1、5日串中华人民共和国出入境检验检疫行业标准SN/T 1950-2007 进出口茶叶中多种有机磷农药残留量的检测方法气相色谱法Determination of organphosphorus pesticides multiresidues in tea for import and export-Gas chromatography 2007-08-06发布2008-曰-01实施在重重坏培v垂直司z槌HZ酣幽阳，可当7中y华人民共和国发布罔家质量监督检验检夜总局前言本标准的附录A为资料性附录。本标准出国家认证认可监督管理委员会提出并归口。本标准起草单位:巾华人民共和国湖南出入境检验检疫局。本标
2、x1主要起草人z张莹、颜鸿飞、孙非、黄志强、王美玲、李拥军。本标准系首次发布的出入境检检疫行业标准。SN/T 1950一20071 范围进出口茶叶中多种有机磷农药残留量的检测方法气相色谱法SN/T 1950-2007 本标准规定了茶叶中敌敌畏、甲胶磷、乙眈甲胶磷、甲拌磷、氧乐果、乙拌陈、异稻瘟净、乐泉、皮蝇磷、毒死蝇、杀奴硫磷、对硫磷、7240C(lmin), c) 进样口温度，250C;dl 检测器温度，250C，e) 我气:氮气，纯度大于等于99.99%. m: Gt 5.0 m1 fl 氢气，75mL/min , g) 空气，100mL/min; h) F6吹气，20mL/min; 。进
3、样方式无分流进样，1.0 进样量，2L。色谱测定抑14.0min、杀螺硫磷14.8min、对硫磷15.5min.水胶硫磷16.1 min、杀扑磷17.3min、乙硫磷19.6 min.三瞠磷21.3 min.芬硫磷22.3 min、末硫磷23.1 m川、亚胶硫磷23.5 min.伏杀硫磷24.6 min、毗陪磷25.5min , 标准品的色谱分离因参见附录A中阁A.l，6.4 空白试验除不加试样外，按上述测定步骤进行。7 结果计算和表述用色i汗数据处理机或投式(1)计算试样中有机磷残留量.f-1):结果需扣除空白值。2 ( 1 ) SNjT 1950-2007 式中zX 样品中有机磷含量，单位
4、为毫克每千克(mg/kg), A一样液中有机磷的峰回积1As一-一标准工作溶液中有机磷的峰面积;c 标准工作溶液中有机磷的浓度，单位为做克每毫升(lg/mL), V一一样l!i最终定容你积，单位为毫升(mL)，m 称取的试样质量，单位为克(g)。B 方法的测定低限、回收率本方法的测定低限和1回收率数据见表10测定低限和回收率数据农药名称添加范罔/C可Ikg)回收率范t可fYc测定低限/Cmg/kg)敌敌畏O. 02 .a 也7声84.01050.02 甲胶磷O. 020. 2 ./ 79.5122，7/ 0.02 乙I!:t甲胶磷0.020.2 /卢l79).118 0.02 甲拌磷20扩/J
5、J dST庐094.00.02 氧乐果O. 02 , I , ., .:;0. 1 0.02 乙拌磷0.02 69.8101 0.02 异稻瘟净O. 01 幅L.82. Q土气J.8卢, 0.01 乐果O. 020. 2 / 何h0.02 皮蝇磷O. 020. /凡川17_，0.02 毒死蝉0.02-1- 2 f 7L9lCI 0日2JA鲤硫磷0.02 10.2 7旷主斗1.l0.02 对硫磷0.02 :_C.2 f 0.02 水胶硫磷0.01 卡0.1jsu12 0.01 杀扑磷0.02 -e.2、.f 77. 7rfS 0.02 乙硫磷0.0匈2/842 119 / 0.02 三Il磷。f
6、 78.4 俨1D2J/0.02 芬硫磷O. 01O. 1 ._.，且78. 525 0.01 苯硫磷O. 01 O. 1 74. 898. 6 0.01 亚胶硫磷0.02-0.2 77.2-115 0.02 伏杀硫磷O. 020. 2 85.0-119 。.02口吐畸磷0.01-0.1 83. 5119 0.02 3 SN/T 1950-2007 4 900 。800 700 600 500 400 300 200 100 。l 敌敌畏$2 甲胶磷53 乙酌甲胶磷34 甲拌磷g5 氧乐果$6 乙拌磷g7 异韬瘟净$8 乐果g9 皮蝇磷s10-毒死牌g11-杀蟆硫磷$12 对硫磷，13 水胶硫
7、磷$14一杀扑磷g15一一乙硫磷，16 三略磷;17一芬硫磷$18 苯硫磷z19 亚胶硫陇320一伏杀硫磷$21 毗晴磷.附录A资料性附录)21种有机磷农药的标准气相色i昔图2 5 10 15 20 25 mm 图A.1 21种有机磷农药标准品的气中目色i普图-SN/T 1950-2007 Foreword Annex A 01 this standard is an inlormative annex. This standard was proposed by and is under the charge 01 the Certilication and Accreditation Ad
8、min istration 01 the Peoples Republic 01 China This standard was dralted by Hunan Entry-Exit Inspection and Quarantine Bureau 01 the Peoples Re public 01 China The main drafters 01 this standard are Zhang Ying Yan Honglei Huang Zhiqiang Wang Meiling Li Yongjun This standard is a prolessional standar
9、d lor entry-ex!t inspection and quarantine promulgated lor the lirst time Note; This English vers旧atranslation from the Chnese text is soleJy for guidance. P J a SN/T 195-2007 Determination of organophosphorus pesticide multi-residues in tea for import and export-Gas chromatograph 1 Scope This stand
10、ard specifies the method for the determination of dichlorvos. methodophos acephate phorate omethoate disulfoton IBP dimelhoate fenchlorphos chlorpyrifos fe41itrothion parathion isocar bophosl methidathion ethion triazoph吟fensthionoateEPN phosm叫pho$lonepyrazophos residues by gas chromatography in tea
11、 for impo凹nnrt.-c.;-3 Reagents and materials 。rdeionized water 3. 1 Ethyl acetat: Redistilled. 3.2 Hexane: Redistilled. 3.3 Acetone:Redistilled. 3.4 Anhydrous sodium sulfate: Ignite at 650t for 4 h. 3.5 Organophosphorus pesticide standard: Purity二，98%.3. 6 Organophosphorus pesticide standard solutio
12、n: Accurately weigh proper amount of organophos phorus pesticide standard. to prepare a solution of 100 19 mL in acetone as the standard stock solu tion Accordin9 to the requirement prepare a standard working solution of appropriate concentration 6 SN/T 1950-2007 in ethyl acetate. 3.7 Envl-Carb colu
13、mn 3 mLsupelco or equivalent). 4 Apparatus and equipment 4. 1 Gas chromatograph equipped with a flame ph口tometricdetector FPD with a specific filter for phosphorus at 526 nm 4.2 Vortex mixer. 4.3 4.4 4.5 4.6 Test-tube, 10 mL. 4.7 Glass capillary-tip pipettes. The test samples of tea should be stored
14、 below OC -4(; In the course of sampling and sample prep arat旧n.precaution must be taken to avoid contamir旧tionor any factors which may cause the change 。fresidue content 6 Test Procedure 6. 1 Extraction Weigh O. 5 9 of the test sample accurate to O. 001 9 in 10 mL centrifuge tube. Marinate the test
15、 sam-7 SN/T 1950-2007 ple in 1 mL of water for 10 min Add enough anhydrous sodium sulfate. and vortex for 2 min. Extract with 2 x 2 ml ethyl acetate by vortex for 2 min. and centrifuge for 3 min. Add 2 mL ethyl acetate hexane (1 + 1) to the pellet vortex and repeat steps above combining supernatants
16、 6.2 Cleanup Add anhydrous sodium sulfate on the Envl-Carb SPE column to the height of 1 cm Condition the col umn with 4 mL ethyl acetate. Load the extract solution (6.1) on the column Elute with 4 mL ethyl acetate and 2 mL ethyl acetate-hexane (1 + 1 ). Evaporate the eluate to O. 50 mL under nitrog
17、en stream at 40t The solution is ready for GC analysis 6.3 Determination 6.3. 1 GC operating conditions a) Column: EQUITY-1701.fused silica臼pillarycolumn 3D m x O. 53 mm(i d x 1. 0 I,m. or equiva lent, 10t/min ._- ,. 5t/min b) Column temperature: 100t (1 min)一一160t(1 min)-=一一一:2400C(8 min) , c) Inje
18、ction port temperature: 250t , d) Detector temperature: 250t , e) Carrier gas: Nitrogen. purity二，99.99%.5.0 mL/min, f) Hydrogen: 75 mL/min, gl Oxygen 100 mL/min, hl Make-up gas:20 mL/min, il Injection mode: Splitless, j) Injection volume:2L 6.3.2 GC determination According to the approximate concent
19、ration of organophosphorus pesticide in the test sample solu. tion select the standard working solution with similar peak area to that of sample solution The re sponses of multiple organophosphorus pesticides in the standard working solution and sample solu tion should be within the linear range of
20、the instrumental detection The standard working solution B SN/T 1950-2007 should be injected randomly in between the injections of sample solution of equal volume Under the above GC opening conditions, chromatogram of organophosphorus pesticide standards are shown in Figre A. 1 in Annex A 6.3.3 Blan
21、k test The operation of the blank test is the same as that described in the method of determination but with omission of sample addition. 7 Calculation and expression of result The calculation of organophosphorus pesticide content in the sample is carried out by GC data pro cessor or according to th
22、e formula (1) , The blank value should be subtracted from the result of calcu lation A.c.V x=一一一一一(1 ) As.m where X-the residue content of multiple organophosphorus in the test sample , mg/kg , A -the peak area of multiple organophosphorus in the sample solution, As-the peak area of multiple organop
23、hosphorus in the standard working solution, c-the concentration of multiple organophosphorus in the standard working solution，g/mL， V-the final volume of sa门、口lesolution mL, m-the corresponding mass of test sample in the final sample solution,g. 8 limit of determination and recovery The limit of det
24、ermination of this method and its corresponding recoveries of fortifying concentra tions show on table 1 Table l-Li mit of determination and recovery Pesticides Spiked level/(mg/kg) Recove叩1%lOD!(mg!kg) dichlorvos 0.02-0.2 84.0-105 0.02 methodophos 0.02-0.2 79.5-122 0.02 acephate 0.02-0.2 79.0-118 0
25、.02 phora飞e0.02-0.2 70.0-94.0 0.02 omethoate 0.02-0.2 73.5-96.1 。口2disulfoton 0.02-0.2 69.8-101 0.02 IBP 0.01-口182.0-128 0.01 dimethoate 0.02-0.2 88.9-113 0.02 fenchlorphos 0.02-0.2 76.4-117 0.02 9 8:1/1 1950-2007 Table 1 (continue) Pesticides Spiked level!(mg/kg) Recoverv/% LOD/(mg!kgJ chlorpyrfos
26、0.02-0.2 71.9-104 0.02 fenitrothion 0.02-0.2 76.6-111 0.02 parathion 。口2-0.279.7-110 0.02 socarbophosl 0.01-0.1 86.3-125 0.01 methidathion 0.02-0.2 77.7-115 0.02 ethion 0.02-0.2 84.2-119 0.02 triazophos 0.02-0.2 78.4-109 。.02fensthionoate 0.01 ，-，-EPN 74日-9丘6。.01phosmet 0.02-0.2，阜n2-115 O. 02 phosa!
27、one 口M泣气一85.0-1;町0.02 pyrazophos 。01-0.83.r:.119 0.02 / 10 1飞i800 700 600 500 400 300 200 100 。l-Dichlorvos; 2-methodophos; 3 - Acephate; 4-Phorate; 5-0methoate; 6-Disulfoton; 7-IBP; B口imethoate;9-Fenchlorphos; 10-Chlorpyrifos; 11一-Fenitrothion; 12-Parathion; 13一Isocarbophosl;14 -Methidathion; 15-Et
28、hion; 16一Triazophos;7-Fensthionoate; 18-EPN; 19-Phosmet; 20-Phosalone; 21-Pyrazophos 手5 Annex A (1 nformative) Chromatogram of the standards 10 15 20 SN/T 1950-2007 25 mm Figure A. 1-Chromatogram of mixed solution of organophosphorus pesticide standards 中华人民共和国出入境检验检疫行业标准进出口茶叶中多种有机磷农药残留量的检测方法气相色谱法SNjT 1950-2007 3峰中国标准出版社出版北京复兴门外三里河北街16号邮政编码100045阿址电话，6852394668517548 中国标准出版社秦皇岛印刷厂印刷峰开本880X12301/16 印张1字数24干字2007年11月第一版2007年11月第一次印刷印数1-2000晤书号:155066.2-18232 定价10.00元
