分散固相萃取-气相色谱质谱联用法测定穿山龙中23种农药残留

 目的 本实验建立了穿山龙中有机氯，有机磷，拟除虫菊酯类等23种农药残留的（QuEChERS提取及其气相色谱质谱分析法。方法 样品经乙腈提取并浓缩后加入N-丙基乙二胺(PSA、石墨化碳黑(GCB进行分散固相萃取净化,气相色谱-电子轰击离子源质谱分时段选择离子监测技术测定与确证,外标法定量。结果 在5、20和50 μg·kg^-13个添加水平下所有农药的平均回收率在 80.2%～118.5%，RSD在1.6%～8.5%，可以满足农药残留分析的要求。结论 方法简便、快速，可应用于穿山龙药材中农药多残留的检测。

Determination of 23 Kinds of Pesticide Residues in Dioscoreae Nipponicae Rhizoma by Using Gas Chromatography-mass Spectrometry with Offline Disperse Solid Phase Extraction

OBJECTIVE To develop a method for the determination of 23 kinds of pesticide residues in Dioscoreae Nipponicae Rhizoma with the technique of disperse solid phase extraction and gas chromatography_electron impact mass spectrometry _selected ion monitoring (GC MS SIM. METHODS The interested pesticides were extracted from the samples with acetonitrile, then cleaned up by dispersive solid phase extraction with sorbents of primary secondary amine(PSA and graphitedcarbonblack(GCB. RESULTS The recoveries of all pesticides were in the range of 80.20%-118.5% at three spiked levels(5, 20 and 50 μg·kg^-1, and the relative standard deviations were 1.6%-8.5%. CONCLUSION The method is specific and suitable for the confirmatory of pesticide residues in Dioscoreae Nipponicae Rhizoma.