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

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500 μg·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2.7 μg·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 exte rnal 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.