EN 15637:2008
(Main)Foods of plant origin - Determination of pesticide residues using LC-MS/MS following methanol extraction and clean-up using diatomaceous earth
Foods of plant origin - Determination of pesticide residues using LC-MS/MS following methanol extraction and clean-up using diatomaceous earth
This European Standard describes a method for the analysis of pesticide residues in foods of plant origin, such as fruits, vegetables, cereals, nuts as well as processed products including dried fruits. The method has been collaboratively studied on a large number of commodity/pesticide combinations.
Pflanzliche Lebensmittel - LC-MS/MS-Verfahren zur Bestimmung von Pestizidrückständen mit Methanolextraktion und Reinigung an Diatomeenerde
Diese Europäische Norm beschreibt ein Verfahren für die Analyse von Pestizidrückständen in pflanzlichen Lebens¬mitteln, wie Früchten, Gemüse, Getreide, Nüssen, als auch verarbeiteten Erzeugnissen, wie beispiels-weise getrockneten Früchten. Das Verfahren wurde gemeinsam mit einer großen Anzahl an Ernte-güter/Pestizid-Kombinationen überprüft.
Aliments d'origine végétale - Détermination des pesticides par LC-MS/MS après extraction méthanolique et purification sur terre de diatomées
La présente Norme européenne spécifie les exigences auxquelles doivent satisfaire les produits manufacturés en polystyrène expansé, avec ou sans parements ou revêtements, utilisés pour l'isolation thermique des bâtiments. Les produits sont fabriqués sous forme de panneaux ou de rouleaux ou toute autre présentation préformée.
La présente norme européenne décrit les caractéristiques du produit et contient les procédures d’essai, d’évaluation de la conformité, de marquage et d’étiquetage.
Les produits relevant du domaine d'application de la présente norme européenne sont également utilisés pour l’isolation acoustique dans des systèmes d'isolation thermique et des panneaux composites préfabriqués ; la performance des systèmes dans lesquels entrent ces produits n'est pas définie.
La présente norme européenne ne spécifie pas, pour une propriété donnée, le niveau exigé que doit atteindre un produit pour démontrer son aptitude à l’emploi dans une application particulière. Les classes et niveaux requis pour une application donnée figurent dans les réglementations ou normes non conflictuelles.
Les produits dont la résistance thermique déclarée à une température de 10 °C est inférieure à 0,25 m2.K/W ou dont la conductivité thermique déclarée à une température de 10°C est supérieure à 0,060 W/(m.K) ne sont pas du domaine d'application de la présente norme européenne.
Hrana rastlinskega izvora - Določanje ostankov pesticidov z uporabo LC-MS/MS za ekstrakcijo z metanolom in čiščenjem z diatomejsko zemljo
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Pflanzliche Lebensmittel - LC-MS/MS-Verfahren zur Bestimmung von Pestizidrückständen mit Methanolextraktion und Reinigung an DiatomeenerdeAliments d'origine végétale - Détermination des pesticides par LC-MS/MS après extraction méthanolique et purification sur terre de diatoméesFoods of plant origin - Determination of pesticide residues using LC-MS/MS following methanol extraction and clean-up using diatomaceous earth67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 15637:2008SIST EN 15637:2009en,fr,de01-april-2009SIST EN 15637:2009SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15637November 2008ICS 67.050 English VersionFoods of plant origin - Determination of pesticide residues usingLC-MS/MS following methanol extraction and clean-up usingdiatomaceous earthAliments d'origine végétale - Détermination des résidus despesticides par LC-MS/MS après extraction méthanolique etpurification sur terre de diatoméesPflanzliche Lebensmittel - LC-MS/MS-Verfahren zurBestimmung von Pestizidrückständen mitMethanolextraktion und Reinigung an DiatomeenerdeThis European Standard was approved by CEN on 13 September 2008.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 CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, 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© 2008 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15637:2008: ESIST EN 15637:2009
Example for appropriate experimental conditions.17 Annex B (informative)
Precision data.21 Bibliography.63
1 Scope This European Standard describes a method for the analysis of pesticide residues in foods of plant origin, such as fruits, vegetables, cereals, nuts as well as processed products including dried fruits. The method has been collaboratively studied on a large number of commodity/pesticide combinations. 2 Principle The sample is extracted with methanol after addition of some water. After partition into dichloromethane the organic phase is evaporated and the residue is reconstituted with methanol. Quantification of pesticide residues is performed by liquid chromatography with tandem mass spectrometric detection, using electrospray ionisation. To achieve the required selectivity the mass spectrometer is operated in the selected reaction monitoring mode (SRM). 3 Reagents 3.1 General and safety considerations Unless otherwise specified, use reagents of recognised analytical grade. Take every precaution to avoid possible contamination of water, solvents, inorganic salts, etc.
3.2 Ammonium formate
3.3 Sodium chloride 3.4 Water, HPLC quality 3.5 Dichloromethane, for residue analysis
3.6 Methanol, HPLC quality 3.7 Internal Standard (ISTD) solutions in methanol,
= 10 µg/ml to 50 µg/ml1)
Table 1 shows a list of potential internal standards that may be used in this method. The concentrations listed refer to the ISTD solutions that should be added at the first extraction step (5.2) and to standard solutions.
Table 1: Potential internal standards (ISTDs) or quality control (QC) standards Name of the compound Log P (octanol-water partion coefficient) Chlorine atoms Concentration C ISTD µg/ml Triphenyl phosphate 4,59 - 20 Tris-(1,3-dichlorisopropyl)-phosphate
3,65 6 50 Bis-nitrophenyl urea (nicarbazin) 3,76 - 10
1)
ρ = mass concentration SIST EN 15637:2009
3.8 Pesticide stock solutions Prepare individual stock solutions of analytical standards at concentrations that are sufficiently high to allow the preparation of complex pesticide mixtures. The solvent used should not negatively influence the stability of the pesticides employed.
NOTE Usually, store stock solutions at ≤ -18 °C. Check the stability of stock solutions during storage regularly. In some cases the addition of acids or bases can be helpful to enhance stability and extend the acceptable storage period. 3.9 Pesticide mixtures Because of the broad applicability of this method and due to the partly divergent pH-stability of pesticides, analyte mixtures of different composition can be needed. These are prepared by mixing together defined volumes of the required analyte stock solutions (3.8) and appropriately diluting them with methanol. The analyte concentrations in this mixture should be sufficient to allow the preparation of the required matrix matched standards (see 3.10.3) with moderate dilution of the blank sample extract (e.g. less than 20 %). Usually, store pesticide mixtures at ≤ -18 °C. Since the stability of the pesticides in the mixture may be lower than in stock solutions, stability has to be checked regularly. In some cases the addition of acids or bases can be helpful to enhance stability and extend acceptable storage times. 3.10 Standard solutions 3.10.1 Standard solutions prepared in pure solvent (solvent-based standards)
Solvent-based standards are prepared by mixing a certain volume of methanol with known amounts of pesticide mixtures (3.9). The preparation of multiple standards of different pesticide concentration is useful to cover a broad concentration range.
NOTE An analyte concentration of 1 µg/ml correlates to a residue level of 0,4 mg/kg when a 10 g sample is employed (e.g. samples with water content > 30 %) or 0,8 mg/kg when a 5 g sample is employed (e.g. cereals). 3.10.2 Standard solutions with internal standard prepared in pure solvent Solvent-based standards with ISTD are prepared by mixing a certain volume of methanol with known amounts of pesticide mixtures (3.9) and a fixed volume of internal standard solution (3.7). The volume used shall result in that concentration of ISTD which is obtained in the final extracts after sample extraction and clean-up (see 5.2 and 5.3). The concentration of internal standard in the final extract (CsampleISTD ) can be calculated using Equation (1). The preparation of multiple standards of different pesticide concentration but with constant ISTD concentration is useful to cover a broad concentration range. endexISTDISTDsampleISTDVVVVVVCVC×××−××=2312)( (1) where: V ISTD is the volume of internal standard solution (3.7) added to the test portion; C ISTD is the concentration of internal standard solution (3.7); V1 is the volume of NaCl solution (2,5 ml); V2 is the volume of measuring flask used in 5.2 (10 ml); SIST EN 15637:2009
3.10.3 Standard solutions prepared in blank matrix extracts (matrix-matched standards)
Prepare matrix-matched standards in the same way as the solvent-based standards, however, instead of pure methanol use extracts of blank samples (prepared as described in 5.2, but without ISTD addition). To minimize errors caused by matrix induced effects during chromatography, it is best to choose similar commodities (e.g. apple for apple samples, carrots for carrot samples, etc.).
The stability of pesticide in matrix-matched standards may be lower than that of standards in pure acetonitrile and has to be checked more thoroughly. 3.11 5 ml cartridge for solid supported liquid/liquid extraction, 5 ml sample volume, diatomaceous earth, for example ChemElut CE 10052)
3.12 20 ml cartridge for solid supported liquid/liquid extraction, 20 ml sample volume, diatomaceous earth, for example ChemElut CE 10202)
4 Apparatus Usual laboratory apparatus and, in particular, the following: 4.1 Carving board and knife, for chopping up food samples for analysis 4.2 Homogenizer or high speed blender, fitted with jar 4.3 Laboratory balance 4.4 Measuring flasks, 10 ml and 20 ml 4.5 Ultrasonic bath 4.6 Centrifuge tubes, 80 ml 4.7 Centrifuge, capable of producing a relative centrifugal force (RCF) of at least 3000 g (at the bottom of the tube) 4.8 Round bottom flasks, 50 ml and 250 ml 4.9 Glass syringe, minimum volume 2 ml
2) ChemElut is a product supplied by Varian, Inc. (Palo Alto, 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. SIST EN 15637:2009
A laboratory sample that is wholly or extensively spoiled or degraded should not be analysed. When possible, prepare laboratory samples immediately after arrival and in any event, before any significant physical or chemical changes have taken place. If a laboratory sample cannot be prepared without delay, it should be stored under appropriate conditions to keep it fresh and to avoid deterioration. Generally, laboratory samples should not be stored longer than 3 days before preparation. Dried or similarly processed samples should be analysed within their stated shelf life.
5.1.3 Partly-prepared test sample
For preparation of the partly-prepared test sampl
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