自制固相微萃取探头用于分析大白菜中有机磷农药  

Analysis of Organophosphorus Pesticides in Celery Cabbage Samples by Using Self-Made Solid-Phase Microextraction Fiber

作　　者：王一龙[1] 曾昭睿[1] 杨敏[1] 董春洲[1] 

机构地区：[1]武汉大学化学与分子科学学院

出　　处：《武汉大学学报（理学版）》2006年第2期137-141,共5页Journal of Wuhan University:Natural Science Edition

基　　金：湖北省科技攻关计划资助项目(2003AA207B06);武汉理工大学校基金资助项目(XJJ2002062)

摘　　要：采用溶胶-凝胶方法制备的聚甲基苯基乙烯基硅氧烷／羟基硅油（PMPVS／OH-TSO）固相微革取探头与气相色谱（GC）联用对大白菜样品中的有机磷农药（敌敌鼹、二嗪农、甲摹对硫磷、马拉硫磷和乙基对硫磷）进行了分析，同时优化了固相微革取的实验条件．该探头较商用探头萃取能力更强，方法的检出限低（1．01～2．56ng／g），重现性好（3．5％～9．9％），线性范围宽（2个数量级），对市售的大白菜样品进行了标准加入回收实验，5种有机磷农药的同收率分别为80．2％，90．3％，85．4％，81．9％和91.8％，A home-made sol-gel-derived poly （methylphenylvinylsiloxane） （PMPVS） / hydroxy-terminated silicone oil （OH TSO） solid phase microextraction fiber coupled to gas chromatography （GC）/nitro gen-phosphorus detection （NPD） was firstly developed to determine organophosphorus pesticides （OPPs： dichlorvos, diazinon, methyl parathion, malathion and ethyl parathion） in celery cabbage samples. The following parameters effecting on the headspace solid-phase microextraction （HS-SPME） extraction efficiency were optimized. The detection limits of the method varied from 1.01 to 2.56 ng/g, and the relative standard deviations （n=5） for these pesticides were found to be from 3.5% to 9.9%. The linearity range was two orders of magnitude. Compared with commercial SPME stationary phases, this fiber shows better selectivity and sensitivity towards these pesticides. For celery cabbage samples trom market, the recoveries of five OPPs were 80.2%, 90.3%, 85.4%, 81.9% and 91.8% , respectively.

关 键 词：溶胶-凝胶技术 聚甲基苯基乙烯基硅氧烷/羟基硅油 同相微萃取 大白菜样品 有机磷农药 

分 类 号：O657.7[理学—分析化学]