分散固相萃取-气相色谱-质谱法分析蕨菜、黑米中53种农药残留量  

Determination of 53 pesticide residues in bracken and black kerneled rice using dispersive solid-phase extraction and gas chromatography-mass spectromery

作　　者：郝开拓[1,2] 孔祥虹 杜宝中[1] 何强 黄江锐[1,2] 张璐 

机构地区：[1]西安理工大学理学院,西安710054 [2]陕西出入境检验检疫局,西安710068

出　　处：《分析试验室》2011年第6期69-74,共6页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局科研项目(2009IK285);国家公益性行业科研项目(201010040)资助

摘　　要：采用分散固相萃取(Dispersive solid-phase extraction)样品前处理方法,建立了蕨菜、黑米等生态农产品中53种农药残留的气相色谱-质谱(GC-EI/MS)的分析方法。样品由含0.1%冰醋酸的乙腈提取,以环氧七氯为内标,经分散固相萃取法净化。每种农药选择了合适的离子及其驻留时间,采用气相色谱-质谱方法在选择离子监测模式下进行测定。53种农药标准在5～500μg/kg下均有良好的线性,在10,50,100μg/kg三种不同的添加水平下进行回收率实验。蕨菜、党参和黑米三种基质中所有残留农药的平均回收率在75.2%～119.8%,相对标准偏差低于14%,检出限在0.4～8.0μg/kg之间。该方法不仅能用于生态农产品中53种农药残留的检测,而且还能较好的解决蕨菜基质出现的干扰问题。An optimized analytical method using dispersive solid-phase extraction（Dispersive-SPE） and gas chromatography-mass spectrometery（GC-EI/MS） has been developed for the rapid determination of 53 pesticides in three eco-agricultural products in Southern Shaanxi.Prior to analysis,a sample preparation approach based on acetonitrile containing 0.1% acetic acid for extraction and dispersive-SPE method for cleanup was implemented and validated for pesticides.The extracts were determined by GC-EI/MS using heptachlor epoxide as internal standard,appropriate ions were set for each pesticide to eliminate the interference of co-extracted matrix components,and the dwell time of each ion was also optimized.All analytes displayed good linearies in the range of 5～200 μg/kg.The method was reliable and stable.The recoveries of all pesticides were in the range from 75.2% to 119.8% at spiked levels of 10,50 and 100 μg/kg into three eco-agricultural products（bracken,radix codonopsitis,black kerneled rice）,and the relative standard deviations were less than 14%.In this work,the method had obtained an enhanced limit of detection for the analytes in the range of 0.4～8.0 μg/kg.

关 键 词：分散固相萃取 气相色谱-质谱 生态农产品 农药残留 

分 类 号：O657.63[理学—分析化学]