微波萃取气相色谱法测定淀粉中14种有机氯农药残留  

Simultaneous Determination of 14 Organochlorine Pesticides in Starch by MAE/GC Method

作　　者：张本山[1] 于淑娟[1] 曾新安[1] 梁勇[2] 

机构地区：[1]华南理工大学轻工与食品学院,广东广州510641 [2]华南师范大学化学与环境学院,广东广州510006

出　　处：《分析测试学报》2011年第3期344-348,共5页Journal of Instrumental Analysis

基　　金：国家科技支撑计划资助项目(2006BAD27B04);广东省科技计划资助项目(2008A08040300;2008A08040301)

摘　　要：建立了淀粉中14种有机氯农药：六六六及滴滴涕的4种异构体、五氯硝基苯、四氯硝基苯、四氯苯胺、五氯苯胺、腐霉利、甲基五氯苯基硫醚（MPCPS）的微波辅助和气相色谱分析方法。优化了气相色谱检测条件，考察了提取方法、萃取条件、净化条件对提取效果的影响。目标农药在20，200μg／kg范围内线性良好，平均回收率在68％～108％范围内，检出限为0．1-0．3μg／kg，定量下限为0．5～0．8μg／kg。该方法操作简单、快速，灵敏度高，可用于淀粉中有机氯农药残留的快速检测。A microwave-assisted extraction and gas chromatographic （MAE/GC）method was established for the simultaneous determination of 14 organochlorine pesticides, including the four isomers of DDT and BHC, pentachloronitrobenzene （ PCNB ）, tetrachloronitrobenzene, tetrachloroaniline, pentachloroaniline, procymidone and methyl-5-chlorophenyl sulfide（MPCPS） in starch. The samples were extracted with n-hexane -dichloromethane mixed solvent（ 1 ： 2, by volume）. The extract was purified with a Florisil column using n-hexane -diehloromethane （1 ： 5, by volume） as elution sol- vent. Experimental conditions were optimized, and three different extraction methods of ultrasonic extraction, microwave assisted extraction and soxhlet extraction were compared. Extraction conditions were studied by the orthogonal test. Under the optimal conditions, the calibration curves showed good linearities in the range of 20 - 200 μg/kg for 14 organochlorine pesticides. The recoveries of 14 organochlorine pesticides at spiked levels were in the range of 68% - 108% . The detection limits ranged from 0. 1 μg/kg to 0. 3 μg/kg and the quantitation limits ranged 0. 8 μg/kg. The method was easy to operate, rapid, accurate and sensitive, from 0. 5 μg/kg to and was suitable for the determination of organochlorine pesticides residues in starch sample.

关 键 词：微波萃取 气相色谱 淀粉 有机氯 农残 

分 类 号：O657.71[理学—分析化学] F767.2[理学—化学]