1、BRITISH STANDARDBS EN ISO 15753:2006Animal and vegetable fats and oils Determination of polycyclic aromatic hydrocarbonsICS 67.200.10nullnull nullnullnullnullnullnullnull nullnullnullnullnullnullnull nullnullnull nullnullnullnullnullnullnullnullnullnull nullnullnullnullnullnull nullnull nullnullnull
2、nullnullnullnullnullnull nullnull nullnullnullnullnullnullnullnullnull nullnullnull+A1:2011Exclusion of olivepomace oil from the scopeCopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-
3、,-,-National forewordThis British Standard is the UK implementation of EN ISO 15753:2006+A1:2011. It is identical to ISO 15753:2006, incorporating amendment 1:2011. It supersedes BS EN ISO 15753:2006, which is withdrawn.The start and finish of text introduced or altered by amendment is indicated in
4、the text by tags. Tags indicating changes to ISO text carry the number of the ISO amendment. For example, text altered by ISO amendment 1 is indicated by !“.The UK participation in its preparation was entrusted to Technical Committee AW/307, Oil seeds, animal and vegetable fats and oils and their by
5、-products.A list of organizations represented on AW/307 can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity fro
6、m legal obligations.BS EN ISO 15753:2006+A1:2011This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2006 BSI 2011Amendments/corrigenda issued since publicationDate Comments 30 September 2011 Implementation of ISO amendment 1:2011 with
7、CEN endorsement A1:2011ISBN 978 0 580 71734 5Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 15753August 2011ICS 67.200.10En
8、glish VersionAnimal and vegetable fats and oils - Determination of polycyclicaromatic hydrocarbons - Exclusion of olive pomace oil from the scope (ISO 15753:2006)Corps gras dorigines animale et vgtale - Dterminationdes hydrocarbures aromatiques polycycliques (ISO15753:2006)Tierische und pflanzliche
9、Fette und le - Bestimmung vonpolycyclischen aromatischen Kohlenwasserstoffen (ISO15753:2006)This European Standard was approved by CEN on 19 August 2006.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the statu
10、s of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards 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
11、ion in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia,
12、 Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES K
13、OMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 15753:2006: E:2006+A1Copyright European Committee for Standardization Provided by IHS under license with
14、 CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Foreword This document (EN ISO 15753:2006) has been prepared by Technical Committee ISO/TC 34 “Agricultural food products“ in collaboration with Technical Committee CEN/TC 307 “Oilseeds,vegetable and animal fats a
15、nd oils and their by-products - Methods of sampling and analysis“, the secretariat of which is held by AFNO R.This European Standard shall be given the status of a national standard, either by publication ofan identical textor by endorsement, at the latestbyMarch 2007, and conflicting nationalstanda
16、rds shall bewithdrawn at the latest by March 2007. According to the CEN/CENELEC Internal Regulations, the national standards organizations ofthe following countries are bound to implement this European Standard: Austria, Belgium,Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Gre
17、ece, Hungary,Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and Unit ed Kingdom. Endorsement notice The text of ISO 15753:2006 has been approved by CEN as EN ISO 15753:2006 without anymodif
18、ications. Foreword to amendment A1 This document (EN ISO 15753:2006/A1:2011) has been prepared by Technical Committee ISO/TC 34 “Food products“ in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sampling and analysis”
19、 the secretariat of which is held by AFNOR. This Amendment to the European Standard EN ISO 15753:2006 shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by February 2012, and conflicting national standards shall be withdrawn
20、at the latest by February 2012. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the
21、 national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherl
22、ands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 15753:2006/Amd 1:2011 has been approved by CEN as a EN ISO 15753:2006/A1:2011 without any modification. BS EN ISO 15753:2006+A1:2011EN ISO 15753:2006+A1:
23、2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Reference numberISO 15753:2006(E)INTERNATIONAL STANDARDISO15753First edition2006-09-01Animal and vegetable fats and oils D
24、etermination of polycyclic aromatic hydrocarbons Corps gras dorigines animale et vgtale Dtermination deshydrocarbures aromatiques polycycliquesCopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license
25、from IHS-,-,-ii BS EN ISO 15753:2006+A1:2011EN ISO 15753:2006+A1:2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-iiiContents PageForeword iv1 Scope. 12 Normative referenc
26、es. 13 Terms and definitions. 14 Principle.25 Reagents and materials. 26 Apparatus 37 Sampling 48 Sample preparation 59 Procedure for determination of PAHs from fats and oils: General method . 59.1 Preliminaryremarks .59.2 Blank 59.3 Determination of recovery values (without matrix) . 59.4 Extractio
27、n (liquid/liquid extraction) 69.5 Purification on C18-bonded phase cartridge (solid/liquid extraction) 69.6 Purification on Florisil-bonded phase cartridge (solid/liquid extraction). 610 Procedure for determination of PAHs from fats and oils: Method specific for coconut oil . 710.1 First extraction
28、(liquid/liquid extraction) 710.2 Second extraction (liquid/liquid extraction). 810.3 Purification on C18-bonded phase cartridge (solid/liquid extraction) 810.4 Purification on Florisil-bonded phase cartridge (solid/liquid extraction). 811 High-performance liquid chromatography (HPLC) . 911.1 Operati
29、ng conditions 911.2 Detection parameters.1011.3 Analysis of samples and standards 1111.4 Confirmation of the presence of PAHs. 1212 Expression ofresults. 1213 Precision 1213.1 Interlaboratorytest. 1213.2 Repeatability 1313.3 Reproducibility 1314 Test report. 13Annex A (informative) Recovery values,
30、flow charts, chromatograms and injection sequences. 14Annex B (informative) Results of the interlaboratory test . 19Bibliography. 22BS EN ISO 15753:2006+A1:2011EN ISO 15753:2006+A1:2011 (E)Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reprodu
31、ction or networking permitted without license from IHS-,-,-iv 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 technical comm
32、ittees. Each member bodyinterested in a subject for which a technical committee has beenestablished 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 closel ywith the In
33、ternational 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 Standards. Draft International
34、Standardsadopted 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 of this document may be the su
35、bject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 15753 wasprepared by Technical Committee ISO/TC 34, Food products , Subcommittee SC 11, Animaland vegetable fats and oils. BS EN ISO 15753:2006+A1:2011EN ISO 15753:2006+A1:2011 (E)Copyright E
36、uropean Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-1Animal and vegetable fats and oils Determination ofpolycyclic aromatic hydrocarbons 1 Scope This International Standard describes two method
37、s for the determination of 15 polycyclic aromatic hydrocarbons (PAHs) in animal and vegetable fats and oils: a general method, and a method specific for coconut oil and vegetable oils with short-chain fattyacids.These methods are not quantitative for the very volatile compounds such as naphthalene,
38、acenaphthene and fluorene. Due to interferences provided by the matrix itself, palm oil and olive pomac e oil cannot be analysedusing this method. The quantification limit is 0,2 g/kg for almost all compounds analysed, except for fluoranthene and benzo(g , h , i )perylene where the quantification li
39、mit is 0,3 g/kg, and indeno(1,2,3-c , d )pyrene where the quantification limit is 1 g/kg. 2 NormativereferencesThe following referenced documents are indispensable for the application of this document. For datedreferences, only the edition cited applies. For undated references, the latest edition of
40、 the r eferenceddocument (including any amendments) applies.ISO 661, Animal and vegetable fats and oils Preparation of test sample3 Terms and definitions For the purposes of this document, the following terms and definitions apply.3.1 polycyclic aromatichydrocarbon PAHcompound that contains two or m
41、ore condensed (fused) aromatic hydrocarbon rings and the content of which can be determined according to the method specified in this International Standard NOTE 1 The content is given in micrograms per kilogram. NOTE 2In general PAHs are divided into light PAHs with two to four aromatic rings, and
42、heavy PAHs with five or morearomatic rings. EXAMPLES Light PAHs include: naphthalene (CAS RN 91-20-3), acenaphthene (CAS RN 83-32-9), acenaphthylene (CAS RN208-96-8), fluorene(CAS RN 86-73-7), anthracene (CAS RN 120-12-7), phenanthrene (CAS RN 85-01-8), fluoranthene (CAS RN 206-44-0), chrysene (CAS
43、RN 218-01-9), benz(a )anthracene (CAS RN 56-55-3), pyrene (CAS RN 129-00-0). NOTE The results for olive pomace oil in Annex B show that this method is not applicable to this type of oil. The precision data determined are very poor. !“BS EN ISO 15753:2006+A1:2011EN ISO 15753:2006+A1:2011 (E)Copyright
44、 European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-2 Heavy PAHs include:benzo(a )pyrene (CAS RN 50-32-8), benzo(b )fluoranthene (CAS RN 205-99-2), benzo(k )fluoranthene (CAS RN 207-08-9), be
45、nzo(g , h , i )perylene (CAS RN 191-24-2), dibenz( a , h )anthracene (CAS RN 53-70-3),indeno(1,2,3-c , d )pyrene (CAS RN 193-39-5). 4 Principle The polycyclic aromatic hydrocarbons ar e extracted with an acetonitrile/acetone mixture followed bypurification on C18 reversed-phase and then Florisil bon
46、ded-phase cartridges. Determination of the content of the individual polycyclic aromatic hydrocarbons after separation is achieved by means of high-pressure liquidchromatography (HPLC) and by measuring the fluorescence at various excitation and emission wavelengths. 5 Reagentsand materials WARNING A
47、ttention is drawn to the regulations governing the handling of dangerous matter.Technical, organizational and personal safety measures must be followed. Use only reagents of recognized analytical grade unless otherwise stated. Check the quality of solvents before use by concentrating the solvent abo
48、ut 1 000 times by evaporation and analysing the concentrate by HPLC (300 ml to 300 l). The chrom atogram shall be free from peaks in the elution area of PAHs. 5.1 Methanol, ultra resi-analysed grade1).5.2 Hexane , HPLC grade1).5.3 Acetonitrile, HPLC grade1). 5.4 Acetone , HPLC grade 1).5.5 Dichloromethane, HPLC grade1). 5.6 Toluene , HPLC grade1).5.7 Water, HPLC grade1).5.8 Tetrahydrofuran, HPLC grade1). 5.9 Solvent mixture 1 : acetonitrile/acetone (volume fraction 60 % / 40 %). Quantityused per sample: 41 ml for general method, 36 ml formethod specific for
