EN 12393-2:2008
(Main)Foods of plant origin - Multiresidue methods for the gas chromatographic determination of pesticide residues - Part 2: Methods for extraction and cleanup
Foods of plant origin - Multiresidue methods for the gas chromatographic determination of pesticide residues - Part 2: Methods for extraction and cleanup
This European Standard specifies methods for the extraction and clean-up of food samples of plant origin for quantitative determination of pesticide residues.
Different solvents can be used for this purpose. These pesticide residues are generally associated with other co-extracted compounds which would interfere in the analysis. To purify the crude extracts to be analysed, several techniques can be used.
This standard contains the following extraction and clean-up methods that have been subjected to interlaboratory studies and /or are adopted throughout Europe:
- method L: Extraction with acetone, liquid-liquid partition with dichloromethane and clean-up on a silica gel/charcoal column [1];
- method M: Extraction with acetone and liquid-liquid partition with dichloromethane/light petroleum, if necessary clean-up on Florisil® 1) [2], [3], [4];
- method N: Extraction with acetone, liquid-liquid partition with dichloromethane or cyclohexane/ethyl acetate and clean-up with gel permeation and silica gel chromatography [5], [6];
- method P: Extraction with ethyl acetate, and if necessary, clean-up by gel permeation chromatography [7].
This European Standard specifies the details of methods L to P for the extraction and the clean-up of food samples of plant origin. Several solvents at different volumes are used for extraction. Techniques of clean-up are listed such as liquid-liquid partition, liquid chromatography on various adsorbents and gel permeation chromatography.
A table providing the couples (matrix/pesticide) which have been submitted to collaborative studies and a list of indicative applicability of the method to different pesticides are given for each method, wherever possible.
Pflanzliche Lebensmittel - Multiverfahren zur gaschromatographischen Bestimmung von Pestizidrückständen - Teil 2: Verfahren zur Extraktion und Reinigung
Diese Europäische Norm legt Verfahren für die Extraktion und Reinigung pflanzlicher Lebensmittel zur Bestimmung von Pestizidrückständen fest.
Zu diesem Zweck können verschiedene Lösemittel verwendet werden. Die Pestizidrückstände liegen im Allgemeinen gemeinsam mit mitextrahierten Begleitstoffen vor, die bei der Analyse stören können. Zur Reinigung dieser rohen Extrakte können unterschiedliche Verfahren angewendet werden.
Diese Europäische Norm enthält die folgenden Extraktions und Reinigungsverfahren, die in Ringversuchen erfolgreich geprüft worden und/oder in ganz Europa anerkannt sind:
- Verfahren L: Extraktion mit Aceton, Flüssig/flüssig Verteilung mit Dichlormethan und Reinigung an einer Kieselgel/Aktivkohle Säule [1];
- Verfahren M: Extraktion mit Aceton und Flüssig/flüssig Verteilung mit Dichlormethan/Petroleumbenzin, falls erforderlich, Reinigung an Florisil® ) [2], [3], [4];
- Verfahren N: Extraktion mit Aceton, Flüssig/flüssig Verteilung mit Dichlormethan oder Cyclohexan/Ehtyl-acetat und Reinigung durch Gelpermeations und Kieselgel Chromatographie [5], [6];
- Verfahren P: Extraktion mit Ethylacetat und, falls erforderlich, Reinigung durch Gelpermeations-Chromatographie [7].
Diese Europäische Norm legt Einzelheiten der Verfahren L bis P zur Extraktion und Reinigung von Proben pflanzlicher Lebensmittel fest. Zur Extraktion werden mehrere Lösemittel in unterschiedlichen Mengen verwendet. Als Reinigungsverfahren werden z. B. die Flüssig/flüssig Verteilung, die Flüssigkeitschromatogra-phie an verschiedenen Adsorptionsmitteln und die Gelpermeations Chromatographie aufgeführt.
Soweit möglich, ist in jedem Verfahren der jeweilige Anwendungsbereich beschrieben, und die Pestizid/ Matrix-Kombinationen, die in Ringversuchen untersucht wurden, sind tabellarisch aufgelistet, siehe Tabelle 3.
Aliments d'origine végétale - Méthodes multirésidus de détermination par chromatographie en phase gazeuse de résidus de pesticides - Partie 2: Méthodes d'extraction et de purification
La présente Norme européenne spécifie des méthodes pour l'extraction et la purification d'échantillons d'aliments d’origine végétale en vue du dosage des résidus de pesticides.
Différents solvants peuvent ainsi être utilisés. Ces résidus de pesticides sont généralement associés à d'autres composés co-extraits pouvant interférer avec l'analyse. Plusieurs méthodes peuvent être utilisées pour purifier les extraits bruts devant être analysés.
La présente Norme européenne contient les méthodes suivantes qui ont été soumises à des études interlaboratoires et/ou qui sont adoptées dans toute l'Europe :
méthode L : Extraction par acétone, partage liquide-liquide par dichlorométhane et purification sur colonne de silicagel/charbon actif [1] ;
méthode M : Extraction par acétone, partage liquide-liquide par dichlorométhane/éther de pétrole et purification sur colonne de Florisil® ) si nécessaire [2], [3], [4] ;
méthode N : Extraction par acétone, partage liquide-liquide par dichlorométhane ou cyclohexane/acétate d’éthyle et purification par chromatographie par perméation sur gel et au silicagel [5], [6] ;
méthode P : Extraction avec acétate d'éthyle et, si nécessaire, purification par chromatographie par perméation de gel [7].
La présente Norme européenne détaille les méthodes L à P, pour l'extraction et la purification d'échantillons d'aliments d’origine végétale. L'extraction fait appel à plusieurs solvants, à différents volumes. Les techniques de purifications telles que la séparation liquide-liquide, la chromatographie liquide sur divers adsorbants et la chromatographie sur colonne de perméation de gel sont indiquées.
Un tableau contenant les couples (matrice/pesticide) qui ont été soumis à des études collaboratives, ainsi qu'une liste indicative d'applicabilité de la méthode aux différents pesticides sont donnés pour chaque méthode, lorsque c'est possible.
Živila rastlinskega izvora - Multirezidualne metode za določevanje ostankov pesticidov s plinsko kromatografijo - 2. del: Metode za ekstrakcijo in čiščenje
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Pflanzliche Lebensmittel - Multiverfahren zur gaschromatographischen Bestimmung von Pestizidrückständen - Teil 2: Verfahren zur Extraktion und ReinigungAliments d'origine végétale - Méthodes multirésidus de détermination par chromatographie en phase gazeuse de résidus de pesticides - Partie 2: Méthodes d'extraction et de purificationFoods of plant origin - Multiresidue methods for the gas chromatographic determination of pesticide residues - Part 2: Methods for extraction and cleanup67.080.01Sadje, zelenjava in njuni proizvodi na splošnoFruits, vegetables and derived products in general67.050Splošne preskusne in analizne metode za živilske proizvodeGeneral methods of tests and analysis for food productsICS:Ta slovenski standard je istoveten z:EN 12393-2:2008SIST EN 12393-2:2009en,fr,de01-februar-2009SIST EN 12393-2:2009SLOVENSKI
STANDARDSIST EN 12393-2:19991DGRPHãþD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 12393-2November 2008ICS 67.080.01Supersedes EN 12393-2:1998
English VersionFoods of plant origin - Multiresidue methods for the gaschromatographic determination of pesticide residues - Part 2:Methods for extraction and cleanupAliments d'origine végétale - Méthodes multirésidus dedétermination par chromatographie en phase gazeuse derésidus de pesticides - Partie 2: Méthodes d'extraction etde purificationPflanzliche Lebensmittel - Multiverfahren zurgaschromatographischen Bestimmung vonPestizidrückständen - Teil 2: Verfahren zur Extraktion undReinigungThis 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 12393-2:2008: ESIST EN 12393-2:2009
Average water content of crops and foods.37 Bibliography.38
- Part 2 "Methods for extraction and clean-up" presents methods L to P for the extraction and clean-up using techniques such as liquid-liquid partition, adsorption column chromatography or gel permeation column chromatography, etc.
- Part 3 "Determination and confirmatory tests" gives some recommended techniques for the qualitative and the quantitative measurements of residues and the confirmation of the results.
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, 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 the United Kingdom. SIST EN 12393-2:2009
Different solvents can be used for this purpose. These pesticide residues are generally associated with other co-extracted compounds which would interfere in the analysis. To purify the crude extracts to be analysed, several techniques can be used. This standard contains the following extraction and clean-up methods that have been subjected to interlaboratory studies and /or are adopted throughout Europe: method L: Extraction with acetone, liquid-liquid partition with dichloromethane and clean-up on a silica gel/charcoal column [1]; method M: Extraction with acetone and liquid-liquid partition with dichloromethane/light petroleum, if necessary clean-up on Florisil® 1) [2], [3], [4]; method N: Extraction with acetone, liquid-liquid partition with dichloromethane or cyclohexane/ethyl acetate and clean-up with gel permeation and silica gel chromatography [5], [6]; method P: Extraction with ethyl acetate, and if necessary, clean-up by gel permeation chromatography [7]. This European Standard specifies the details of methods L to P for the extraction and the clean-up of food samples of plant origin. Several solvents at different volumes are used for extraction. Techniques of clean-up are listed such as liquid-liquid partition, liquid chromatography on various adsorbents and gel permeation chromatography. A table providing the couples (matrix/pesticide) which have been submitted to collaborative studies and a list of indicative applicability of the method to different pesticides are given for each method, wherever possible. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 12393-1:2008, Foods of plant origin – Multiresidue methods for the gas chromatographic determination of pesticide residues – Part 1: General considerations EN 12393-3, Foods of plant origin – Multiresidue methods for the gas chromatographic determination of pesticide residues – Part 3: Determination and confirmatory tests 3 Principles As already described in the introduction, in certain occasions it is possible to improve the method performance by variations in equipment used, extraction, clean-up and chromatographic conditions. Such variations shall be always clearly documented and demonstrated to give valid results.
1) Florisil® is an example of a suitable product available commercially. This information is given for convenience of users of this standard and does not constitute an endorsement by CEN of this product. SIST EN 12393-2:2009
(M S) g (V S) ml M S / V S g/ml L 100 Acetone: 200 ½
M 100 Acetone: 200 ½
N
100 a Acetone: 200 ½
P 50 Ethyl acetate: 100 ½
a Only relevant if the water content of the matrix is greater than 70 %. 4.2 Clean-up 4.2.1 Liquid-liquid partition The liquid-liquid partition procedures are summarized in Table 2. Table 2 —Liquid-liquid partition Methods Aliquot portion of extract Volume of added water Volume of solvent Ratio
(A E) ml (V W) ml (V S) ml A E / V W L 50 (= 20 %) 250 50 1/5 M 80 0 200 - a N 200 x a 100 - a a Depends on the water content of the matrix. Two techniques of liquid-liquid partition are proposed: with added water (methods L, N); no added water (method M).
4.2.2 Adsorption column chromatography Methods: L, M, N with different adsorbents: silica gel, charcoal, Florisil®, used pure or in mixture. SIST EN 12393-2:2009
Heat at 500 °C for at least 4 h, allow to cool and store in a stoppered bottle. 5.2.9 Activated charcoal 5.2.10 Silica gel 60 for column chromatography, 63 µm to 200 µm (70 mesh to 230 mesh) 5.2.11 Celite® 5453) (optional) 5.3 Apparatus Usual laboratory equipment in accordance with EN 12393-1 and, in particular, the following:
2) BioBeads® S-X 3 is an example of a suitable product available commercially. This information is given for convenience of users of this standard and does not constitute an endorsement by CEN of this product. 3) Celite® 545 is an example of a suitable product available commercially. This information is given for convenience of users of this standard and does not constitute an endorsement by CEN of this product. SIST EN 12393-2:2009
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