固相萃取-毛细管气相色谱法测定人参制品中19种有机氯农药的残留量  

Determination of Organochlorine Pesticide Residues in Preserved Ginseng by Solid-Phase Extraction and Capillary Gas Chromatography

作　　者：陈丹[1] 初丽伟[1] 侯志广[1] 尚梅[2] 范志先[2] 李月茹[1] 

机构地区：[1]吉林农业大学测试中心,长春130118 [2]青岛科技大学化工学院

出　　处：《应用化学》2007年第2期210-214,共5页Chinese Journal of Applied Chemistry

基　　金：农业部标准资助项目(02098)

摘　　要：建立了人参制品保鲜参、人参蜜片及人参茶中有机氯(六六六4个异构体,滴滴涕5个异构体,四氯苯胺、六氯苯、七氯、五氯苯胺、五氯硝基苯、百菌清、环氧七氯、艾氏剂、狄氏剂和异狄氏剂共19种)农药残留量的固相萃取毛细管气相色谱(SPE-CGC)分析方法。以石油醚-丙酮混合溶液作提取剂,采用索氏提取法提取样品。然后用SPE C_(18)固相萃取小柱快速净化提取物。采用OV-1701弹性石英毛细管(25 m×0．25 mm×0．5μm)气相色谱柱分离样品,^(63)Ni电子捕获检测器检测,高纯N_2气为载气。进样口温度为300℃,检测器温度为300℃。不分流进样,程序升温,结果19种农药的峰面积与其质量浓度均有良好的线性关系,相关系数均大于0．992。最小检测量为1．5×10^(-13)～2．5×10^(-12)异,样品的加标平均回收率为73．7％～96．6％。The solid-phase extraction and capillary gas chromatography （SPE-CGC） was introduced for the determination of 19 kinds of organochlorine pesticide residues including 4 isomers of hexachlorocyclohexane （BHC） （α-BHC, β-BHC, γ-BHC, δ-BHC）; 5 isomers of 4,4＇-dichl-orodiphenylthrichloroethane, （DDT） （pp＇-DDE, pp＇-DDD, op＇-DDT, op＇-DDE and pp＇-DDT） ; tetra, penta-chloroaniline; heXachlorobenzene; heptaehlor; quintozene; ehlor-othalonil; heptachlor epoxide; aldrin; dieldrin and endlrin in preserved ginseng, ginseng honey plate and ginseng tea. The organochlorine pesticides were extracted form the samples with the solvents of the mixture of petrolic-aether acetone, followed by the purification with SPECIO solid- phase extraction column. Then the extract was separated by using gas chromatography and OV-1701 flexible quartz capillary（25 m ×0. 25 mm ×0. 5 μm） chromatographic column. Sample was detected by 63Ni electron capture detector（ECD） with N2（99. 99% ） as the carrier gas. The temperatures of the injector and detector were both at 300 ℃ and increased automatically. The good linearity were obtained for the 19 kinds of organichlorine pesticides with the average relative coefficient larger than 0. 992. The minim detectable sample wasl. 5 × 10 ^-13 -2. 5 × 10^ -12 g, and the average recoveries range was from 73.7% to 96. 6%.

关 键 词：毛细管气相色谱法 有机氯农药 固相萃取 人参制品 

分 类 号：O657.7[理学—分析化学]