SIST EN 12393-3:2009
(Main)Foods of plant origin - Multiresidue methods for the gas chromatographic determination of pesticide residues - Part 3: Determination and confirmatory tests
Foods of plant origin - Multiresidue methods for the gas chromatographic determination of pesticide residues - Part 3: Determination and confirmatory tests
This European Standard gives guidance on some recommended techniques for the determination of pesticide residues in foods of plant origin and on confirmatory tests.
The identity of any observed pesticide residue is confirmed, particularly in those cases in which it would appear that the maximum residue limit has been exceeded.
Pflanzliche Lebensmittel - Multiverfahren zur gaschromatographischen Bestimmung von Pestizidrückständen - Teil 3: Verfahren zur Bestimmung und Absicherung
Diese Europäische Norm gibt Leitlinien für einige Techniken zur Ermittlung der Pestizidrückstände in
pflanzlichen Lebensmitteln und Absicherung der Ergebnisse.
Die Identität jedes gefundenen Pestizid-Rückstandes wird insbesondere dann bestätigt, wenn die
Höchstmenge anscheinend überschritten ist.
Aliments d'origine végétale - Méthodes multirésidus de détermination par chromatographie en phase gazeuse de résidus de pesticides - Partie 3 : Détermination et essais de confirmation
La présente Norme européenne énonce des lignes directrices relatives aux techniques recommandées pour la détermination des résidus de pesticides et aux essais de confirmation.
L'identité de tout résidu de pesticide est confirmée, en particulier lorsqu'il semble que la limite maximale de résidu a été dépassée.
Živila rastlinskega izvora - Multirezidualne metode za določevanje ostankov pesticidov s plinsko kromatografijo - 3. del: Določevanje in potrditveni preskusi
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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 3: Verfahren zur Bestimmung und AbsicherungAliments d'origine végétale - Méthodes multirésidus de détermination par chromatographie en phase gazeuse de résidus de pesticides - Partie 3 : Détermination et essais de confirmationFoods of plant origin - Multiresidue methods for the gas chromatographic determination of pesticide residues - Part 3: Determination and confirmatory tests67.080.01Sadje, 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 12393-3:2008SIST EN 12393-3:2009en,fr,de01-februar-2009SIST EN 12393-3:2009SLOVENSKI
STANDARDSIST EN 12393-3:19991DGRPHãþD
SIST EN 12393-3:2009
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 12393-3November 2008ICS 67.080.01Supersedes EN 12393-3:1998
English VersionFoods of plant origin - Multiresidue methods for the gaschromatographic determination of pesticide residues - Part 3:Determination and confirmatory testsAliments d'origine végétale - Méthodes multirésidus dedétermination par chromatographie en phase gazeuse derésidus de pesticides - Partie 3: Détermination et essais deconfirmationPflanzliche Lebensmittel - Multiverfahren zurgaschromatographischen Bestimmung vonPestizidrückständen - Teil 3: Verfahren zur Bestimmungund AbsicherungThis 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 12393-3:2008: ESIST EN 12393-3:2009
EN 12393:2008 (E) 2 Contents Page Foreword.3 Introduction.4 1 Scope.5 2 Normative references.5 3 General.5 4 Determination.5 4.1 Gas chromatography (GC).5 4.1.1 General.5 4.1.2 GC columns.6 4.1.3 Injection techniques.6 4.1.4 Detectors.7 4.2 Preliminary tests.7 4.3 Determination.7 5 Confirmatory tests.7 5.1 General.7 5.2 Mass spectrometry.8 5.3 Alternative GC columns.8 5.4 Alternative GC detectors.8 5.5 High performance liquid chromatography (HPLC).8 5.6 Column fractionation.9 5.7 Derivatization.9 5.7.1 Chemical reactions.9 5.7.2 Physical reactions.9 5.7.3 Other methods.9 5.8 Spectral measurements.9 Annex A (informative) Typical GC operating conditions.10 A.1 Organochlorine pesticides.10 A.1.1 Operating conditions 1.10 A.1.2 Operating conditions 2.10 A.2 Organophosphorus pesticides.10 A.2.1 Operating conditions 1.10 A.2.2 Operating conditions 2.10 Annex B (informative)
Analysis of pesticide residues using mass spectrometry.12 Bibliography.13
SIST EN 12393-3:2009
EN 12393:2008 (E) 3 Foreword This document (EN 12393-3:2008) has been prepared by Technical Committee CEN/TC 275 “Food analysis - Horizontal methods”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by May 2009, and conflicting national standards shall be withdrawn at the latest by May 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 12393-3:1998 with following significant technical changes: a) revision of Clause 4 “Determination”: outdated techniques are deleted; b) revision of Clause 5 “Confirmatory tests”: outdated techniques are deleted. This European Standard EN 12393 " Foods of plant origin - Multiresidue methods for the gas chromatographic determination of pesticide residues" is divided in three parts: Part 1 "General considerations" provides general considerations with regard to reagents, apparatus, gas chromatography, etc., applying to each of the analytical selected methods; 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 12393-3:2009
EN 12393:2008 (E) 4 Introduction This European Standard comprises a range of multi-residue methods of equal status: no single method can be identified as the prime method because, in this field, methods are continuously developing. The selected methods included in this standard have been validated and/or are widely used throughout Europe. Because these methods can be applied to the very wide range of food commodities/pesticide combinations, using different systems for determination, there are occasions when variations in equipment used, extraction, clean-up and chromatographic conditions are appropriate to improve method performance, see Clause 3. SIST EN 12393-3:2009
EN 12393:2008 (E) 5 1 Scope This European Standard gives guidance on some recommended techniques for the determination of pesticide residues in foods of plant origin and on confirmatory tests. The identity of any observed pesticide residue is confirmed, particularly in those cases in which it would appear that the maximum residue limit has been exceeded. 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 12393-2, Foods of plant origin – Multiresidue methods for the gas chromatographic determination of pesticide residues – Part 2: Methods for extraction and clean-up 3 General The methods specified in this European Standard permit identification and quantification of pesticide residues by gas chromatography using selective detectors. All relevant results require confirmation of identity and quantity. The procedures listed for confirmation such as alternative GC columns, alternative GC detectors, high-performance liquid chromatography (HPLC), column fractionation, derivatization, spectral measurements, etc. are all of value. Results obtained using mass spectrometry (MS) present the most definitive evidence for confirmation/identification purpose. 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. 4 Determination 4.1 Gas chromatography (GC) 4.1.1 General A suitable GC system, preferably equipped with separate heaters for injector, detector and column ovens, shall be used. The facility to inject directly on the GC column is generally of advantage. Although the choice of the different parts of the GC system is a matter for the experience of the analyst, the following general recommendations are made. The detectors should be properly adjusted, according to the manufacturers' instructions. Variations in detector sensitivity should be checked periodically by verifying the linearity of the calibration curves using standard solutions of pesticides. SIST EN 12393-3:2009
EN 12393:2008 (E) 6 The quantification unit of the gas chromatographic apparatus should include an integration system which permits the calculation not only of peak heights but also peak areas. It has been found in practice that equivalent results can be achieved despite the adoption of different GC conditions, and different makes of instruments. On the other hand, specifying standard GC parameters does not guarantee that the quality of the results generated will be identical. For typical GC conditions, see Annex A. 4.1.2 GC columns Columns should be conditioned for at least 24 h at a temperature near the maximum recommended operating temperature with the type of stationary phase used and should then be tested for their efficiency and selectivity at the required operating temperature using standard mixtures of pesticides. The end of the column should always be disconnected from the detector during conditioning. Pure (oxygen-free) and dry (water-free) nitrogen, hydrogen or helium should be used as carrier gas. The flow rate depends on the size and type of column used. Generally, ensure that gas flow rates are controlled as accurately as possible. Gas purification filters should be installed for all gas supplies and replaced regularly. Finally, make sure that the GC conditions (column length, stationary phase type, injector, detector and column temperatures, gas flow rates, etc.) are such that the separation of the pesticides likely to be present is as complete as possible. Fused silica columns having an internal diameter of 0,20 mm to 0,35 mm and a length of between 10 m and 60 m have proved particularly satisfactory because of their separation efficiency, service life and mechanical properties. Wide bore columns having an internal diameter of 0,5 mm to 0,8 mm may also be useful in some cases. The following stationary phases are frequently used as coatings: SE-301)
(equivalent to OV-1, DB-1, CP Sil 5, BP-1, SPB-1, etc.) SE-54 (equivalent to DB-5, CP Sil 8, BP-5, SPB-5, etc.) OV-17 (equivalent to OV-11, OV-22, SP-2250, DC-710, DB-608, etc.) DB-1301 (equivalent to DB-624, etc.) DB-1701 (equivalent to OV-1701, CP-SIL-19-CB, BP-10, SPB-7, etc.) OV-225 (equivalent to DB-225, SIL-43-CB, SPB-2330, etc.) Wax (equivalent to DB-Wax, Wax-52-CB, Carbowax 20M1), etc.) 4.1.3 Injection techniques Various injection techniques are useful such as split/splitless injection or programmed temperature vaporization (PTV) injection. The applicability of these techniques depends on the apparatu
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