利用固相萃取-气相色谱-负化学离子源质谱技术快速分析茶叶中3种杀螨剂和八氯二丙醚农药残留

建立了茶叶中3种杀螨剂及八氯二丙醚农药残留快速分析的固相萃取-气相色谱-负化学离子源质谱检测(GC-NCI-MSD)方法，并应用于出口欧盟茶叶中农残检测及基地监管.样品经正己烷-丙酮(1∶1，V∶V)提取后，用固相萃取柱(Agela)除去茶叶中干扰物质，以环氧七氯为内标物，经气相色谱-负化学离子源质谱分时段选择离子监测...

Rapid Determination of 3 Acaricides and Octachloro-Dipropyl Ether(S-421) Pesticide Residues in Tea by Gas Chromatography-Negative Chemical Ionization Mass Spectrometry

A solid phase extraction(SPE)-gas chromatography(GC)-negative chemical ionization mass spectrometry(NCI/MS) method has been set up for the analysis of 3 acaricides and octachloro-dipropyl-ether pesticides in tea,and has been applied to the detection and base regulation of pesticide residues in tea for EU exports.Pesticide residues were extracted from tea samples with hexane-acetone(1∶1,by vol) and cleaned-up by active carbon and Florisil SPE column to remove co-extractives,and with heptachlor-epoxide as the internal standard.Analytical screening was determined by the technique of gas chromatography-negative chemical ionization mass spectrometry-selected ion monitoring.The recoveries of all pesticides were in the range of 80%～110%at three spiked level(5～80 μg/kg) and relative standard deviations were below 5.5%.The detection limits of tetradifon,dicofol,pyridaben,and S-421 are 0.1 μg/kg,0.4 μg/kg,1.0 μg/kg and 2.0 μg/kg respectively.The method showed excellent sensitivity and selectivity for 3 acaricides and octachloro-dipropyl-ether pesticides.