柱头进样结合气相色谱质谱分析动物源食品中热不稳定性氨基甲酸酯类农药  

On-column Injection Coupled with Gas Chromatography/Mass Spectrometry for Determination of Thermoliable Carbamates Pesticides in Animal Derived Sample

作　　者：胡艳云[1] 徐业平[1] 姚剑[1] 韩芳[1] 郑平[1] 盛旋[1] 

机构地区：[1]安徽出入境检验检疫局,合肥230022

出　　处：《分析化学》2011年第3期330-334,共5页Chinese Journal of Analytical Chemistry

基　　金：国家质检总局科研项目(No.2007IK156);安徽省自然科学基金项目(No.090415210)资助

摘　　要：对柱头进样结合气相色谱-质谱法(GC/MS)应用于复杂基体中热不稳定性氨基甲酸酯农药检测的可行性及可靠性进行了探讨。在常规不分流进样和柱头进样模式下,对13种氨基甲酸酯类农药的热不稳定性进行了比较。以猪肉、鸡蛋、牛奶为研究基体,采用乙腈提取,凝胶渗透色谱结合中性氧化铝固相萃取柱净化,柱头进样-GC/MS检测。研究表明:在不同添加水平下,平均回收率为81%～90%;相对标准偏差为2.8%～6.0%;定量检测下限均为0.01 mg/kg。对柱头进样的长期稳定性进行了研究,在80次连续进样内可获得正常的色谱性能。The feasibility and reliability of using on-column injection-gas chromatography/mass spectrometry（GC/MS） for the determination of thermo-liable carbamates pesticides in complex matrices has been investigated.The thermal instability of 13 carbamates pesticides was evaluated with conventional splitless injector and on-column injector.According to the properties of pig,egg and milk samples studied,the present method was involved in extraction with acetonitrile and cleanup with Gel permeation chromatography（GPC） and N-alumina SPE followed by on-column injection-GC/MS determination.The average recovery was in the range of 81%-90% with RSD in the range of 2.8%-6.0% at different spiked levels.The LOQs for pesticides were 0.01 mg/kg.The long-term stability by using on-column injection was studied and normal chromatographic performance could be obtained within 80 analyses

关 键 词：柱头进样 气相色谱-质谱 热不稳定 氨基甲酸酯类农药 

分 类 号：TS207.53[轻工技术与工程—食品科学]