1、November 2016 English price group 14No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 67.200.10!%YS“2585448www.din.de
2、DIN EN ISO 15753Animal and vegetable fats and oils Determination of polycyclic aromatic hydrocarbons (ISO 15753:2016);English version EN ISO 15753:2016,English translation of DIN EN ISO 15753:2016-11Tierische und pflanzliche Fette und le Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen
3、 (ISO 15753:2016);Englische Fassung EN ISO 15753:2016,Englische bersetzung von DIN EN ISO 15753:2016-11Corps gras dorigines animale et vgtale Dtermination des hydrocarbures aromatiques polycycliques (ISO 15753:2016);Version anglaise EN ISO 15753:2016,Traduction anglaise de DIN EN ISO 15753:2016-11Su
4、persedesDIN EN ISO 15753:201111www.beuth.deDocument comprises 31 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.10.16 DIN EN ISO 15753:2016-11 2 A comma is used as the decimal marker. National foreword This document (EN ISO 15
5、753:2016) has been prepared by Technical Committee ISO/TC 34 “Food products” (Secretariat: AFNOR, France) in collaboration with Technical Committee CEN/TC 307 “Oil seeds, vegetable and animal fats and oils and their by-products Methods of sampling and analysis” (Secretariat: AFNOR, France). The resp
6、onsible German bodies involved in its preparation were DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products) and the Deutsche Gesellschaft fr Fettwissenschaft (German Fat Research Society), Joint Working Committee NA 057-05-05 AA G
7、emeinschaftsausschuss fr die Analytik von Fetten, len, Fettprodukten, verwandten Stoffen und Rohstoffen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 661 DIN EN ISO 661 ISO 835 DIN EN ISO 835 ISO 1042 DIN EN ISO 1042 ISO 4788 DIN EN
8、ISO 4788 ISO 5555 DIN EN ISO 5555 ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DIN EN ISO 15753:2011-11 as follows: a) milk and milk products (or fat coming from milk and milk products) are now excluded from the scope of the standard; b) the standard has
9、been editorially revised and brought in line with the current rules of presentation. Previous editions DIN EN ISO 15753: 2006-12, 2011-11 DIN EN ISO 15753:2016-11 3 National Annex NA (informative) Bibliography DIN EN ISO 661, Animal and vegetable fats and oils Preparation of test sample DIN EN ISO 8
10、35, Laboratory glassware Graduated pipettes DIN EN ISO 1042, Laboratory glassware One-mark volumetric flasks DIN EN ISO 4788, Laboratory glassware Graduated measuring cylinders DIN EN ISO 5555, Animal and vegetable fats and oils Sampling DIN ISO 5725-1, Accuracy (trueness and precision) of measureme
11、nt methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN EN ISO 15753:2016-11 4 This page
12、 is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15753 April 2016 ICS 67.200.10 Supersedes EN ISO 15753:2006English Version Animal and vegetable fats and oils - Determination of polycyclic aromatic hydrocarbons (ISO 15753:2016) Corps gras dorigines animale et vgtale -
13、 Dtermination des hydrocarbures aromatiques polycycliques (ISO 15753:2016) Tierische und pflanzliche Fette und le - Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen (ISO 15753:2016) This European Standard was approved by CEN on 11 March 2016. CEN members are bound to comply with the CE
14、N/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Ce
15、ntre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as t
16、he official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Nethe
17、rlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rig
18、hts of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15753:2016 EEuropean foreword .31 Scope . 52 Normative references 53 Terms and definitions . 54 Principle 65 Reagents and materials . 66 Apparatus . 77 Sampling 88 Sample preparation . 99 Pr
19、ocedure for determination of PAHs from fats and oils: General method 99.1 Preliminary remarks 99.2 Blank 99.3 Determination of recovery values (without matrix) 99.4 Extraction (liquid/liquid extraction) . 99.5 Purification on C18-bonded phase cartridge (solid/liquid extraction) 109.6 Purification on
20、 Florisil-bonded phase cartridge (solid/liquid extraction) 1110 Procedure for determination of PAHs from fats and oils: Method specific for coconut oil 1210.1 First extraction (liquid/liquid extraction) . 1210.2 Second extraction (liquid/liquid extraction) . 1210.3 Purification on C18-bonded phase c
21、artridge (solid/liquid extraction) 1210.4 Purification on Florisil-bonded phase cartridge (solid/liquid extraction) 1311 High-performance liquid chromatography (HPLC) .1411.1 Operating conditions 1411.2 Detection parameters . 1411.3 Analysis of samples and standards . 1611.4 Confirmation of the pres
22、ence of PAHs . 1612 Expression of results .1613 Precision 1713.1 Interlaboratory test 1713.2 Repeatability 1713.3 Reproducibility 1714 Test report 18Annex A (informative) Recovery values, flow charts, chromatograms and injection sequences .19Annex B (informative) Results of the interlaboratory test
23、.24Bibliography .27Contents PageDIN EN ISO 15753:2016 11 -EN ISO 15753:2016 (E)2Foreword 4European foreword This document (EN ISO 15753:2016) has been prepared by Technical Committee ISO/TC 34 “Food products” in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats a
24、nd oils and their by-products - Methods of sampling and analysis” the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by October 2016, and conflicting national
25、standards shall be withdrawn at the latest by October 2016. 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. This document supersedes E
26、N ISO 15753:2006. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Mace
27、donia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 15753:2016 has been approved by CE
28、N as EN ISO 15753:2016 without any modification. DIN EN ISO 15753:2016 11 -EN ISO 15753:2016 (E)3 ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally car
29、ried 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 the work.
30、 ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the differe
31、nt approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may b
32、e the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents)
33、.Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles i
34、n the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils.This second edition cancels and replaces the first edition (ISO 15753:200
35、6), of which it constitutes a minor revision. It also incorporates Amendment ISO 15753:2006/Amd.1:2011. A non-applicability statement for milk and milk products has been added to the Scope.DIN EN ISO 15753:2016 11 -EN ISO 15753:2016 (E)4 1 ScopeThis International Standard describes two methods for t
36、he determination of 15 polycyclic aromatic hydrocarbons (PAHs) in animal and vegetable fats and oils: a general method; a specific method for coconut oil and vegetable oils with short-chain fatty acids.These methods are not quantitative for the very volatile compounds such as naphthalene, acenaphthe
37、ne and fluorene. Due to interferences provided by the matrix itself, palm oil and olive pomace oil cannot be analysed using 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 limit is 0,3 g/kg
38、, and indeno(1,2,3-c,d)pyrene, where the quantification limit is 1,0 g/kg.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. Milk and milk products (or fat coming from milk and milk products) are
39、excluded from the scope of this International Standard.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest e
40、dition of the referenced document (including any amendments) applies.ISO 661, Animal and vegetable fats and oils Preparation of test sample3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1polycyclic aromatic hydrocarbonPAHcompound that contains t
41、wo or more condensed (fused) aromatic hydrocarbon rings and the content of which can be determined according to the method specified in this International StandardNote 1 to entry: The content is given in micrograms per kilogram.Note 2 to entry: In general, PAHs are divided into light PAHs with two t
42、o four aromatic rings, and heavy PAHs with five or more aromatic rings.EXAMPLE Light PAHs include:naphthalene (CAS RN 91-20-3), acenaphthene (CAS RN 83-32-9), acenaphthylene (CAS RN 208-96-8), fluorene (CAS RN 86-73-7), anthracene (CAS RN 120-12-7), phenanthrene (CAS RN 85-01-8), fluoranthene (CAS R
43、N 206-44-0), chrysene (CAS RN 218-01-9), benz(a)anthracene (CAS RN 56-55-3), pyrene (CAS RN 129-00-0).DIN EN ISO 15753:2016 11 -EN ISO 15753:2016 (E)5 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), benzo(g,h,i)peryl
44、ene (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 PrincipleThe polycyclic aromatic hydrocarbons are extracted with an acetonitrile/acetone mixture followed by purification on C18 reversed-phase and then Florisil bonded-phase cartridges. Determ
45、ination of the content of the individual polycyclic aromatic hydrocarbons after separation is achieved by means of high-pressure liquid chromatography (HPLC) and by measuring the fluorescence at various excitation and emission wavelengths.5 Reagents and materialsWARNING Attention is drawn to the reg
46、ulations governing the handling of dangerous matter. Technical, organizational and personal safety measures should be followed.Use only reagents of recognized analytical grade unless otherwise stated.Check the quality of solvents before use by concentrating the solvent about 1 000 times by evaporati
47、on and analysing the concentrate by HPLC (300 ml to 300 l). The chromatogram shall be free from peaks in the elution area of PAHs.5.1 Methanol, “ultra resi-analysed” grade.1)5.2 Hexane, HPLC grade.1)5.3 Acetonitrile, HPLC grade.1)5.4 Acetone, HPLC grade.1)5.5 Dichloromethane, HPLC grade.1)5.6 Toluen
48、e, HPLC grade.1)5.7 Water, HPLC grade.1)5.8 Tetrahydrofuran, HPLC grade.1)5.9 Solvent mixture 1: acetonitrile/acetone (volume fraction 60 %/40 %).Quantity used per sample: 41 ml for general method, 36 ml for specific method for coconut oil.5.10 Solvent mixture 2: acetonitrile/acetone (volume fraction 80 %/20 %).Quantity used per sample: 2 11 ml for method specific for coconut oil.5.11 Solvent mixture 3: hexane/dichloromethane (volume fraction 75 %/25 %).Quantity used per samp
