微型固相萃取柱结合胃袋式大体积进样-气相色谱-质谱法同时快速测定菠菜中的13种有机磷农药残留  

Rapid and Simultaneous Determination of Thirteen Organic Phosphorous Pesticide Residues in Spinach Using Gas Chromatography-Mass Spectrometry Coupled with Stomach Large Volume Injection and Mini Solid Phase Extraction

作　　者：李礼[1] 许秀丽[1] 丁罡斗[1] 李翔[1] 张垚[1] 孙毅之[1] 何裕建[2] 仲维科[1] 陈彦长[1] 王大宁[1] 

机构地区：[1]中国检验检疫科学研究院,北京100025 [2]中国科学院研究生院化学与化学工程学院(本部),北京100049

出　　处：《色谱》2007年第4期573-576,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金资助项目(No.20475051);国家质检总局课题(2006IK156)

摘　　要：利用微型固相萃取柱对样品进行前处理,采用胃袋式大体积进样技术结合气相色谱-质谱（GC-MS）,建立了菠菜中13种有机磷农药残留的同时快速分析方法。以保留时间和特征离子丰度比定性,以峰面积外标法定量,以3倍信噪比实验值确定方法的检出限（LODs）,以10倍信噪比实验值确定方法的定量限（LOQs）。结果表明,除乐果外,其余12种有机磷农药的添加回收率为76.8%-114.0%,相对标准偏差为1.5%-17.6%,LODs为0.5-25μg/kg。该方法前处理简单快速,分析成本低,分析时间短,灵敏度、准确度和精密度均符合农药多残留检测技术的要求,适用于食品中多种有机磷农药残留的快速灵敏检测。A stomach large volume injection-gas chromatography-mass spectrometry （LVI-GC- MS ） coupled with mini solid phase extraction （SPE） method for the rapid and simultaneous de-termination of 13 organic phosphorous pesticide residues in spinach samples is presented. The compounds were identified with their retention times and the abundance ratios of qualifier and target ions. Quantification was calculated based on the extraction of spiking standards in a blank sample. The limit of detection （ LOD ） was determined by the experimental value of the signal-to-noise ratio of 3： 1, and the limit of quantification （LOQ） was defined at the experimental value of the signal-to-noise ratio of 10：1. The recoveries obtained ranged from 76.8% to l l4.0% with the relative standard deviations between I. 5% and 17, 6% except dimethoate. The LODs ranged from 0.5 to 25 μg/kg. This simple, rapid and reliable method has wide applications for the simultaneous determination of multiple pesticide residues in spinach and possibly other species.

关 键 词：固相萃取 胃袋式大体积进样 气相色谱-质谱 有机磷农药 菠菜 

分 类 号：O658[理学—分析化学]