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

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1、BS ISO 8260:2008 ICS 67.100.01 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Milk and milk products Determination of organochlorine pesticides and polychlorobiphenyls Method using capillary gas-liquid chromatography with electron-capture detectionThis Britis

2、h Standard was published under the authority of the Standards Policy and Strategy Committee on 31 2008 BSI 2008 ISBN 978 0 580 58540 1 Amendments/corrigenda issued since publication Date Comments BS ISO 8260:2008 National foreword This British Standard is the UK implementation of ISO 8260:2008. The

3、UK participation in its preparation was entrusted to Technical Committee AW/5, Chemical analysis of milk and milk products. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of

4、a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. DecemberBS ISO 8260:2008 BS ISO 8260:2008Reference numbers ISO 8260:2008(E) IDF 130:2008(E) ISO and IDF 2008INTERNATIONAL STANDARD ISO 8260 IDF 130 First e

5、dition 2008-07-15 Milk and milk products Determination of 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 chromatograp

6、hie capillaire en phase gazeuse-liquide avec dtection capture dlectrons BS ISO 8260:2008 BS ISO 8260:2008 ISO 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 edit

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9、use by ISO member bodies and IDF national committees. In the unlikely event 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 pub

10、lication may be reproduced or utilized in any form or by any means, electronic 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

11、 20 Diamant Building Boulevard Auguste Reyers 80 B-1030 Brussels Tel. + 41 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 reserved

12、BS ISO 8260:2008 BS ISO 8260:2008 ISO 8260:2008(E) IDF 130:2008(E) ISO and IDF 2008 All rights reserved iii Contents 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

13、 8 Preparation of sample 4 8.1 Milk . 4 8.2 Evaporated milk 5 8.3 Sweetened condensed milk. 5 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

14、 milk products, butter, butterfat and cheese 6 10 Procedure 6 10.1 General. 6 10.2 Blank test. 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 re

15、sponse factor 8 11.3 Calculation of the organochlorine compound content. 8 11.4 Expression of 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) I

16、nterlaboratory trial 11 Annex B (informative) Example of a chromatogram. 12 Bibliography . 14 BS ISO 8260:2008 BS ISO 8260:2008 ISO 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 natio

17、nal standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out 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. Internati

18、onal organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rul

19、es given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. 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

20、least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements 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 8260 IDF 130 was prepared by Technical Committee

21、ISO/TC 34, Food products, Subcommittee SC 5, Milk and milk products, and the International Dairy Federation (IDF). It is being published jointly by ISO and IDF. BS ISO 8260:2008 BS ISO 8260:2008 ISO 8260:2008(E) IDF 130:2008(E) ISO and IDF 2008 All rights reserved v Foreword IDF (the International D

22、airy Federation) is a non-profit organization representing the dairy sector worldwide. IDF membership comprises National Committees 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 represe

23、nted on the IDF Standing Committees carrying out the technical work. IDF collaborates with ISO in the development of standard methods 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

24、Committees for voting. Publication as an International Standard requires approval by at least 50 % of the IDF National Committees casting 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 fo

25、r identifying any or all such patent rights. ISO 8260 IDF 130 was prepared by the International Dairy Federation (IDF) and Technical 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-

26、ISO Action Team on Organic contaminants of the Standing Committee on Analytical methods for additives and contaminants under the aegis of its project leader, Mr. R. de Knegt (NL). ISO 8260 IDF 130:2008 cancels and replaces IDF 130A:1991, which has been technically revised. BS ISO 8260:2008 BS ISO 82

27、60:2008 ISO 8260:2008(E) IDF 130:2008(E) vi ISO and IDF 2008 All rights reservedIntroduction This International Standard is intended for use in the research, monitoring and control of organochlorine compounds in milk and milk products by isolation of these compounds. In the past, polychlorinated bip

28、henyls (PCBs) were generally determined by “empirical” methods, most of which used “peak pattern comparison” employing gas-liquid chromatography with electron-capture detection (GLC-ECD) and packed columns. For reference compounds, mixtures produced by perchlorination to decachlorobiphenyl (and GLC-

29、ECD determination) or dechlorination to biphenyl were used. The determination was carried out by high-performance liquid chromatography with ultraviolet detection (HPLC-UV) or by gas- liquid chromatography with flame-ionization detection (GLC-FID). The aforementioned techniques have three important

30、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 isomers is lost. This information is, however, extremely useful for indicating the sources of contamination and for differentiating between backgrou

31、nd and recent contamination. 2) “PCB contents” determined by the methods mentioned above might be obtained in many different ways as, for most PCB data, what is meant by “PCB content” is not clearly defined. Most reported “PCB contents” cannot, therefore, be compared, and interpretation of the data

32、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) Chlorobiphenyls are individual chemical compounds which have different properties (e.g. biodegradability, toxicological effects, tendency to accumulate

33、). Therefore, it would be highly desirable to determine these compounds separately. As a broad concept, the analysis of PCBs needs to be applicable to milk and milk products in different countries throughout the world. To achieve this, the following basic considerations apply: a) the need to conside

34、r the different situations in different laboratories, for example the equipment available, the level of training of the laboratory personnel, the budget available and the special tasks of the laboratory; b) the need to define the purpose of the analysis, for example screening, monitoring and control

35、 with respect to legal limits, or research; c) the need to determine simultaneously the PCB and organochlorine pesticide (OCP) content; d) the need to include, as far as possible, information on the PCB isomer-distribution pattern; e) the need to define clearly the contents to be reported; f) the ne

36、ed to control carefully the separation of the PCBs from the OCPs in order to avoid interference. BS ISO 8260:2008 BS ISO 8260:2008 INTERNATIONAL STANDARD ISO 8260:2008(E) IDF 130:2008(E) ISO and IDF 2008 All rights reserved 1 Milk and milk products Determination of organochlorine pesticides and poly

37、chlorobiphenyls Method using capillary gas-liquid chromatography with electron-capture detection WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use

38、. 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 International Standard specifies a method for the determination of the contents of individual organochlorine pesticides (OCPs) an

39、d polychlorinated biphenyls (PCBs) in milk, evaporated milk, sweetened condensed milk, powdered milk products, butter and butterfat, cheese and other milk products. The method is capable of determining low levels of specific OCPs down to 5 g of OCP per kilogram of fat and levels of specific PCBs dow

40、n 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 documents are indispensable for the application of this document. For dated references, only the edition cited applies. For unda

41、ted references, the latest edition of the referenced document (including any amendments) applies. ISO 14156 IDF 172, Milk and milk products Extraction methods for lipids and liposoluble compounds 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.

42、1 OCP and PCB contents mass fractions of organochlorine pesticides and polychlorinated biphenyls as determined by the procedure specified in this International Standard. NOTE 1 For products containing more than 2 % fat, the organochlorine compound content is expressed in micrograms or milligrams per

43、 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 product. BS ISO 8260:2008 BS ISO 8260:2008 ISO 8260:2008(E) IDF 130:2008(E) 2 ISO and IDF 2008 All rights reserved4 Principle The fat

44、 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 Florisil SPE (solid-phase extraction) cartridges, respectively. The eluate is concentrated and dissolved in a s

45、uitable 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 and materials All reagents shall be of recognized analytical grade and be suitable for pesticide-residue ana

46、lysis. 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 highly volatile as well as toxic and/or highly inflammable. Observe current safety precautions for handling,

47、use and disposal. 5.1 Acetonitrile (CH 3 CN). 5.2 Methylene chloride (CH 2 Cl 2 ). 5.3 Petroleum ether, with a boiling point of 40 C to 60 C, distilled, if necessary, using a Raschig column of length at least 500 mm. 5.4 Diethyl ether (C 2 H 5 ) 2 O. 5.5 n-Hexane (C 6 H 14 ), distilled, if necessary

48、, using a Raschig column of length at least 500 mm, or, alternatively, iso-octane (C 8 H 18 ). 5.6 Sodium sulfate (Na 2 SO 4 ). 5.7 Sodium oxalate (Na 2 C 2 O 4 ). 5.8 Acetone (CH 3 COCH 3 ). 5.9 Methanol (CH 3 OH). 5.10 Dodecane (C 12 H 26 ). 5.11 Eluting solvents, as follows: 5.11.1 Acetonitrile/m

49、ethylene 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 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