全自动固相萃取-三重串联四极杆气相色谱/质谱联用测定食用菌中49种农药残留

Determination of 49 pesticide residues in edible fungi by automatic solid phase extraction and gas chromatography coupled with triple quadrupole tandem mass spectrometry

目的建立全自动固相萃取-三重串联四极杆气相色谱/质谱联用(GC-MS/MS)同时测定食用菌中49种农药残留的分析方法。方法样品加乙腈超声提取后经全自动固相萃取仪净化,采用三重串联四极杆气相色谱/质谱联用在多反应监测模式(MRM)下进行测定。结果在MRM模式下用两对离子对4大类49种常用农药进行分析,基线漂移少,且在5 V^40 V能量范围内,对母离子进行了碰撞能量优化;49种农药的线性范围为0.01μg/ml^10.0μg/ml,线性相关系数在0.9900~0.9994之间,检出限为0.01μg/kg^3.0μg/kg,定量限为0.03μg/kg^10.0μg/kg,平均加标回收率为80.1%~110.0%,相对标准偏差(RSD)均<10%。结论该方法具有良好的回收率及稳定性,适合食用菌中多种农药残留的测定。

Objective To establish an analytical method for simultaneous determination of 49 pesticide residues in edible fungi by automatic solid phase extraction and gas chromatography coupled with triple quadrupole mass spectrometry（ GC/ MS/ MS）. Methods The samples were extracted with acetonitrile,cleaned up by automatic solid phase extracter,then analyzed by gas chromatography-triple quadrupole tandem mass spectrometry using multiple reaction monitoring（ MRM） mode. Results Forty-nine kinds of commonly used pestcides from 4 categories were analyzed in the MRM mode using two pairs of ions,with less baseline drift. The collision energy of the parent ion was optimized in the eneergy range of 5 V - 40 V. The linear range of 49 pesticides were between 0. 01 μg/ ml and 10. 0 μg/ ml,the linear correlation coefficients were from 0. 9900 to 0. 9994,the limits of detection were from 0. 01 μg/ kg to 3. 0 μg/ kg,the limits of quantication were from 0. 03 μg/ kg to 10. 0 μg/ kg,the average recovery rates were in the range of 80. 1% - 110. 0% and the relative standard deviations（ RSD） were all less than 10%. Conclusion The method is applied to the routine analysis of multiple pesticides in edible fungi,with better recovery rate and statbility.