《BS-ISO-3890-1-2000.pdf》由会员分享，可在线阅读，更多相关《BS-ISO-3890-1-2000.pdf（26页珍藏版）》请在三一文库上搜索。
1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 3890-1:2000 ICS 67
2、.100.01 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Milk and milk products Determination of residues of organochlorine compounds (pesticides) Part 1: General considerations and extraction methods Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 03:35:50 GMT+00:00 200
3、6, Uncontrolled Copy, (c) BSI This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 September 2000 BSI 09-2000 ISBN 0 580 36176 4 BS ISO 3890-1:2
4、000 Amendments issued since publication Amd. No.DateComments National foreword This British Standard reproduces verbatim ISO 3890-1:2000 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee AW/5, Chemical analysis of milk and mil
5、k products, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and
6、 promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Standards Catalogue under the section
7、entitled International Standards Correspondence Index, or by using the Find facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Complia
8、nce with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to v, a blank page, pages 1 to 16, an inside back cover and a back cover. The BSI copyright notice displa
9、yed throughout this document indicates when the document was last issued. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 03:35:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 3890-1:2000(E) INTERNATIONAL STANDARD ISO 3890-1 First edition 2000-07-01 Milk and milk products D
10、etermination of residues of organochlorine compounds (pesticides) Part 1: General considerations and extraction methods Lait et produits laitiers Dtermination des rsidus de composs organochlors (pesticides) Partie 1: Considrations gnrales et mthodes dextraction Licensed Copy: sheffieldun sheffieldun
11、, na, Mon Nov 27 03:35:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 3890-1:2000(E) ii Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 03:35:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 3890-1:2000(E) iii Contents Page Forewordv 1 Scope 1 2 Normative references2 3 Term and definition
12、 .2 4 Principle2 4.1 Extraction .2 4.2 Clean-up2 4.3 Determination.2 4.4 Confirmation.2 5 Requirements for reagents and materials.3 5.1 General3 5.2 Check for purity of reagents.3 6 Requirements for apparatus.4 6.1 General4 6.2 Gas-liquid chromatography apparatus .5 7 Sampling.6 8 Preparation of tes
13、t sample6 8.1 Milk6 8.2 Evaporated milk.6 8.3 Sweetened condensed milk6 8.4 Powdered milk products.6 8.5 Butter and butterfat .6 8.6 Cheese 6 8.7 Other milk products.7 9 Procedure.7 9.1 General7 9.2 Extraction .7 9.3 Clean up7 10 Preliminary tests7 11 Quantitative determination.8 12 Confirmatory tes
14、ts.8 13 Evaluation of results .8 13.1 Calculation of results 8 13.2 Presentation and expression of results 8 14 Precision.9 14.1 Evaluation of precision .9 14.2 Repeatability.9 14.3 Reproducibility.9 14.4 Limit of determination.10 15 Test report10 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov
15、27 03:35:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 3890-1:2000(E) iv Annex A (normative) Extraction of fat and organochlorine compounds and determination of fat content11 Annex B (informative) Analysis in the presence of polychlorinated biphenyl (PCBs).15 Bibliography16 Licensed Copy: sheffi
16、eldun sheffieldun, na, Mon Nov 27 03:35:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 3890-1:2000(E) v Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is no
17、rmally 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. International organizations, governmental and non-governmental, in liaison with ISO, also take part in
18、 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 rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the tech
19、nical 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 of this part of ISO 3890 may be the subject of patent righ
20、ts. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 3890-1 was prepared by Technical Committee ISO/TC 34, Agricultural food products, Subcommittee SC 5, Milk and milk products, in collaboration with the International Dairy Federation (IDF)
21、and AOAC International, and will also be published by these organizations. ISO 3890 consists of the following parts, under the general title Milk and milk products Determination of residues of organochlorine compounds (pesticides): Part 1: General considerations and extraction methods Part 2: Test m
22、ethods for crude extract purification and confirmation Annex A forms a normative part of this part of ISO 3890. Annex B is for information only. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 03:35:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon
23、Nov 27 03:35:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD ISO 3890-1:2000(E) 1 Milk and milk products Determination of residues of organochlorine compounds (pesticides) Part 1: General considerations and extraction methods WARNING The use of this part of ISO 3890 may involve
24、hazardous materials, operations and equipment. This standard does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this standard to establish safety and health practices and determine the applicability of regulatory limitations prior to
25、use. 1 Scope This part of ISO 3890 describes general considerations and extraction methods for the determination of residues of organochlorine pesticides in milk and milk products. Annex A specifies a method for high-fat products. Guidance is given on the conduct of analyses in the presence of polyc
26、hlorinated biphenyls (PCBs) in annex B. The applicability of the various methods is given in Table 1. Table 1 Application of methods to various compounds Method ? ? ? ?-HCH -HCH ? ? ? ?-HCH Aldrin/ dieldrin Heptachlor Heptachlor- epoxide DDT DDE TDE isomers Chlordane Oxy- chlordane Endrin Delta- ket
27、o- endrin HCB A+ B+ C+ + D+ + E+ + F+ G+ H+ + Key: + applicable not applicable Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 03:35:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 3890-1:2000(E) 2 2 Normative references The following normative documents contain provisions which, through re
28、ference in this text, constitute provisions of this part of ISO 3890. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISO 3890 are encouraged to investigate the possibility of applying the m
29、ost recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 3890-2, Milk and milk products Determination of residues
30、 of organochlorine compounds (pesticides) Part 2: Crude extract purification and confirmation test methods. ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions. ISO 5725-2:1994, Accuracy (trueness and precision) of measurem
31、ent methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method. 3 Term and definition For the purposes of this part of ISO 3890, the following term and definition applies. 3.1 contents of organochlorine compounds mass fraction
32、 of substances determined using the procedures specified in this part of ISO 3890 NOTE It is expressed in milligrams per kilogram, either on a fat basis or on a product basis (for low fat products). 4Principle NOTE The methods are based on a four-stage process; two stages may sometimes be combined,
33、in whole or in part. 4.1 Extraction Residues from the sample substrate are extracted by appropriate solvents, so as to obtain the maximum efficiency of extraction of the residues and minimum co-extraction of any substances which may give rise to interference in the determination. 4.2 Clean-up Interf
34、ering materials are removed from the extract to obtain a solution of the extracted residue in a solvent which is suitable for quantitative examination by the selected method of determination. 4.3 Determination The content of organochlorine compounds is determined by gas-liquid chromatography with el
35、ectron-capture detection. 4.4 Confirmation The identity of the observed pesticide residues is confirmed, particularly in those cases where it would appear that the maximum permitted level has been exceeded. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 03:35:50 GMT+00:00 2006, Uncontrolled
36、Copy, (c) BSI ISO 3890-1:2000(E) 3 Interference of PCBs and pesticides is a well-know problem in packed columns and to a lesser extent in with capillary columns. In the case of relatively high levels of PCBs, it is recommended to determine PCBs according to IDF 130A 14. 5 Requirements for reagents a
37、nd materials 5.1 General Use only reagents of recognized analytical grade, unless otherwise specified, and distilled or demineralized water or water of equivalent purity. Redistil water and solvents used and check their purity (see 5.2). The limit of the impurity of each of the used reagents shall n
38、ot exceed the limit of determination defined in 14.4. The total impurity of all reagents used in the method, however, may exceed that limit. Purify and periodically activate adsorbents according to the requirements of the different analytical methods. Check their purity (see 5.2.5). Every precaution
39、 shall be taken to avoid possible contamination of water, solvents, adsorbents, etc. by plastic or rubber materials. Store all purified reagents, adsorbents etc. in glass bottles with glass stoppers or with PTFE wads in the caps. Do not leave them exposed to the atmosphere after purification. Aceton
40、e-washed aluminium foil provides suitable protection in many situations. 5.2 Check for purity of reagents 5.2.1 Solvents Concentrate solvents by the factor involved in the method to be used. Test for purity by GLC (see 6.2). The chromatogram shall not show any interfering impurity whose concentratio
41、n exceeds the limit of determination defined in 14.4. Extract or concentrate acetonitrile, dimethylformamide (DMF) and methylene chloride in the same volumes as used in the method and examine the resulting solution by gas chromatography. 5.2.2 Water Extract 10 parts (by volume) of water with 1 part
42、(by volume) of n-hexane or light petroleum. Separate the organic phase. Concentrate by the factor involved in the method used and test for purity by GLC (see 6.2). The chromatogram shall not show any interfering impurity whose concentration exceeds the limits of determination defined in 14.4. 5.2.3
43、Inorganic salts Extract inorganic salts (e.g. sodium chloride), after purification according to the requirements of the different analytical methods, and any aqueous solutions used with n-hexane or light petroleum. Concentrate the extract by the factor involved in the method used and test by GLC. Th
44、e chromatogram shall not show any interfering impurity whose concentration exceeds the limit of determination defined in 14.4. 5.2.4 Cotton wool, glass wool and quartz wool Extract these with n-hexane and acetone using a Soxhlet extractor, until they are sufficiently free from interfering substances
45、. 5.2.5 Adsorbents Elute an amount of adsorbent equal to that used in the analytical method with the corresponding type and volume of solvent mixture. Concentrate the eluate as indicated in the analytical method and test for purity by GLC (see 6.2). The chromatogram shall not show any interfering im
46、purity whose concentration exceeds the limit of determination defined in 14.4. Check the activity of adsorbents regularly. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 03:35:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 3890-1:2000(E) 4 5.2.6 Standard solutions Use materials of at leas
47、t 95 % purity to prepare standard solutions for pesticide residue analysis. If stored at 20 ?C, they are generally stable for at least 1 or 2 years. Stock solutions of concentration 1 mg/ml, kept in a refrigerator at about 4 ?C, are usually stable for 2 to 3 months. Prepare diluted solutions freshly
48、 each day. NOTE Changes in volume by solvent evaporation, for example through the pores between a glass stopper and the neck of a flask, might be a source of error. Store standard solutions in glass bottles in a refrigerator and take every precaution to avoid possible contamination by plastic or rub
49、ber materials. Do not expose standard solutions to sunlight or ultraviolet light for extended periods. Mass spectrometry and gas-liquid chromatography may be used to examine analytical standards for impurities. Experience has shown that faults introduced in the preparation, handling and storage of standards and standard solutions are a major source of error. 6 Requirements for apparatus 6.1 General Thoroughly clean all glassware used for residue analysis. Hot chromic/sul