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1、BS EN 12393-3:2008 ICS 67.080.01 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Foods of plant origin Multiresidue methods for the gas chromatographic determination of pesticide residues Part 3: Determination and confirmatory tests Licensed Copy: London South
2、 Bank University, South Bank University, 31/01/2009 03:22, Uncontrolled Copy, (c) BSI This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 November 2008 BSI 2008 ISBN 978 0 580 58224 0 Amendments/corrigenda issued since publication DateComments
3、 BS EN 12393-3:2008 National foreword This British Standard is the UK implementation of EN 12393-3:2008. It supersedes BS EN 12393-3:1999 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee AW/-/3, Food analysis - Horizontal methods. A list of organizatio
4、ns represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations.
5、Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:22, Uncontrolled Copy, (c) BSI BS EN 12393-3:2008 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 12393-3 November 2008 ICS 67.080.01Supersedes EN 12393-3:1998 English Version Foods of plant origin - Multiresidue
6、methods for the gas chromatographic determination of pesticide residues - Part 3: Determination and confirmatory tests Aliments dorigine vgtale - Mthodes multirsidus de dtermination par chromatographie en phase gazeuse de rsidus de pesticides - Partie 3: Dtermination et essais de confirmation Pflanz
7、liche Lebensmittel - Multiverfahren zur gaschromatographischen Bestimmung von Pestizidrckstnden - Teil 3: Verfahren zur Bestimmung und Absicherung This European Standard was approved by CEN on 13 September 2008. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulat
8、e 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 to the CEN Management Centre or to any CEN member. This European Standard exi
9、sts 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 CEN Management Centre has the same status as the official versions. CEN members are the national standards
10、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.
11、 EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2008 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 12393-3:2008: E Licens
12、ed Copy: London South Bank University, South Bank University, 31/01/2009 03:22, Uncontrolled Copy, (c) BSI BS EN 12393-3:2008 EN 12393:2008 (E) 2 Contents Page Foreword3 Introduction.4 1 Scope 5 2 Normative references5 3 General5 4 Determination.5 4.1 Gas chromatography (GC)5 4.1.1 General5 4.1.2 GC
13、 columns6 4.1.3 Injection techniques6 4.1.4 Detectors 7 4.2 Preliminary tests7 4.3 Determination.7 5 Confirmatory tests.7 5.1 General7 5.2 Mass spectrometry8 5.3 Alternative GC columns8 5.4 Alternative GC detectors.8 5.5 High performance liquid chromatography (HPLC).8 5.6 Column fractionation.9 5.7
14、Derivatization .9 5.7.1 Chemical reactions9 5.7.2 Physical reactions .9 5.7.3 Other methods .9 5.8 Spectral measurements 9 Annex A (informative) Typical GC operating conditions10 A.1 Organochlorine pesticides .10 A.1.1 Operating conditions 110 A.1.2 Operating conditions 210 A.2 Organophosphorus pest
15、icides.10 A.2.1 Operating conditions 110 A.2.2 Operating conditions 210 Annex B (informative) Analysis of pesticide residues using mass spectrometry12 Bibliography13 Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:22, Uncontrolled Copy, (c) BSI BS EN 12393-3:2008 EN
16、 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
17、 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
18、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
19、 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
20、 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 confir
21、matory 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 Europe
22、an 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 K
23、ingdom. Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:22, Uncontrolled Copy, (c) BSI BS EN 12393-3:2008 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 pr
24、ime 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
25、 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. Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:22, Uncontrolled Copy,
26、 (c) BSI BS EN 12393-3:2008 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 th
27、ose 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 t
28、he 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 det
29、ermination 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
30、 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 th
31、e 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 cl
32、early 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
33、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 c
34、hecked periodically by verifying the linearity of the calibration curves using standard solutions of pesticides. Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:22, Uncontrolled Copy, (c) BSI BS EN 12393-3:2008 EN 12393:2008 (E) 6 The quantification unit of the gas
35、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
36、 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
37、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 (wa
38、ter-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. F
39、inally, 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 m
40、m 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
41、 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-C
42、B, 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
43、 applicability of these techniques depends on the apparatus used and on special requirements. 1) SE-30. Carbowax 20M 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 thes
44、e products. Licensed Copy: London South Bank University, South Bank University, 31/01/2009 03:22, Uncontrolled Copy, (c) BSI BS EN 12393-3:2008 EN 12393:2008 (E) 7 4.1.4 Detectors See EN 12393-1:2008, 3.4. 4.2 Preliminary tests Determine the linear dynamic range of detector response under the actual
45、 GC conditions used by injecting diluted standard solutions. Inject into the gas chromatograph an appropriate volume (between 1,0 l and 10,0 l, depending on the system) of the purified extracts obtained according to the analytical method used in EN 12393-2. The chromatogram so obtained should enable
46、 both the identity and the approximate concentration of the compounds present in the extracts to be established. 4.3 Determination Make sure that all the measurements are performed within the linear dynamic range of the system. Prepare at least two standard solutions of the identified pesticide in t
47、he same solvent as used in the final extract. Their concentrations should encompass the probable concentration expected in the final extract. Then inject equal volumes of the final extracts obtained and of the two or more standard solutions into the gas chromatograph. It is essential that the inject
48、ions of the purified portions of the sample extracts are preceded and followed by injection of the standard solutions. Measure the peak areas or peak heights. The results obtained from any two successive injections of the same standard solution should not differ more than approximately 10 % from eac
49、h other. Inclusion of an internal standard is useful. It is necessary to ensure that the standard materials and samples are dissolved in the same solvent, otherwise varying evaporation profiles will result which could lead to changes in the retention times and peak areas or heights. A quantitative determination is possible if the mean of recoveries from replicate determinations falls within the range of 70 % up to 110 %, with a relative standard deviation less or equal to 20 %. Compliance with this condition has to be checked perio
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