1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 1528-4 : 1997 The E
2、uropean Standard EN 1528-4 : 1996 has the status of a British Standard ICS 67.040 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 4. Determination, confirmatory tests, miscellaneousBS EN 1528-4 :
3、1997 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Board, was published under the authority of the Standards Board and comes into effect on 15 June 1997 BSI 1997 The following BSI references relate to the work on this standard: Committee
4、 reference AW/-/3 Draft for comment 94/505478 DC ISBN 0 580 27382 2 Amendments issued since publication Amd. No. Date Text affected Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Panel AW/-/3, Food analysis Horizontal methods, upo
5、n which the following bodies were represented: Association of Public Analysts Department of Trade and Industry (Laboratory of the Government Chemist) Food and Drink Federation Institute of Food Science and Technology Ministry of Agriculture Fisheries and Food Royal Society of ChemistryBS EN 1528-4 :
6、 1997 BSI 1997 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 Text of EN 1528-4 3ii BSI 1997 BS EN 1528-4 : 1997 National foreword This British Standard has been prepared by Technical Committee AW/-/3 and is the English language version of EN 1528-4 : 1996
7、Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 4 : Determination, confirmatory tests, miscellaneous published by the European Committee for Standardization (CEN). EN 1528-4 was produced as a result of international discussions in which the United Kingdom took an act
8、ive part. Cross-references Publication referred to Corresponding British Standard EN 1528-1 : 1996 BS EN 1528-1 : 1997 Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 1 : General EN 1528-2 : 1996 BS EN 1528-2 : 1997 Fatty food Determination of pesticides and polychlo
9、rinated biphenyls (PCBs) Part 2 : Extraction of fat, pesticides and PCBs, and determination of fat content EN 1528-3 : 1996 BS EN 1528-3 : 1997 Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 3 : Clean-up methods Compliance with a British Standard does not of itself
10、confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 10, an inside back cover and a back cover.CEN European Committee for Standardization Comite Europe en de Normalisation Europa isches Ko
11、mitee fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1996 Copyright reserved to all CEN members Ref. No. EN 1528-4 : 1996 E EUROPEAN STANDARD EN 1528-4 NORME EUROPE ENNE EUROPA ISCHE NORM November 1996 ICS 67.040 Descriptors: Food products, edible fats, chemical analysis, dete
12、rmination of content, pesticides, polychlorobiphenyl, purity, tests, chemical residues, gas chromatography English version Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 4: Determination, confirmatory tests, miscellaneous Aliments gras Dosage des pesticides et des p
13、olychlorobiphe nyls (PCB) Partie 4: De termination, essais de confirmation, divers Fettreiche Lebensmittel Bestimmung von Pestiziden und polychlorierten Biphenylen (PCB) Teil 4: Verfahren zur Bestimmung und Absicherung, Verschiedenes This European Standard was approved by CEN on 1996-10-27. CEN memb
14、ers 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 applicati
15、on to 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 s
16、ame status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.Page 2 EN 1528-4 : 1996 BSI 1997 Forewo
17、rd 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 shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the lat
18、est by May 1997, and conflicting national standards shall be withdrawn at the latest by May 1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, Fran
19、ce, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. This European Standard consists of the following Parts. Part 1 General presents the scope of the standard and describes general considerations with regard to re
20、agents, apparatus, gas chromatography etc., applying to each of the analytical methods selected. Part 2 Extraction of fat, pesticides and PCBs, and determination of fat content presents a range of analytical procedures for extracting the fat portion containing the pesticide and PCB residues from dif
21、ferent groups of fat-containing foodstuffs. Part 3 Clean-up methods presents the details of methods A to H for the clean-up of fats and oils or the isolated fat portion, respectively, using techniques such as liquidliquid partition, adsorption or gel permeation column chromatography. Part 4 Determin
22、ation, confirmatory tests, miscellaneous gives guidance on some recommended techniques for the determination of pesticides and PCBs in fatty foodstuffs and on confirmatory tests, and lists a clean-up procedure for the removal of the bulk of lipids when analysing large quantities of fat. Contents Pag
23、e Foreword 3 Introduction 3 1 Scope 3 2 Normative references 3 3 General 3 4 Determination 3 5 Confirmatory tests 1 5 6 Additional clean-up procedure for large quantities of fats using Calflo E8 7 Annexes A (informative) Bibliography 9 B (informative) Typical GC operating conditions 9Page 3 EN 1528-
24、4 : 1996 BSI 1997 1) Gaschrom Q, Chromosorb W/HP , Anachrom Q, Apiezon L, DC-11 . Carbowax 20 M are examples of suitable products available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of these products.
25、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 methods selected for inclusion in this standard have been validated and are widely u
26、sed throughout Europe. Any variation in the methods used should be shown to give comparable results. 1 Scope This Part of EN 1528 gives guidance on some recommended techniques for the determination of pesticides and polychlorinated biphenyls (PCBs) in fatty foodstuffs and on confirmatory tests, and
27、lists a clean-up procedure for the removal of the bulk of lipids when analysing large quantities of fat. 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
28、 text and the publications are listed hereafter. For dated references, subsequent 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 ap
29、plies. EN 1528-1 : 1996 Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 1 : General EN 1528-2 : 1996 Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 2 : Extraction of fat, pesticides and PCBs, and determination of fat content EN 1528-
30、3 : 1996 Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 3 : Clean-up methods 3 General The methods described in this Part of EN 1528 permit the residues present to be provisionally identified and quantified, by gas chromatographic methods using selective detectors.
31、All positive results require confirmation 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 measurem
32、ents, etc., are all of value. Results obtained using mass spectrometry (MS) present definitive evidence for confirmation/identification purposes. 4 Determination 4.1 Gas chromatography 4.1.1 General A suitable GC system, preferably equipped with separate heaters for injector, detector and column ove
33、ns, should be used. 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 sh
34、ould be checked periodically by verifying the linearity of the calibration curves using standard solutions of pesticides. The quantification unit of the gas chromatographic system needs to include an integration system which permits the calculation not only of peak heights but also of peak areas. It
35、 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 in any way guarantee that the quality of the results generated will be identical. For
36、typical GC conditions, see annex B. 4.1.2 Columns Either packed or capillary columns may be used. When packed columns are to be used, then glass columns of lengths between 1,5 m and 3 m and of internal diameter (i.d.) 2 mm to 6 mm, are recommended, however, they are not suitable for the separation o
37、f PCB congeners. A robust, inert support should be used. Materials such as Gaschrom Q, Chromosorb W/HP , Anachrom Q in 125mm to 150 mm (100 to 120 mesh), 150mm to 190mm (80 mesh to 100 mesh) or 190mm to 250mm (60 to 80 mesh) ranges have been successfully employed. 1)Page 4 EN 1528-4 : 1996 BSI 1997
38、2) SE-30 . Carbowax 20 M are examples of suitable products available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of these products. A variety of stationary phases and stationary phase mixtures have been
39、used successfully for a variety of residue analyses. For example, the following types are most frequently used Hydrocarbon: Apiezon L; 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
40、, OV-210, SF-2401; Phenylcyanopropylmethylsilicones: DB-1301, DB-1701, OV-225, XE-60; Polyethylene glycol: Carbowax 20 M 1) . Stationary phases should be coated onto the support with care, the ratio depending on the support/phase combination chosen. Newly filled columns should be conditioned for at
41、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 di
42、sconnected from the detector during conditioning. Pure, dry nitrogen (oxygen-free, especially when using an electron capture detector (ECD), or an argon/methane mixture (in the case of a pulsed ECD), should be used as carrier gas for packed columns. The flow rate depends on the size and type of colu
43、mn used. Generally, gas flow rates should be controlled as accurately as possible. Molecular sieve filters should be installed for all gas supplies and regenerated regularly. Finally, GC conditions (column length, stationary phase type, injector, detector and column temperatures, gas flow rates, etc
44、.) should be such that the separation of the pesticides and PCBs likely to be present is as complete as possible. Capillary GC has a separation power superior to that of packed columns. This technique is recommended especially in the case of complex extracts. Fused silica columns having an internal
45、diameter of 0,20 mm to 0,35 mm and a length of between 20 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
46、 stationary phases are frequently used as coatings: SE-30 (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); DB-1701(equivalent to OV-1701,
47、 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, CP-WAX-52-CB, Carbowax 20 M, etc.) 2) A test for separation efficiency of capillary columns, is given in 7.2 of EN 1528-1 : 1996. 4.1.3 Injection techniques Various injection tech
48、niques are useful such as: a) Grob splitless injection. b) On-column injection. c) Programmed Temperature Vaporization (PTV) injection. The applicability of these techniques depends on the apparatus used and on special requirements. 4.2 Preliminary tests Determine the linear dynamic range of detecto
49、r response under the actual GC conditions used by injecting dilute standard solutions. Inject into the gas chromatograph an appropriate volume (between 1,0ml and 10ml depending on the system) of the purified extracts obtained according to the analytical method used. The chromatogram so obtained should enable both the identity and the approximate concentration of the compounds present in the extracts to be established. 4.3 Determination Make sure that all measurements are performed within the li
