BS-684-2.47-1998 ISO-15302-1998.pdf
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1、BRITISH STANDARD BS 684-2.47: 1998 ISO 15302: 1998 Methods of analysis of fats and fatty oils Part 2: Other methods Section 2.47: Determination of benzoapyrene content by reverse-phase high-performance liquid chromatography ICS 67.200.10 Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 13:38:0
2、4 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 684-2.47:1998 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 August 1998 BSI 04-1999 ISBN 0 580 29
3、946 5 National foreword This British Standard reproduces verbatim ISO 15302:1998 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee AW/11, Animal and vegetable fats and oils, which has the responsibility to: aid enquirers to un
4、derstand 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 promulgate them in the UK. A list of organizations represented
5、on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Ind
6、ex”, 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. Compliance with a British Standard does not of itself c
7、onfer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the ISO title page, page ii, pages 1 to 4 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be
8、 indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 13:38:04 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 684-2.47:1998 BSI 04-1999i Contents Page National forewordInside front c
9、over Forewordii 1Scope1 2Normative reference1 3Principle1 4Reagents1 5Apparatus1 6Sampling2 7Preparation of test sample2 8Procedure2 9Expression of results3 10Precision3 11Test report3 Annex A (informative) Results of interlaboratory test4 Annex B (informative) Bibliography4 Table A.1 Statistical re
10、sults4 Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 13:38:04 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 13:38:04 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 13:38:04 GMT+00
11、:00 2006, Uncontrolled Copy, (c) BSI BS 684-2.47:1998 ii BSI 04-1999 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 normally carried out through ISO technic
12、al 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 collaborates closely wi
13、th the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. 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
14、the member bodies casting a vote. International Standard ISO 15302 was prepared by Technical Committee ISO/TC 34, Agricultural food products, Subcommittee SC 11, Animal and vegetable fats and oils. Annex A and Annex B of this International Standard are for information only. Descriptors: Agricultural
15、 products, food products, animal fats, vegetable fats, animal oils, vegetable oils, chemical analysis, determination of content, benzopyrene, high performance liquid chromatography. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 13:38:04 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 684-2.47
16、:1998 BSI 04-19991 1 Scope This International Standard specifies a method for the determination of benzoapyrene in crude or refined edible oils and fats by reverse-phase high-performance liquid chromatography (HPLC) using fluorimetric detection in the range from 0,1 4g/kg to 10 4g/kg. 2 Normative re
17、ference The following standard contains provisions, which through reference in this text, constitute provisions of this International Standard. At the time of publication the edition indicated was valid. All standards are subject to revision and parties to agreements based on this International Stan
18、dard are encouraged to investigate the possibility of applying the most recent edition of the standard indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 661:1989, Animal and vegetable fats and oils Preparation of test sample. 3 Principle Adsor
19、ption of a suitable amount of sample on an alumina column, followed by elution with light petroleum of any benzoapyrene present, and subsequent analysis of the eluate by HPLC using a fluorimetric detector. 4 Reagents All reagents shall be of recognized analytical grade. Where analytical grade solven
20、ts other than the recommended ones are used, a full blank analysis shall be carried out and the results of this blank analysis reported. 4.1 Water, double distilled, filtered through a membrane filter of 0,45 4m pore size; deionized water obtained by purifying demineralized water systems may also be
21、 used. 4.2 Light petroleum (boiling point range between 40 C and 60 C), or hexane, redistilled over potassium hydroxide pellets (4 g/l). 4.3 Acetonitrile, suitable for HPLC. 4.4 Tetrahydrofuran, suitable for HPLC. 4.5 Toluene, suitable for HPLC. 4.6 Sodium sulfate, granular, anhydrous. 4.7 Alumina,
22、activity grade 4, prepared from neutral aluminium oxide, activity grade super 1, deactivated by the addition of 10 ml distilled water to 90 g of alumina. CAUTION THE REACTION IS EXOTHERMIC AND PRESSURE MAY BUILD UP. Shake the container for about 15 min and allow the contents to equilibriate for 24 h
23、. Store the alumina in a closed vessel at ambient temperature. 4.8 Benzoapyrene, 99,0 % purity. CAUTION BENZOaPYRENE IS A KNOWN CARCINOGEN. CARRY OUT ALL WORK WITH IT IN A FUME HOOD, WEARING GLOVES TO MINIMIZE EXPOSURE. 4.9 Benzoapyrene solutions1) 4.9.1 Stock solution Weigh, to the nearest 0,1 mg,
24、about 12,5 mg of benzoapyrene in a 25 ml graduated flask. Dissolve it in toluene (4.5) and fill to the mark. This solution contains about 0,5 mg/ml benzoapyrene and should be stored in the dark at 4 C when it is stable for 6 months at least. 4.9.2 Standard solutions Prepare two standard solutions co
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