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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 12393-3:1999 The Eu
2、ropean Standard EN 12393-3:1998 has the status of a British Standard ICS 67.050 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Non-fatty foods Multiresidue methods for the gas chromatographic determination of pesticide residues Part 3: Determination and confirmatory tests Lic
3、ensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 08:46:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 12393-3:1999 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Committee, was published under the authority of the Standards Commit
4、tee and comes into effect on 15 March 1999 BSI 03-1999 ISBN 0 580 30562 7 Amendments issued since publication Amd. No.DateText affected National foreword This British Standard is the English language version of EN 12393-3:1998. The UK participation in its preparation was entrusted to Technical Panel
5、 AW/-/3, Food analysis horizontal methods, which has the responsibility to: aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European
6、 developments and promulgate them in the UK. A list of organizations represented on this panel can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Cat
7、alogue under the section entitled International Standards Correspondence Index, or by using the Find facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their cor
8、rect application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 8, an inside back cover and a back cover. Licensed Copy: sheffieldun sheffieldu
9、n, na, Sat Oct 28 08:46:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI CEN European Committee for Standardization Comite Europe en de Normalisation Europa isches Komitee fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any me
10、ans reserved worldwide for CEN national Members. Ref. No. EN 12393-3:1998 E EUROPEAN STANDARDEN 12393-3 NORME EUROPE ENNE EUROPA ISCHE NORM October 1998 ICS 67.040 Descriptors: food products, chemical analysis, determination of content, pesticides, pesticide residues, chromatographic analysis, gas c
11、hromatography, designation, purity, tests English version Non-fatty foods Multiresidue methods for the gas chromatographic determination of pesticide residues Part3: Determination and confirmatory tests Aliments non gras Me thodes multire sidus de de termination par chromatographie en phase gazeuse
12、de re sidus de pesticides Partie 3: De termination et essais de confirmation Fettarme Lebensmittel Multiverfahren zur gaschromatographischen Bestimmung von Pestizidru cksta nden Teil 3: Verfahren zur Bestimmung und Absicherung This European Standard was approved by CEN on 7 September98. CEN members
13、are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application t
14、o 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 translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same
15、status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: sheffieldun
16、 sheffieldun, na, Sat Oct 28 08:46:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 2 EN 12393-3:1998 BSI 03-1999 Foreword This European Standard has been prepared by Technical Committee CEN/TC 275, Food analysis horizontal methods, the Secretariat of which is held by DIN. This European Standard s
17、hall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by April 1999, and conflicting national standards shall be withdrawn at the latest by April 1999. This European Standard EN 12393, Non-fatty foods Multiresidue methods for the
18、 gas chromatographic determination of pesticide residues, consists of 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 clea
19、n-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
20、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, Czech Republic, Denmark, Finland, France, Ger
21、many, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Contents Page Foreword2 Introduction3 1Scope3 2Normative references3 3General3 4Determination3 5Confirmatory tests5 Annex A (informative) Typical GC operating conditio
22、ns7 Annex B (informative) Analysis of pesticide residues using mass spectrometry8 Annex C (informative) Bibliography8 Licensed Copy: sheffieldun sheffieldun, na, Sat Oct 28 08:46:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 3 EN 12393-3:1998 BSI 03-1999 Introduction This European Standard comp
23、rises 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 metho
24、ds can be applied to a 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 1 are appropriate to improve method performance, see clause 3. 1 Sc
25、ope This European Standard gives guidance on some recommended techniques for the determination of pesticide residues in non-fatty foods 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 residu
26、e limit has been exceeded. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequ
27、ent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. EN 12393-1:1998, Non-fatty foods Multiresidue methods for the gas chrom
28、atographic determination of pesticide residues Part 1: General considerations. 3 General The methods described in this European Standard permit the residues present to be provisionally identified and quantified by gas chromatographic methods using selective detectors. All positive results require co
29、nfirmation of identity and quantity. The procedures listed for confirmation, such as alternative GC columns, alternative GC detectors, thin-layer chromatography (TLC), high-performance liquid chromatography (HPLC), column fractionation, derivatization, spectral measurements, etc. are all of value. R
30、esults obtained using mass spectrometry (MS) present the most definitive evidence for confirmation/identification purpose. As already described in the introduction, on certain occasions it is possible to improve the method performance by variations in equipment used, extraction, clean-up and chromat
31、ographic conditions. Such variations shall always be 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 facili
32、ty 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 instr
33、uctions. Variations in detector sensitivity should be checked periodically by verifying the linearity of the calibration curves using standard solutions of pesticides. The quantification unit of the gas chromatographic apparatus should include an integration system which permits the calculation not
34、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
35、 generated will be identical. For typical GC conditions, see annex A. 4.1.2 GC columns 4.1.2.1 General Either packed or capillary columns can be used. Capillary columns have a separation power superior to that of packed columns. The capillary technique is recommended, especially in the case of compl
36、ex extracts. 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 pest
37、icides. The end of the column should always be disconnected from the detector during conditioning. Pure (oxygen-free) and dry (water-free) nitrogen, especially when using an electron capture detector (ECD), or an argon/methane mixture (in the case of a pulsed ECD), should be used as the carrier gas
38、for packed columns. The flow rate depends on the size and type of column used. Generally, ensure that gas flow rates are controlled as accurately as possible. Molecular sieve filters should be installed for all gas supplies and regenerated regularly. Licensed Copy: sheffieldun sheffieldun, na, Sat O
39、ct 28 08:46:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 4 EN 12393-3:1998 BSI 03-1999 1) Gaschrom Q, Chromosorb W/HP, Anachrom Q, are examples of suitable products available commercially. This information is given for the convenience of users of this standard and does not constitute an endors
40、ement by CEN of these products. 2) Apiezon L, ., Carbowax 20 M are examples of suitable products available commercially. This information is given for the convenience of users of this standard and does not constitute an endorsement by CEN of these products. 3) SE-30. Carbowax 20 M are examples of su
41、itable products available commercially. This information is given for the convenience of users of this standard and does not constitute an endorsement by CEN of these products. Finally, make sure that the GC conditions (column length, stationary phase type, injector, detector and column temperatures
42、, gas flow rates, etc.) are such that the separation of the pesticides likely to be present is as complete as possible. 4.1.2.2 Packed columns Glass columns, of length between 1 m and 3 m and of internal diameter (i.d.) 2 mm to 6 mm, are recommended. A robust, inert support should be used: materials
43、 such as Gaschrom Q, Chromosorb W/HP, Anachrom Q in 60 mesh/80 mesh (190 mm to 250 mm), 80 mesh/100 mesh (150 mm to 190 mm) and 100 mesh/120 mesh (125 mm to 150 mm) ranges have been successfully employed1). A variety of stationary phases and stationary phase mixtures have been used successfully for
44、a variety of residue analyses. For example, the following types are most frequently used: Hydrocarbon:Apiezon L2) Methylsilicones:DC-11, DC-200, OV-1, OV-101, SP-2100, SE-30 Methylphenylsilicones:OV-17, OV-25, OV-61, SP-2250, SE-52, SE-54 Trifluoropropylmethylsilicones:QF-1, OV-210, SF-2401 Phenylcy
45、anopropylmethylsilicones:DB-1301, DB-1701, OV-225, XE-60 Polyethylene glycol:Carbowax 20 M2) Stationary phases should be coated onto the support with care, the ratio depending on the support/phase combination chosen. 4.1.2.3 Capillary columns Fused silica columns having an internal diameter of 0,20
46、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 phase
47、s are frequently used as coatings: SE-303)(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
48、, SPB-7 etc.) OV-225(equivalent to DB-225, SIL-43-CB, SPB-2330 etc.) Wax(equivalent to DB-Wax, Wax-52-CB, Carbowax 20 M2)etc.) 4.1.3 Injection techniques Various injection techniques are useful, such as: a) Grob splitless injection; b) on-column injection; c) programmed temperature vaporization (PTV
49、) injection. The applicability of these techniques depends on the apparatus used and on special requirements. 4.1.4 Detectors See EN 12393-1:1998, 3.4. 4.2 Preliminary tests Determine the linear dynamic range of detector response under the actual GC conditions used by injecting diluted standard solutions. Inject into the gas chromatograph an appropriate volume (between 1,0 ml and 10,0 ml, depending on the system) of the purified extracts obtained according to the analytical method used. The chromatogram so obtained should enabl