GC-MS/MS法测定8种植物提取物中15种拟除虫菊酯类农药的残留量

Determination of 15 kinds of pyrethroid pesticide residues in 8 kinds of plant extracts by GC-MS /MS

建立了8种植物提取物中15种拟除虫菊酯类农药残留的气相色谱-三重四级杆串联质谱（GC—MS／MS）分析方法。试样经正己烷提取，弗罗里硅土（Florisil）固相萃取小柱净化，采用GC—MS／MS法在多反应离子监测（MRM）模式下进行检测，外标法定量。结果表明，15种拟除虫菊酯农药在0．008～1．0 mg／L范围内线性关系良好，相关系数（r2）均大于0．9989；加标回收率为63．4％～133．0％；RSD为2．9％～17％（n=6）；方法的定量限（LOQ）为0．001-0．06mg／kg。方法适用于石榴皮等8种植物提取物中15种拟除虫菊酯类农药残留的定性、定量分析。

An effective method was developed and applied to determination of 15 kinds of pyrethroid pesticide residues in 8 kinds of plant extracts with gas chromatography-triple quadrupole mass spectrometry （GC-MS/ MS）. After extracted by n-hexane and purified on a Florisil solid-phase extraction column, samples were determined by GC-MS/MS in multi-reaction monitoring （MRM） mode, and the external calibrations was used for the quantification. The results showed good linearity with the correlation coefficients （ r2 ） higher than 0. 9989 in the range of 0. 008 ~ 1.0 mg/L, the limits of quantification （ LOQ ） were 0. 003 ~ 0. 17 mg/kg. The recoveries were in the range of 63.4% - 133.0% with the relative standard deviations（ RSDs ）between 2. 9% and 17% （n =6）. This method is simple, sensitive, and can be used for quantification and qualitative analysis of pomegranate peel and other 8 kinds of plant extracts.