SN 0598-1996.Method for the determination of the multiple resi dues of or ganochlorine pesticides in aquatic products for export.
范围
SN 0598规定了出口水产品中的六六六(BHC)及异构体、六氯苯0HCB)、七氯、环氧七氯、艾氏剂狄氏剂、异狄氏剂、滴滴涕(DT)及异构体和类似物(DDD DDE)残留量检验的抽样、制样和气相色诸测定方法。
2曲样和制样
2.1检验批
以不超过10000箱为一检验批。同一检验批的商品应具有相同的特征，如包装、标记、产地、规格和等级等。
2.2抽样数量
批量，箱             最低抽样数，箱
150及以下                   3
151~3200                   8
3201~10000              13
23抽样方法
按2.2规定的抽样箱数随机抽职,逐件开启。每箱至少职500 g作为原始样品,原始样品总量不得少于2kg。装入盛样器内,加封后,标明标记、 及时送实验室。
2.4试样制备
将抽职的样品去鳞、去骨、去内脏后,将所有可食部分充分搅碎和混匀。用四分法缩分出1kg,均分为二份,分别装入洁净容器内,作为试样。密封,并标明标记。
2.5试样保存
将试样于-18℃以下冷袜保存。
注:在抽样和制样的操作过程中,必须防止样品受到污染或发生残留物含量的变化。

中华人民共和国进出口商品检验行业标准SN0598-1996
出口水产品中多种有机氯农药残留量检验方法
Method forthedeterminationofthe multiple residues of organochlorine pesticidesin aquatic products for export1996-11-15发布
1997-05-01实施
中华人民共和国国家进出口商品检验局发布SN0598-1996
本标准是根据GB/T,1.1一1993《标准化工作导则第1单元：标准的起草与表述规则第1部分：标准编写的基本规定》及SN/T0001一1995《出口商品中农药、鲁药残留量及生物毒素检验方法标准编写的基本规定》进行编写的。其中测定方法参照了“AOAC第15版983.21”中所载的有机氯农药残留量的检验方法，通过研究、改进和验证后制定的。本标准同时制定了抽样和制样方法。的。
测定低限是根据国际上对水产品中的多种有机氧农药残留最高限量和测定方法的灵敏度而制定本标准的附录A为提示的附录，
本标准由中华人民共和国国家进出口商品检验局提出并归口。本标准起草单位：中华人民共和国辽宁进出口商品检验局。本标准主要起草人：宋文斌、姜伟、王喆、曹际娟、刘生梅、孙海鸥。本标准系首次发布的行业标准。范围
中华人民共和国进出口商品检验行业标准出口水产品中多种有机氯农药残留量检验方法
Method forthedeterminationofthe multiple residues of organochlorine pesticidesinaquaticproductsforexport
SN0598-1996
本标准规定了出口水产品中的六六六(BHC)及异构休、六氟苯(HCB)、七氯、环氧七氯、艾氏剂、狄氏剂、异狄氏剂、滴滴涕（DDT)及异构体和类似物（DDD、DDE)残留量检验的抽样、制样和气相色谱测定方法。
本标准适用于出口鳕鱼中14种有机氯农药（α-BHC、β-BHC、Y-BHC、6-BHC、六氮苯、七氟、环氧七氯、艾氏剂、狄氏剂、异狄氏剂、0,p'-DDT、P,p\-DDT、P,p*-DDD、P,p\-DDE残留量的检验。2抽样和制样
2.1检验批
以不超过10000箱为一检验批。同一检验批的商品应具有相同的特征，如包装、标记、产地、规格和等级等。
2.2抽样数量
批量，箱
150及以下
.151~3200
3201~10000
2.3抽样方法
最低抽样数，箱
按2.2规定的抽样箱数随机抽取，逐件开启。每箱至少取500g作为原始样品，原始样品总量不得少于2kg。装入盛样器内，加封后，标明标记，及时送实验室。2.4试样制备
将抽取的样品去鳞、去骨、去内脏后，将所有可食部分充分搅碎和混匀。用四分法缩分出1kg，均分为二份，分别装入洁净容器内，作为试样。密封，并标明标记。2.5试样保存
将试样于一18℃以下冷冻保存。注；在抽样和制样的操作过程中，必须防止样品受到污染或发生残留物含量的变化。3测定方法
3.1方法提要
试样经与无水硫酸钠一起研磨干燥后，用丙酮-石油醛提取农药残留，提取液经氟罗里硅土柱净化，中华人民共和国国家进出口商品检验局1996-11-15批准1997-05-01实施
SN0598-1996
净化后样液用配有电子俘获检测器的气相色谱仪测定，外标法定量。3.2试剂和材料
所用试剂除注明外均为分析纯，水为蒸馏水。3.2.1丙酮：重蒸馏。
3.2.2石油醚：沸程60～90℃。经氧化铝(3.3.2)柱净化后用全玻璃蒸馏器蒸馏，收集60～90℃馏分。3.2.3乙醚：重蒸馏。
3.2.4乙醛-石油醚淋洗溶液：15十85。3.2.5无水硫酸钠：650℃灼烧4h，冷却后，储于密闭容器中。3.2.6氧化铝：层析用，中性，100～200目，800℃灼烧4h，冷却至室温储于密闭容器中备用。使用前，应在130℃干燥2h。
3.2.7氟罗里硅土：60100目，650℃C灼烧4h，冷却后储于密闭容器内备用。使用前于130℃烘1h。注：每批氟罗里硅土用前应做淋洗曲线。3.2.8有机氛农药标准品：α-BHC、β-BHC、Y-BHC、8-BHC、六氯苯、七氯、环氧七氟、艾氏剂、狄氏剂、异狄氏剂、O,P\-DDT、P,P\-DDT、P,p-DDD、P,P-DDE标准品，纯度均≥99%。3.2.914种有机氯农药标准溶液：准确称取适量的每种农药标准品，分别用少量苯溶解，然后用石油醚配成浓度各为0.100mg/mL的标准储备溶液。根据需要再以石油醚配制成适用浓度的混合标准工作溶液。
3.3仪器和设备
3.3.1气相色谐仪：配有电子俘获检测器。3.3.2氧化铝净化柱：300mm×20mm（内径）玻璃柱，装入氧化铝（3.2.6)40g，上端装入10g无水硫酸钠(3.2.5)干法装柱，流量为2mL/min。注：该柱可连续净化处理石油醛1000mL。3.3.3氟罗里硅土净化柱：200mm×20mm(内径)玻璃柱，装入氟罗里硅土（3.2.7)13g，上端装入5g无水硫酸钠（3.2.5)，干法装柱，使用前用40mL石油醚（3.2.2)淋洗。3.3.4索氏提取器：250mL。
3.3.5绞肉机。
3.3.6全玻璃重蒸馏装置。
3.3.7玻璃研钵：口径11.5cm。
3.3.8旋转蒸发器或氮气流浓缩装置：配有250mL蒸发瓶。3.3.9微量注射器：10μL。
3.3.10脱脂棉：经过丙酮-石油醚(2+8)混合液抽提6h处理过。3.4.测定步骤
3.4.1提取
称取试样10.0g(精确至0.1g)于研钵中，加15g无水硫酸钠(3.2.5)研磨几分钟，将试样制成干松粉末。装入滤纸简内。放入索氏提取器中。在提取器的瓶中加入100mL丙酮-石油醛（2十8)混合液，在水浴上提取6h（回流速度每小时10~12次）。将提取液减压或氮气流浓缩至约5mL。3.4.2净化
将提取液（3.4.1)全部移入氟罗里硅土净化柱（3.3.3)中。弃去流出液。注入200mL乙醚-石油醚淋洗液（3.2.4)进行洗脱。开始时，取部分乙醚-石油醚混合液反复清洗提取瓶，并把洗液注入净化柱中。洗脱流速为23mL/min，收集流出液于250mL蒸发瓶中。在减压或氮气流中浓缩并定容至10mL，供气相色谱测定。Www.bzxZ.net
3.4.3测定
3.4.3.1色谱条件
SN0598-1996
a）色谱柱：SGE毛细管柱(或等效的色谱柱)，25mX0.53mm(内径），膜厚：0.15μm。固定相：HT5(非极性)键合相；
b）载气：氮气（纯度≥99.99%），10mL/min；c）助气：氮气（纯度≥99.99%），40mL/min：d）柱温：程序升溢如下：
5C/min
100℃-
-140℃
10C/min
+200℃
e）进样口温度：200℃；
f）检测器温度：300℃；
g）进样方式：柱头进样方式。
3.4.3.2色谱测定
15℃/min
+230℃
根据样液中有机氧农药种类和含量情况，选定峰高相近的相应标准工作混合液。标准工作混合液和样液中各有机氯农药响应值均应在仪器检测线性范围内。对标准工作混合液和样液等体积参插进样测定。在上述色谱条件下，各有机氯农药出峰顺序和保留时间如下。14种有机氰农药标准品的色谱图见附，录A中图AI。
农药名称
α-BHC
艾氏剂
环氧七氯
狄氏剂
P,p'-DDE
异狄氏剂
O,p'-DDT
P,p-DDD
P,P'-DDT
3.4.4空白试验
除不加试样外，均按上述测定步骤进行。3.4.5结果计算和表述
保留时间，min
用色谱数据处理机或按式(1)计算试样中各有机氯农药残留量：X,
式中：X,—试样中各有机氯农药残留量，mg/kg；一样液中各有机氯农药的峰高，mm；h
ha标准工作溶液中各有机氯农药的峰高，mm；标准工作溶液中各有机氯农药的浓度，g/mL；一最终样液的体积，mL；
-称取试样量，g。
注：计算结果需扣除空白值。
·（1）
方法的测定低限、回收率
4.1测定低限
本方法的测定低限分别为
农药名称
α-BHC
β-BHC
艾氏剂
环氧七氟
狄氏剂
P,p*-DDE
异狄氏剂
O,p-DDT
P,p'-DDD
P,p'-DDT
4.2回收率
回收率的实验数据：
农药名称
α-BHC
β-BHC
艾氏剂
0598-1996
测定低限，mg/kg
添加浓度，mg/kg
回收率，%
环氧七氯
狄氏剂
P,p-DDE
异狄氏剂
o,p\-DDT
P,p-DDD
P,p'-DDT
0598-1996
SN0598-1996
附录A
(提示的附录）
标准品色谱图
图A114种有机氯农药标准品色谱图图中，10.557min为e-BHC
10.767min为HCB
11. 758 min为Y-BHC
12.106 min为β-BHC
12. 904 min为0-BHC
13.087min为七氧
13.975min为艾氏剂
15.042min为环氢七氧
16.280min为致氏熟
16. 440 min 为 P+p’-DDE
16.756min为异致氏剂
17.128min为o.p*-DDT
17.449min为p.p*-DDD
17.918min为p.p-DDT
SN0598-1996
Foreword
This stardard was drafted in accordance with the requirements of GB/T 1.11993Directives forthe work of standardization-Unit l:Drafting and presentation of standards-Part I:General rules fordrafting standards\ and SN/T 0001-95 \General rules for drafting the standard methods for the de-termination of pesticide,veterinary drug residues and biotoxins in commodities for export\.Themethod of determination was established by referring to the official method of AOAC,983.21 15thediton,through research,modification and verification.In addition,methods of sampling and samplepreparation are also specified in this standard.The limits of determination are defined in this standard on the bases of the current internationalmaximum limits relevant to organochlorine pesticide residues in aguatic produets and the sensitivity ofthe method.
AnnexAinthisstandardisaninformativeannex.This standard was proposed by and is under the charge of the State Administration of Import andExportCommodityInspectionof thePeople'sRepublicofChina.This standard was drafted by Liaoning Import and Export Commodity Inspection Bureau of thePeople'sRepublicof China.
The main drafters of this' standard are Song Wenbin,Jiang Wei,Wang Zhe,Cao Jijuan,Liu Shengmei,SunHaiou.
This standard is a professional standard promulgated for thefirst time.NoteThis English versionga translation from the Chinese text,is solelyfor guidance.ProfessionalstandardofthePeople'sRepublicofChinafor Import and Export Commodity InspectionMethod for the determination ofthemultipleresidues of organochlorinepesticidesin aquatic products for export1Scope
SN0598—1996
This standard specifies the methods of sampling,sample preparation and determination by gaschromatography of benzenehexachloride(BHC)and its isomers,hexachlorobenzene(HCB),hep-tachlor,heptachlor epoxide,aldrin,dieldrin,endrin and dichlorodiphenyltrichloroethane (DDT) and itsisomers and analogs [dichlorodiphenyldichloroethane(DDD),dichlorodiphenyldichloroethylene(DDE)]residues in aquatic product for export.This standard is applicable to the determination of residues of 14 organochlorine pesticides (a-BHC,β-BHC,Y-BHC,-BHC,HCB,heptachlor,heptachlor epoxide,aldrin,dieldrin,endrin,o,p'-DDT,P,p'-DDT,P,p'-DDD,P,p\-DDE)in codfor export.2Samplingandsamplepreparation2.1 Inspection lot
Each inspection lot should not excced 10 000 packagee.The characteristics of the cargo within the same inspection lot,such as packing,mark,origin,specification,grade etc. ,should be the same.2.2Quantity of sample taken
Thenumberofpackages
in each inspection lot
≤150
151—3200
3201—10000
Minimum number of
packages to be taken
2.3Samplingprocedure
A number of packages specified in 2.2 are taken at random and opened one by one. The sampleweight taken as primary sample from each package should be at least 500 g.The total weight of all pri-mary samples should not beless than 2kg,which shall be placed in a sample container,sealed,labeledand sent to laboratory in time.2.4Preparationof test sampleApproved by the State Administration ofImportandExportCommodityInspection ofthe People's Republic of China on Nov.15,19968
ImplementedfromMay1,1997
SN0598—1996
The combined primary sample is scaled and deboned. The edible portions are blended and reducedby quartering to 1 kg.Then divide into two equal portions,each portion is placed in a clean containeras test sample,which is then sealed and labeled.2.5 Storage of the test sampleThe test sample should be stored below-18C.note;In the course of sampling and sample preparation,precaution must be taken to avoid contamination or anyfac-tors which may cause the change of residue content.3Methodof determination
3.1Prinaciple
The test sample,after grinding and blending with anhydrous sodium sulphate,is transfered into aSoxhlet extractor and the pesticide residues are extracted with acetone-petroleum ether. The extract iscleaned up by passing through florisil column. Determine the residues by gas chromatograph with elec-tron capture detector,using external standard method.3.2Reagents and materials
Unless otherwise specified,the reagents used should be analytically pure,\water\ is distilled wa-ter.
3.2.1Acetone;Restilled.
3.2.2 Petroleum ether:Distillation range 60--90C.After cleaned up by passing through aluminacolumn,the reagent is redistilled in all-glass apparatus,and the distillate of 60-90 C is collected.3.2.3Ether.Redistilled.
3.2.4Ether+petroleum'ether rinsesolntion;(15+85)3.2.5Anhydrous sodium sulphate:Ignite at 650C for 4 h,and keep in a tightly closed container af-tercooling
3.2.6Alumina:Chromatographic grade,neutral,100—200mesh.Ignite at 650C for 4h,and keep ina tightly closed container after cooling.Heat at 130C for 2h before using.3.2.7Florisil:60—100 mesh,ignite at 650C for 4 h,and keep in a tightly closed container after cool-ing.Beforeusing,dry at13oCfor1h.note: For each lot of florisil,elution curve should be tested before use3.2.8Organochlorine pesticide standards: a-BHC,β-BHC,Y-BHC, -BHC,HCB, heptachlor,hep-tachlor epoxidealdrin,dieldrin,endrin,p,p'-DDT,o,p'-DDT,p,p'-DDD,p,p'-DDE standards,puri-ty of all≥99%.
3.2.9Standard solutions of'14 organochlorine pesticides:Accurately weigh appropriate amount ofeach pesticide standard,dissolve in a small volume of benzene,then dilute with petroleum ether sepa-rately to prepare the standard stock solutions of o.100 mg/mL in concentration. According to the re-quirementprepare the mixed standard working solutions of appropriate concentrations.3.3Apparatusandequipment
3.3.1 Gas chromatograph,equipped with the electron capture detector (ECD).3.3.2Aluminacolumnforcleanup:Glasscolumn,30cmX2cm(id).Thecolumn isfilledwith 40gofalumina(3.2.6),and topped with 10g of anhydrous sodium sulphate.Theflow rateofpetroleum etherthrough the column is 2 mL/min.Note: This column is used for cleaning up petroleum ether of 1,ooo mL in cepacity.3.3.3Florisil column for cleanup:Glass column,20 cmX2 cm(id).The column is flled with 13g9
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