1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 1528-1 : 1997 The E
2、uropean Standard EN 1528-1 : 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 1. GeneralBS EN 1528-1 : 1997 This British Standard, having been p
3、repared 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 reference AW/-/3 Draft for comment 94/50
4、5374 DC ISBN 0 580 27379 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, upon which the following bodies were represe
5、nted: 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 1528-1 : 1997 BSI 1997 i Contents Page Committees
6、 responsible Inside front cover National foreword ii Foreword 2 Text of EN 1528-1 3ii BSI 1997 BS EN 1528-1 : 1997 National foreword This British Standard has been prepared by Technical Panel AW/-/3 and is the English language version of EN 1528-1: 1996 Fatty food Determination of pesticides and pol
7、ychlorinated biphenyls (PCBs) Part 1: General published by the European Committee for Standardization (CEN). EN 1528-1 was produced as a result of international discussions in which the United Kingdom took an active part. Cross-references Publication referred to Corresponding British Standard EN 152
8、8-2 : 1996 BS EN 1528-2 : 1997 Fatty food Determination of pesticides and polychlorinated 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
9、) Part 3 : Clean-up methods EN 1528-4 : 1996 BS EN 1528-4 : 1997 Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 4 : Determination, confirmatory tests, miscellaneous The Technical Commmittee has reviewed the provisions of ISO 1750, to which normative reference is mad
10、e in the text, and has decided that they are acceptable for use in conjunction with this standard. ISO 5725 : 1986, to which informative reference is made in the text, has been superseded by ISO 5725-1 : 1994, ISO 5725-2 : 1994, ISO 5725-3 : 1994, ISO 5725-4 : 1994 and ISO 5725-6 : 1994 which are id
11、entical with BS ISO 5725 Accuracy (trueness and precision) of measurement methods and results, BS ISO 5725-1 : 1994 General principles and definitions, BS ISO 5725-2 : 1994 Basic method for the determination of repeatability and reproducibility of a standard measurement method, BS ISO 5725-3 : 1994,
12、 Intermediate measures of the precision of a standard measurement method, BS ISO 5725-4 : 1994 Basic method for the determination of the trueness of a standard measurement method, and BS ISO 5725-6 : 1994 Use in practice of accuracy values. Compliance with a British Standard does not of itself confe
13、r 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 12, an inside back cover and a back cover.CEN European Committee for Standardization Comite Europe en de Normalisation Europa isches Komitee
14、 fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1996 Copyright reserved to CEN members Ref. No. EN 1528-1 : 1996 E EUROPEAN STANDARD EN 1528-1 NORME EUROPE ENNE EUROPA ISCHE NORM November 1996 ICS 67.040 Descriptors: Food products, edible fats, chemical analysis, determination
15、 of content, pesticides, polychlorobiphenyl, gas chromatography, generalities English version Fatty food Determination of pesticides and polychlorinated biphenyls (PCBs) Part 1 : General Aliments gras Dosage des pesticides et des polychlorobiphe nyles (PCB) Partie 1 : Ge ne ralite s Fettreiche Leben
16、smittel Bestimmung von Pestiziden und polychlorierten Biphenylen (PCB) Teil 1 : Allgemeines This European Standard was approved by CEN on 1996-10-27. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status
17、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 Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A vers
18、ion 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 status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Gre
19、ece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.Page 2 EN 1528-1 : 1996 BSI 1997 Foreword This European Standard has been prepared by Technical Committee 275, Food analysis, horizontal methods, the secretariat of which is held by
20、 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 1997, and conflicting national standards shall be withdrawn at the latest by May 1997. According to the CEN/CENELEC Internal Regulations,
21、the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. This Euro
22、pean Standard consists of the following Parts. Part 1 General presents the scope of the standard and describes general considerations with regard to reagents, apparatus, gas chromatography etc., applying to each of the analytical methods selected. Part 2 Extraction of fat, pesticides and PCBs, and d
23、etermination of fat content presents a range of analytical procedures for extracting the fat portion containing the pesticide and PCB residues from different 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 i
24、solated fat portion, respectively, using techniques such as liquidliquid partition, adsorption or gel permeation column chromatography. Part 4 Determination, confirmatory tests, miscellaneous gives guidance on some recommended techniques for the determination of pesticides and PCBs in fatty foodstuf
25、fs 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 Page Foreword 2 Introduction 3 1 Scope 3 2 Normative references 3 3 Principle 3 4 Reagents 4 5 Apparatus 5 6 Procedure 7 7 Determination 8 8 Confirmator
26、y tests 8 9 Evaluation 8 10 Practical limit of determination 9 11 Expression of results 9 12 Test report 9 Annexes A (normative) Applicability of methods 10 B (informative) Purification of some solvents and reagents 11 C (informative) Bibliography 12Page 3 EN 1528-1 : 1996 BSI 1997 1) Florisil is an
27、 example of a suitable product available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of the product named. Introduction This European Standard comprises a range of multi residue methods of equal status:
28、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 used throughout Europe. Any variation in the methods used should be shown to give comparable resu
29、lts. 1 Scope This European Standard specifies methods for the determination of residues of pesticides and polychlorinated biphenyls (PCBs) in fatty food. Each method described in this European Standard is suitable for identifying and quantifying a definite range of those non polar organochlorine and
30、/or organophosphorus pesticides which occur as residues in fats and oils as well as in the fat portion of fat containing foodstuffs, both of either animal or vegetable origin. The PCB indicator congeners usually selected for the enforcement of maximum residue limits (MRLs) are determined along with
31、the organochlorine pesticides. This European Standard contains the following clean-up methods that have been subjected to interlaboratory studies and are adopted throughout Europe. Method A. Liquidliquid partitioning with acetonitrile and clean-up on a Florisil 1) column (AOAC) 1. Method B. Liquidli
32、quid partitioning with dimethylformamide and clean-up on a Florisil column (Specht) 2. Method C. Column chromatography on activated Florisil (AOAC) 3. Method D. Column chromatography on partially deactivated Florisil (Stijve) 4. Method E. Column chromatography on partially deactivated aluminium oxid
33、e (Greve if this is not possible, redistil the water, solvents, and reagents used as described in annex B and check their purity (see 4.2). Note that ion-exchange resins used for demineralized water can be a source of interferences. Purify and periodically activate adsorbents according to the requir
34、ements of the different analytical methods; check their purity (see 4.2). Take every precaution to avoid possible contamination of water, solvents, adsorbents etc. from plastics and rubber materials. If an interference is encountered in a reagent blank determination, then check the purity of all rea
35、gents used. 4.2 Check for purity of reagents 4.2.1 Solvents Concentrate solvents by the factor involved in the respective method to be used. Test for purity by GC under the same conditions as used in the method. The chromatogram should not show any interfering impurity. Extract or concentrate aceton
36、itrile, dimethylformamide and dichloromethane in the same volume as used in the method and examine the resulting solution as above by GC. 4.2.2 Water Extract 10 parts by volume of water with one part by volume of n-hexane or light petroleum, dichloromethane or any other non water miscible solvent us
37、ed in the method. Separate the organic phase, concentrate by the factor involved in the respective method and test for purity by GC under the same conditions as used in the method. The chromatogram should not show any interfering impurity. 4.2.3 Inorganic salts Extract inorganic salts, for example s
38、odium chloride, after purification according to annex B or the requirements of the different analytical methods and any aqueous solution used, with n-hexane or light petroleum, dichloromethane or any other non water miscible solvent used in the method. Concentrate the extract by the factor involved
39、in the respective method and test by GC under the same conditions as used in the method. The chromatogram should not show any interfering impurity. 4.2.4 Adsorbents Elute an amount of adsorbent equal to that used in the analytical method with the corresponding type and volume of solvent or solvent m
40、ixture. Concentrate the eluate as indicated in the analytical method and test for purity by GC. The chromatogram should not show any interfering impurity. Check the activity of adsorbents regularly, for example as described in 5.3.9 of EN 1528-3 : 1996. 4.2.5 Standard materials and solutions Use mat
41、erials of at least 95 % purity and traceable quality as standards for residue analysis. Ensure dilute solutions are prepared and checked frequently, and that standard solutions are stored in glass bottles in a refrigerator and every precaution is taken to avoid possible contamination from plastics o
42、r rubber materials. Ensure that the standard solutions are not directly exposed to sunlight or ultraviolet light. Examine analytical standards for impurities. When stored at220 C, standard materials are generally stable for at least a year or two. To allow equilibration, allow the standards to come
43、up to room temperature before the containers are opened. Stock solutions of concentration 1 mg/ml, if kept in a spark proof refrigerator (at about 4 C), are usually stable for 2 to 3 months. NOTE 1. Changes in volume due to solvent evaporation, for example through the space between a glass stopper a
44、nd the neck of a flask, can be a source of error. NOTE 2. Experience has shown that errors introduced in the preparation, handling and storage of standards and standard solutions are major sources of inaccuracies. Experiences obtained by other national, European and international bodies should be observed 9, 10. 4.3 Safety aspects associated with reagents 4.3.1 General The analysis of pesticide and PCB congener residues in a food matrix includes the use of several hazardous chemicals. The list given in 4.3.2 shows some appropriate safety precautions which shall be observed at all times.
