分散固相萃取-气相色谱-三重四极杆串联质谱法测定蒺藜中17种农药残留  

Determination of 17 kinds of pesticide residues in Tribulus terrestris L. by gas chromatography-triple quadrupole tandem mass spectrometry with offline disperse solid phase extraction

作　　者：李媛[1] 肖丽和[2] 殷果[2] 王珏[2] 谢耀轩[2] 李清[1] 王淑红[2] 王铁杰[1,2] 毕开顺[1] 

机构地区：[1]沈阳药科大学,沈阳110016 [2]深圳市药品检验所,深圳518057

出　　处：《药物分析杂志》2013年第4期661-668,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：广东省科技厅科技计划项目:2010A030100018

摘　　要：目的:建立分散固相萃取-气相色谱-三重四极杆串联质谱法(GC-QQQ-MS/MS)测定蒺藜中17种有机氯农药残留,并对36个不同产地的蒺藜药材进行农药残留测定。方法:蒺藜样品经乙腈提取,加入N-丙基乙二胺(PSA)、石墨化碳黑(GCB)进行分散固相萃取净化后,采用GC-QQQ-MS/MS技术在多反应监测(MRM)模式下测定,外标法定量。结果:17种农药成分在0.002～0.200 mg.L-1范围内有良好的线性关系,相关系数在0.9991～1.0000范围内;17种农药成分在3个添加水平下(100、250和500μg.kg-1),加标回收率范围为70.0%～105.1%,RSD%(n=3)为0.6%～9.5%;各农药成分的检出限均小于2.7μg.kg-1。结论:该方法可应用于蒺藜药材中多种农药残留的同时检测。Objective：To develop an analysis method based on gas chromatography-triple quadrupole tandem mass spectrometry（GC-QQQ-MS/MS）with offline disperse solid phase extraction for the determination of 17 kinds of pesticide residues in Tribulus terrestris L.,and to quantify the pesticide residues in 36 Tribulus terrestris L.samples.Methods：Tribulus terrestris L.samples were extracted with acetonitrile by the vortex extraction with acetonitrile,and the extract was further purified by dispersive solid phase extraction with sorbents of N-propyl ethylenediamine（PSA）and graphitized carbon black（GCB）.The prepared samples were then analyzed by GC-QQQ-MS/MS in MRM mode,and the external standard method was applied to quantify the pesticides.Results： All the 17 pesticides showed good linearity in the range of 0.002 to 0.200 mg·L^-1（r=0.9991-1.0000）,the average recoveries of all the pesticides were in the range of 70.0% to 105.1% at three spiked levels of 100,250 and 500 μg·kg-1,the RSD（n=3）were in the range of 0.6% to 9.5%;and the limits of detection（LOD）were all below 2.7 μg·kg-1.Conclusion： The method is suitable for the multiresidues analysis of pesticides in Tribulus terrestris L.

关 键 词：蒺藜 有机氯农药残留 分散固相萃取 气相色谱-三重四极杆串联质谱法 中药农残监测 多反应监测(MRM) 

分 类 号：R917[医药卫生—药物分析学]