BS ISO 8260-2008 Milk and milk products - Determination of organochlorine pesticides and polychlorobiphenyls - Method using capillary gas-liquid chromatography with electron- captu.pdf

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1、BS ISO 8260:2008ICS 67.100.01NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDMilk and milk products Determinationof organochlorinepesticides andpolychlorobiphenyls Method usingcapillary gas-liquidchromatographywith electron-capturedetectionThis British Standardw

2、as published under theauthority of the StandardsPolicy and StrategyCommittee on 31 2008 BSI 2008ISBN 978 0 580 58540 1Amendments/corrigenda issued since publicationDate CommentsBS ISO 8260:2008National forewordThis British Standard is the UK implementation of ISO 8260:2008.The UK participation in it

3、s preparation was entrusted to TechnicalCommittee AW/5, Chemical analysis of milk and milk products.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are respo

4、nsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.DecemberBS ISO 8260:2008Reference numbersISO 8260:2008(E)IDF 130:2008(E)ISO and IDF 2008INTERNATIONAL STANDARD ISO8260IDF130First edition2008-07-15Milk and milk products Determination o

5、f organochlorine pesticides and polychlorobiphenyls Method using capillary gas-liquid chromatography with electron-capture detection Lait et produits laitiers Dosage des pesticides organochlors et des polychlorobiphnyles Mthode par chromatographie capillaire en phase gazeuse-liquide avec dtection ca

6、pture dlectrons BS ISO 8260:2008ISO 8260:2008(E) IDF 130:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed o

7、n the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobes licensing policy. Neither the ISO Central Secretariat nor the IDF accepts any liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the

8、 software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies and IDF national committees. In the unlikely even

9、t that a problem relating to it is found, please inform the ISO Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO and IDF 2008 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electr

10、onic or mechanical, including photocopying and microfilm, without permission in writing from either ISO or IDF at the respective address below. ISO copyright office International Dairy Federation Case postale 56 CH-1211 Geneva 20 Diamant Building Boulevard Auguste Reyers 80 B-1030 Brussels Tel. + 41

11、 22 749 01 11 Tel. + 32 2 733 98 88 Fax + 41 22 749 09 47 Fax + 32 2 733 04 13 E-mail copyrightiso.org E-mail infofil-idf.org Web www.iso.org Web www.fil-idf.org Published in Switzerland ii ISO and IDF 2008 All rights reservedBS ISO 8260:2008ISO 8260:2008(E) IDF 130:2008(E) ISO and IDF 2008 All righ

12、ts reserved iiiContents Page Foreword iv Foreword. v Introduction . vi 1 Scope . 1 2 Normative references . 1 3 Terms and definitions. 1 4 Principle. 2 5 Reagents and materials . 2 6 Apparatus 4 7 Sampling 4 8 Preparation of sample 4 8.1 Milk . 4 8.2 Evaporated milk 5 8.3 Sweetened condensed milk. 5

13、 8.4 Powdered milk products 5 8.5 Butter and butterfat 5 8.6 Cheese . 5 8.7 Other milk products 5 9 Preparation of test sample. 5 9.1 Extraction of milk 5 9.2 Extraction of sweetened condensed milk, powdered milk products, butter, butterfat and cheese 6 10 Procedure 6 10.1 General. 6 10.2 Blank test

14、. 6 10.3 Cryogenic extraction 6 10.4 Clean-up. 6 10.5 Gas chromatography 7 10.6 Blank result . 8 11 Calculation and expression of results 8 11.1 Calculation of the response factor 8 11.2 Expression of the response factor 8 11.3 Calculation of the organochlorine compound content. 8 11.4 Expression of

15、 the result. 9 11.5 Relative retention time . 9 11.6 Expression of the retention time. 9 12 Precision 9 12.1 General. 9 12.2 Repeatability 9 12.3 Reproducibility 9 13 Test report . 10 Annex A (informative) Interlaboratory trial 11 Annex B (informative) Example of a chromatogram. 12 Bibliography . 14

16、 BS ISO 8260:2008ISO 8260:2008(E) IDF 130:2008(E) iv ISO and IDF 2008 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out

17、 through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO col

18、laborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International S

19、tandards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements

20、 of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 8260IDF 130 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 5, Milk and milk products, and the International Dairy Federation (IDF

21、). It is being published jointly by ISO and IDF. BS ISO 8260:2008ISO 8260:2008(E) IDF 130:2008(E) ISO and IDF 2008 All rights reserved vForeword IDF (the International Dairy Federation) is a non-profit organization representing the dairy sector worldwide. IDF membership comprises National Committees

22、 in every member country as well as regional dairy associations having signed a formal agreement on cooperation with IDF. All members of IDF have the right to be represented on the IDF Standing Committees carrying out the technical work. IDF collaborates with ISO in the development of standard metho

23、ds of analysis and sampling for milk and milk products. Draft International Standards adopted by the Action Teams and Standing Committees are circulated to the National Committees for voting. Publication as an International Standard requires approval by at least 50 % of the IDF National Committees c

24、asting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. IDF shall not be held responsible for identifying any or all such patent rights. ISO 8260IDF 130 was prepared by the International Dairy Federation (IDF) and Technical

25、 Committee ISO/TC 34, Food products, Subcommittee SC 5, Milk and milk products. It is being published jointly by IDF and ISO. All work was carried out by the Joint IDF-ISO Action Team on Organic contaminants of the Standing Committee on Analytical methods for additives and contaminants under the aeg

26、is of its project leader, Mr. R. de Knegt (NL). ISO 8260IDF 130:2008 cancels and replaces IDF 130A:1991, which has been technically revised. BS ISO 8260:2008ISO 8260:2008(E) IDF 130:2008(E) vi ISO and IDF 2008 All rights reservedIntroduction This International Standard is intended for use in the res

27、earch, monitoring and control of organochlorine compounds in milk and milk products by isolation of these compounds. In the past, polychlorinated biphenyls (PCBs) were generally determined by “empirical” methods, most of which used “peak pattern comparison” employing gas-liquid chromatography with e

28、lectron-capture detection (GLC-ECD) and packed columns. For reference compounds, mixtures produced by perchlorination to decachlorobiphenyl (and GLC-ECD determination) or dechlorination to biphenyl were used. The determination was carried out by high-performance liquid chromatography with ultraviole

29、t detection (HPLC-UV) or by gas-liquid chromatography with flame-ionization detection (GLC-FID). The aforementioned techniques have three important drawbacks: 1) By reducing the information on the PCB pattern to only one number (the “PCB content”), the information on the distribution pattern of the

30、isomers is lost. This information is, however, extremely useful for indicating the sources of contamination and for differentiating between background and recent contamination. 2) “PCB contents” determined by the methods mentioned above might be obtained in many different ways as, for most PCB data,

31、 what is meant by “PCB content” is not clearly defined. Most reported “PCB contents” cannot, therefore, be compared, and interpretation of the data is difficult. “PCB contents” are not always defined as the sum of the chlorobiphenyl isomers present in the sample, as one would normally expect. 3) Chl

32、orobiphenyls are individual chemical compounds which have different properties (e.g. biodegradability, toxicological effects, tendency to accumulate). Therefore, it would be highly desirable to determine these compounds separately. As a broad concept, the analysis of PCBs needs to be applicable to m

33、ilk and milk products in different countries throughout the world. To achieve this, the following basic considerations apply: a) the need to consider the different situations in different laboratories, for example the equipment available, the level of training of the laboratory personnel, the budget

34、 available and the special tasks of the laboratory; b) the need to define the purpose of the analysis, for example screening, monitoring and control with respect to legal limits, or research; c) the need to determine simultaneously the PCB and organochlorine pesticide (OCP) content; d) the need to i

35、nclude, as far as possible, information on the PCB isomer-distribution pattern; e) the need to define clearly the contents to be reported; f) the need to control carefully the separation of the PCBs from the OCPs in order to avoid interference. BS ISO 8260:2008INTERNATIONAL STANDARD ISO 8260:2008(E)

36、IDF 130:2008(E) ISO and IDF 2008 All rights reserved 1Milk and milk products Determination of organochlorine pesticides and polychlorobiphenyls Method using capillary gas-liquid chromatography with electron-capture detection WARNING Persons using this International Standard should be familiar with n

37、ormal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This I

38、nternational Standard specifies a method for the determination of the contents of individual organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in milk, evaporated milk, sweetened condensed milk, powdered milk products, butter and butterfat, cheese and other milk products. The met

39、hod is capable of determining low levels of specific OCPs down to 5 g of OCP per kilogram of fat and levels of specific PCBs down to 2,5 g of PCB per kilogram of fat, using capillary gas-liquid chromatography with electron-capture detection (GLC-ECD). 2 Normative references The following referenced

40、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. ISO 14156IDF 172, Milk and milk products Extraction methods for lipids and

41、 liposoluble compounds 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 OCP and PCB contents mass fractions of organochlorine pesticides and polychlorinated biphenyls as determined by the procedure specified in this International Standard. NOT

42、E 1 For products containing more than 2 % fat, the organochlorine compound content is expressed in micrograms or milligrams per kilogram of fat. NOTE 2 For low-fat products containing 2 % fat or less, the organochlorine compound content is expressed in micrograms or milligrams per kilogram of produc

43、t. BS ISO 8260:2008ISO 8260:2008(E) IDF 130:2008(E) 2 ISO and IDF 2008 All rights reserved4 Principle The fat and organochlorine compounds are extracted from a test portion. The organochlorine compounds are isolated by cryogenic extraction and cleaned up in two successive operations using C18 and Fl

44、orisil SPE (solid-phase extraction) cartridges, respectively. The eluate is concentrated and dissolved in a suitable volume of n-hexane. The organochlorine compounds are identified, and also quantified, by capillary gas-liquid chromatography, using trans-nonachlor as an internal standard. 5 Reagents

45、 and materials All reagents shall be of recognized analytical grade and be suitable for pesticide-residue analysis. Water shall be distilled water or water of at least equivalent purity, suitable for pesticide-residue analysis. WARNING Several of the solvents used in this International Standard are

46、highly volatile as well as toxic and/or highly inflammable. Observe current safety precautions for handling, use and disposal. 5.1 Acetonitrile (CH3CN). 5.2 Methylene chloride (CH2Cl2). 5.3 Petroleum ether, with a boiling point of 40 C to 60 C, distilled, if necessary, using a Raschig column of leng

47、th at least 500 mm. 5.4 Diethyl ether (C2H5)2O. 5.5 n-Hexane (C6H14), distilled, if necessary, using a Raschig column of length at least 500 mm, or, alternatively, iso-octane (C8H18). 5.6 Sodium sulfate (Na2SO4). 5.7 Sodium oxalate (Na2C2O4). 5.8 Acetone (CH3COCH3). 5.9 Methanol (CH3OH). 5.10 Dodeca

48、ne (C12H26). 5.11 Eluting solvents, as follows: 5.11.1 Acetonitrile/methylene chloride mixture, ratio 3:1. Mix 3 volumes of acetonitrile (5.1) with 1 volume of methylene chloride (5.2). 5.11.2 Petroleum ether/diethyl ether mixture I, ratio 1:1. Mix 50 volumes of petroleum ether (5.3) with 50 volumes

49、 of diethyl ether (5.4). 5.11.3 Petroleum ether/diethyl ether mixture II, ratio 98:2. Mix 98 volumes of petroleum ether (5.3) with 2 volumes of diethyl ether (5.4). 5.11.4 Petroleum ether/diethyl ether mixture III, ratio 85:15. Mix 85 volumes of petroleum ether (5.3) with 15 volumes of diethyl ether (5.4). BS ISO 8260:2008ISO 8260:2008(E) IDF 130:2008(E) ISO and IDF 2008 All rights reserved 35.12 C18 SPE cartridge, of capacity 6 ml, containing 1 g of filter material of particle size 45 m, pore size 60 (e.g.