气相色谱-串联质谱法测定莲雾中的灭蚁灵和哒螨灵残留

建立了同时测定莲雾Syzygium samarangense(Bl.)Merr.et Perry中灭蚁灵和哒螨灵残留的气相色谱-串联质谱(GC-MS/MS)分析方法。样品经乙腈匀浆提取,石墨化碳黑/氨基混合型固相萃取柱净化,GC-MS/MS检测。采用所建立的方法,在0.01~0.5 mg/kg下进行添加回收试验,2种农药的平均回收率在89%~102%之间,相对标准差为1.7%~5.2%(n=5);方法的线性范围为0.01~0.5 mg/L,决定系数(R2)0.99;对灭蚁灵和哒螨灵的定量限均为0.005 mg/kg。所建方法能满足莲雾中灭蚁灵和哒螨灵残留同时检测的要求。

Determination of mirex and pyridaben residues in wax-apple by gas chromatography-tandem mass spectrometry

A novel method for determining mirex and pyridaben residues in wax-apple (Syzygium samarangense(Bl.)Merr. et Perry) was developed by using gas chromatography-tandem mass spectrometry(GC-MS/MS) detection. The samples were extracted with acetonitrile. After cleanup on carbon/NH₂ column with elution solvents of V (acetonitrile): V (toluene)=3:1 and further concentration, GC-MS/MS was used to analyze the samples. The average recoveries of 2 pesticides were 89%-102% at spiked levels of 0.01, 0.05, 0.1 and 0.5 mg/kg, with relative standard deviations (RSDs) in the range of 1.7%-5.2% (n=5). The calibration curve was linear in the range of 0.01-0.5 mg/L and coefficient of determination R²>0.99.The limits of quantitation (LOQ) for mirex and pyridaben were 0.005 mg/kg. The method is applicable for detection of mirex and pyridaben residues in wax-apple.