat - LC-MS-VerfahrenTa slovenski standard je istoveten z:EN 15054:2006SIST EN 15054:2006en67.050ICS:SLOVENSKI
STANDARDSIST EN 15054:200601-september-2006

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15054May 2006ICS 67.060; 67.080.01 English VersionNon fatty foods - Determination of chlormequat and mepiquat -LC-MS methodAliments non gras - Détermination du chlorméquat et dumépiquat - Méthode CL-SMFettarme Lebensmittel - Bestimmung von Chlormequat undMepiquat - LC-MS-VerfahrenThis European Standard was approved by CEN on 20 April 2006.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2006 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15054:2006: E

Examples of experimental conditions.9 Annex B (informative)
Precision data.16 Bibliography.18

3.4 Glacial acetic acid, mass fraction w at least 96 g/100 g 3.5 Acetonitrile, HPLC quality 3.6 Methanol, HPLC quality 3.7 Water, suitable for HPLC 3.8 Chlormequat chloride stock solution, mass concentration (C5H13NCl2) = 4,30 µg/ml in methanol This stock solution contains 3,33 µg/ml chlormequat cation. 3.9 Mepiquat chloride stock solution, (C7H16NCl) = 4,37 µg/ml in methanol This stock solution contains 3,33 µg/ml mepiquat cation.
1) Celite 545 is a product supplied by Celite Corp. (World Minerals Inc., Santa Barbara, CA, USA). This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of the product named. Equivalent products may be used if they can be shown to lead to the same results.

Prepare six calibration solutions (no. 1 to no. 6) in 10 ml volumetric flasks as follows. Into the flasks, pipette 10 µl, 50 µl, 100 µl, 300 µl, 1 000 µl or 3 000 µl each of chlormequat chloride stock solution (3.8) and of mepiquat chloride stock solution (3.9). To all flasks add 60 µl of the internal standard solution 1 (3.10) and 60 µl of the internal standard solution 2 (3.11). Dilute the solutions no. 1 to no. 5 to the mark with a methanol/water mixture 1 + 1 (V/V) and solution no. 6 with water. All six calibration solutions contain 100 ng/ml of d4-chlormequat cation and 100 ng/ml of d3-mepiquat cation. Solutions no. 1 to no. 6 contain 3,3 ng/ml, 16,7 ng/ml, 33,3 ng/ml, 100 ng/ml, 333 ng/ml and 1 000 ng/ml each of chlormequat cation and of mepiquat cation respectively. On the basis of a 20 g test portion, this corresponds to 0,01 mg/kg, 0,05 mg/kg, 0,10 mg/kg, 0,30 mg/kg, 1,00 mg/kg or 3,00 mg/kg each of chlormequat cation and mepiquat cation. 4 Apparatus Usual laboratory apparatus and, in particular, the following: 4.1 Homogenizer or high speed blender, fitted with jar
4.2 Centrifuge, capable of producing a centrifugal acceleration of at least 3 000 g at the bases of the centrifuge tubes 4.3 Syringe, capacity of at least 2 ml 4.4 Syringe filter, pore size 0,45 µm (polyamide or polytetrafluoroethylene) 4.5 Glass vials, 1,8 ml volume; applicable for automatic injection into an autosampler 4.6 LC-MS system, equipped with electrospray interface 5 Procedure 5.1 Preparation of the samples Where possible, carry out the analysis of samples immediately on their arrival in the laboratory. Do not analyse a laboratory sample which is wholly or extensively spoiled. For analysis take only the portion of the laboratory sample to which the maximum residue level applies. No further plant-parts may be removed. A record of the plant-parts which have been removed shall be kept. The sample thus prepared is the test sample.

NOTE 1 Typically, a response ratio of about 1 should be obtained with the calibration solution no. 4 (corresponding to a mass fraction of 0,3 mg/kg for the 20 g test portion). The resulting slope of the calibration graphs should be approximately 3,3 kg/mg. NOTE 2 Since the calibration range shall be appropriate to the residue concentrations found, it may be necessary to construct more than one calibration graph from the results of calibration measurements. Measure the peak height (or peak area) obtained for chlormequat and mepiquat cation in the sample test solution and divide it by the peak height (or peak area) obtained for the peak of the corresponding internal standard (d4-chlormequat or d3-mepiquat, respectively). Based on the resulting response ratios and the two calibration graphs calculate the mass fraction
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