1、June 2009DEUTSCHE NORM English price group 12No part of this standard 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 65.120!$X5t“1531881www.di
2、n.deDDIN EN 15742Animal feeding stuffs Determination of OC-pesticides and PCBs by GC/ECDEnglish version of DIN EN 15742:2009-06Futtermittel Bestimmung der OC-Pestizide und PCBs mittels GC/ECD-VerfahrenEnglische Fassung DIN EN 15742:2009-06www.beuth.deDocument comprises 25 pagesDIN EN 15742:2009-06 2
3、 National foreword This standard has been prepared by Technical Committee CEN/TC 327 “Animal feeding stuffs Methods of sampling and analysis” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte
4、 (Food and Agricultural Products Standards Committee), Technical Committee NA 057-03-03 AA Futtermittel. The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 6497 DIN EN ISO 6497 National Annex NA (informative) Bibliography DIN EN ISO 6497, Ani
5、mal feeding stuffs Sampling EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15742February 2009ICS 65.120English VersionAnimal feeding stuffs - Determination of OC-pesticides andPCBs by GC/ECDAliments des animaux - Dtermination des pesticidesorganochlors (OC) et des polychlorobiphnyles (PCB) parGC/
6、ECDFuttermittel - Bestimmung der OC-Pestizide und PCBsmittels GC/ECD-VerfahrenThis European Standard was approved by CEN on 24 January 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a nation
7、al standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any
8、other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia
9、, 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
10、KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15742:2009: EEN 15742:2009 (E) 2 Contents Page Foreword . 3 1 Scope 4 2 Normative references 4 3 Terms and de
11、finitions . 4 4 Principle 5 5 Reagents and materials 5 6 Apparatus . 12 7 Sampling . 13 8 Preparation of test sample . 13 9 Procedure . 13 10 Calculation and expression of results. 15 11 Precision . 18 12 Test report 21 13 Important considerations . 21 Annex A (informative) Results of interlaborator
12、y tests . 22 Bibliography 23 DIN EN 15742:2009-06 EN 15742:2009 (E) 3 Foreword This document (EN 15742:2009) has been prepared by Technical Committee CEN/TC 327 “Animal feeding stuffs”, the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard,
13、either by publication of an identical text or by endorsement, at the latest by August 2009, and conflicting national standards shall be withdrawn at the latest by August 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN an
14、d/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and supports essential requirements of EC Directive(s). According to the CEN/CENE
15、LEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxemb
16、ourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15742:2009-06 EN 15742:2009 (E) 4 1 Scope This European Standard specifies a gas chromatographic method with electron capture detection (ECD) for the determinati
17、on of organochlorine pesticides (OCs) and polychlorinated biphenyls (PCBs) in animal feeding stuffs. The method is applicable to animal feeding stuffs with a water content up to about 20 wt% and oil/fatty samples containing residues of one or more of the following OCs, PCBs, toxaphene and some of th
18、eir isomers and degradation products: Aldrin; Dieldrin; Chlorocamphene (Toxaphene); Chlordane (= sum of Chlordane isomers and Oxychlordane); DDT (= sum of isomers op-DDT, pp-DDT, pp-TDE (pp-DDD), and pp-DDE); Endosulfan (sum of -/-isomers and Endosulfan-sulphate); Endrin; Heptachlor (= sum of Heptac
19、hlor and -Heptachlorepoxide); Hexachlorobenzene (HCB); Hexachlorocyclohexane isomers -HCH (-BHC), -HCH (-BHC), -HCH (-BHC or lindane); PCB 28, 52, 101, 138, 153 and 180 (“Indicator PCBs”) and PCB 198, 209. The limit of quantification for the mentioned organochlorine pesticides and PCBs is 5 ng/g in
20、general. However, 10 ng/g applies for Heptachlor, Aldrin, Endrin, Dieldrin, and Endosulfan (-, - and sulphate). Individual laboratories are responsible to ensure that the equipment they used will achieve these limits of quantifications. 2 Normative references The following referenced documents are i
21、ndispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 6498, Animal feeding stuffs Preparation of test samples 3 Terms and definitions For t
22、he purpose of this document, the following terms and definitions apply. 3.1 limit of detection smallest measured content, from which it is possible to deduce the presence of the analyte with reasonable statistical certainty DIN EN 15742:2009-06 EN 15742:2009 (E) 5 NOTE The limit of detection is nume
23、rically equal to three times the standard deviation of the mean of blank determinations (n10). 3.2 limit of quantification lowest content of the analyte which can be measured with reasonable statistical certainty NOTE If both accuracy and precision are constant over a concentration range around the
24、limit of detection, then the limit of quantification is numerically equal to 6 times the standard deviation of the mean of blank determinations (n10). 3.3 feed additives substances are feed additives when they comply with the definition of feed additives given in the Regulation 1831/2003 4 Principle
25、 A test portion of animal feeding stuff is fortified with internal standard (PCB 198), and is extracted with ethylacetate. The extract is concentrated and subsequently purified by: Gel permeation chromatography (GPC), with cyclohexane/ethylacetate as eluting solvent chromatography on partially deact
26、ivated silica gel. The collected fraction containing the compounds of interest is concentrated and re-dissolved in a solution containing another internal standard (PCB 209) as a reference standard. After cleanup the analytes are measured using GC-ECD. Indentification is done on the basis of comparin
27、g retention times on capillary columns of different polarity. Quantification is done using the internal standard method. 5 Reagents and materials Use only reagents of recognized analytical grade and with a purity suitable for OC and PCB residue analysis. Check the purity of the reagents by performin
28、g a blank test under the same conditions as used in the method. The chromatogram should not show any interfering impurity at the retention time of compounds of interest. WARNING The use of this European Standard can involve hazardous materials, operations and equipment. This standard does not purpor
29、t to address all the safety problems associated with its use. It is the responsibility of the user of this European Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 5.1 Cyclohexane 5.2 Ethylacetate 5.3 Hexane 5.4 Di
30、chloromethane 5.5 Iso-octane 5.6 Toluene DIN EN 15742:2009-06 EN 15742:2009 (E) 6 5.7 Hexane/toluene = 3+7, parts by volume Mix 30 ml of hexan (5.3) with 70 ml of toluene (5.6) thoroughly. Store at room temperature in a tightly closed glass bottle. 5.8 Sodium Sulphate, anhydrous Heated at 160C durin
31、g at least 24 h. 5.9 Ethylacetate/Cyclohexane = 1+1, parts by volume Mix 500 ml of ethylacetate (5.2) with 500 ml of cyclohexane (5.1) thoroughly. Store at room temperature in a tightly closed glass bottle. 5.10 Silica gel, deactivated with 3,5% water Heat silica gel 60 (63m to 200m = 70 mesh to 230
32、 mesh), at 130C for at least 5 h, allow to cool in a desiccator, and store in a tightly stopped container in the desiccator. To 96,5 g dried silica gel in a 300 ml Erlenmeyer flask with a ground joint, add 3,5 ml water dropwise from a burette, with continuous swirling. Immediately stopper the flask
33、with a ground stopper and shake vigorously for 5 min until all lumps have disappeared. Next shake for 2 h on a mechanical shaker, and then store in a tightly stoppered container. Deactivated silica gel is tenable during approximately 2 weeks if carefully stored. 5.11 Internal standard (PCB 198) 5.12
34、 Internal Standard (PCB 209) 5.13 OC-pesticide reference standards Each with a purity not less than 99%. Aldrin (1R,4S,4aS,5S,8R,8aR)-1,2,3,4,10,10-hexachloro-1,4,4a,5,8,8a-hexahydro-1,4:5,8-dimethanonaphthalene) CAS Number: 309-00-2 Dieldrin (1R,4S,4aS,5R,6R,7S,8S,8aR)-1,2,3,4,10,10-hexachloro-1,4,
35、4a,5,6,7,8,8a-octahydro-6,7epoxy-1,4:5,8-dimethanonaphthalene) CAS Number: 60-57-1 Chlordane (1,2,4,5,6,7,8,8-octachloro-2,3,3a,4,7,7a-hexahydro-4,7-ethano-1H-indene); and isomer CAS Numbers: 5103-71-9 and 5103-74-2 Oxychlordane (4,7-Methanoindan, 1,2,4,5,6,7,8,8-octachloro-2,3-epoxy-3a,4,7,7a-tetra
36、hydro-, exo,endo-) CAS Number: 27304-13-8 op-DDT o,p-(1,1,1-trichloro-2,2-bis(4-chlorophenyl)ethane) CAS Number: 789-02-6 DIN EN 15742:2009-06 EN 15742:2009 (E) 7 pp-DDT p,p-(1,1,1-trichloro-2,2-bis(4-chlorophenyl) ethane) CAS Number: 50-29-3 pp-TDE (p,p-DDD) p,p-1,1-dichloro-2,2-bis(4-chlorophenyl)
37、 ethane CAS Number: 72-54-8 pp-DDE p,p-(1,1-dichloro-2,2-bis(4-chlorophenyl) ethylene) CAS Number: 72-55-9 Endosulfan (6,7,8,9,10,10-hexachloro-1,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin 3-oxide) two stereoisomers, , (I), CAS Number: 959-98-8 and , (II), CAS Number: 33213-65-9. Endo
38、sulfan-sulphate; CAS Number: 1031-07-8 Endrin (1R,4S,4aS,5S,6S,7R,8R,8aR)-1,2,3,4,10,10-hexachloro-1,4,4a,5,6,7,8,8a-octahydro-6,7-epoxy-1,4:5,8-dimethanonaphthalene CAS Number: 72-20-8 Heptachlor (1,4,5,6,7,8,8-heptachloro-3a,4,7,7a-tetrahydro-4,7-methanoindene) CAS Number: 76-44-8 -Heptachlorepoxi
39、de (1,4,5,6,7,8,8-heptachloro-3a,4,7,7a-tetrahydro-4,7-methanoindene(exo) CAS Number: 1024-57-3 HCB (hexachlorobenzene) CAS Number: 118-74-1 -HCH (-BHC) (-1,2,3,4,5,6-hexachlorocyclohexane) CAS Number: 319-84-6 -HCH (-BHC) (-1,2,3,4,5,6-hexachlorocyclohexane) CAS Number: 319-85-7 -HCH (-BHC; lindane
40、) (1,2,3,4,5,6-hexachlorocyclohexane) CAS Number: 58-89-9 Or a Certified Mixture at a concentration of 10 g/ml. 5.14 PCBs reference standards Each with a purity not less than 99%. PCB 28 (2,4,4 trichlorobiphenyl) ; CAS Number: 7012-37-5 PCB 52 (2,2,5,5 tetrachlorobiphenyl) ; CAS Number: 35693-99-3 D
41、IN EN 15742:2009-06 EN 15742:2009 (E) 8 PCB 101 (2,2,4,5,5 pentachlorobiphenyl) ; CAS Number: 37680-73-2 PCB 138 (2,2,3,4,4,5 hexachlorobiphenyl) ; CAS Number: 35065-28-2 PCB 153 (2,2,4,4,5,5 hexachlorobiphenyl) ; CAS Number: 35065-27-1 PCB 180 (2,2,3,4,4,5,5 heptachlorobiphenyl) ; CAS Number: 35065
42、-29-3 Or a Certified Mixture at a concentration of 10 g/ml. 5.15 Chlorocamphene (Toxaphene) Technical mixture. 5.16 Stock solutions, 100 g/ml Weigh 5 -10 mg ( 0,01 mg) of each compound (5.11, 5.12, 5.13, 5.14 and 5.15) in seperate brown medicine glass bottles of 100 ml and add iso-octane (5.5) to ac
43、hieve a concentration of 100 g/ml. Store the solutions in a refrigerator at 4C ( 3C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. Dissolve -HCH in 10 ml toluene (5.6), to achieve complete solvability and dilute further with iso-octane
44、(5.5) to achieve a concentration of 100 g/ml. 5.17 Mixed stock solutions 5.17.1 Mixed stock solution OC (without Endosulfan and Toxaphene) Pipet of each OC-stock solution (5.16) the indicated volume (Table 1) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. The achie
45、ved concentration is given in Table 1. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4C ( 3C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. 5.17.2 Mixed stock solution Endosulfan Pi
46、pet of each Endosulfan-stock solution (5.16) the indicated volume (Table 1) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. The achieved concentration is given in Table 1. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigera
47、tor at 4C ( 3C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. DIN EN 15742:2009-06 EN 15742:2009 (E) 9 Table 1 Concentration of OCs in Mixed stock solution (5.17) and mixed standard solution (5.18) Compound Pipet volume (ml) Mixed stock
48、 solution (5.17 1 Aisis the area internal standard PCB 198; Arsis the area of PCB 209; Qisis the amount of internal standard PCB 198 ng/ml; Qrsis the amount of PCB 209 ng/ml; Qxis the amount of component of interest ng/ml. Consequently the averaged relative response factor is calculated: (n)RRFx1=RR
49、F i=i(n)524(3) where n is the component of interest; DIN EN 15742:2009-06 EN 15742:2009 (E) 17 i is the calibration level (2 thru 5). Consequently the averaged relative response factor is calculated for internal standard (PCB 198): (m)RRFx1=RRF i=i(m)524(4) where m is the internal standard (PCB 198); i is the calibration level (2 thru 5); Calculation concentration component of interest The concentration component of interest is calculated by: R
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