气相色谱-串联质谱法快速检测百合(干)中11种有机氯类农药残留

Rapid Determination of 11 Organochlorine Pesticide Residues in Dried Lily Bulb by Gas Chromatography-Tandem Mass Spectrometry

基于QuEChERS方法,研究建立一种快速检测百合(干)中11种有机氯类农药残留的气相色谱-串联质谱方法。用乙腈提取,N-丙基乙二胺(PSA)、十八烷基键合硅胶(C_(18))、石墨化炭黑(GCB)粉末净化,应用多反应监测模式(Multiple Reaction Monitoring,MRM)。11种农药在0.005~0.300 mg·L^(-1)线性关系良好,相关系数(R^(2))均大于0.999;在0.025 mg·kg^(-1)、0.050 mg·kg^(-1)、0.100 mg·kg^(-1)3个加标水平的平均回收率为88.95%~112.69%,相对标准偏差为0.29%~4.62%,该方法的检出限为0.88~3.13μg·kg^(-1)。该方法操作简单、快速,重复性和精密度良好,可适用于百合(干)中有机氯类农药残留的检测。

Based on the QuEChERS method,a gas chromatography-tandem mass spectrometry method for rapid detection of 11 organochlorine pesticide residues in dried lily bulb was established.The samples were extracted with acetonitrile,the pesticide residues in the supernatant and clean-up with a mixture of sorbents(PSA,C_(18) and GCB),and detected by multiple reaction monitoring.The linear relationship between the 11 pesticides was good at the concentration of 0.005~0.300 mg·L^(-1),and the linear correlation coefficients(R^(2))was greater than 0.999;the average recoveries at three spiking levels(0.025 mg·kg^(-1),0.050 mg·kg^(-1),0.100 mg·kg^(-1))in dried lily bulb ranged from 88.95%to 112.69%,and the relative standard deviations was 0.29%to 4.62%,the limit of detection of the established method were in the range of 0.88μg·kg^(-1) to 3.13μg·kg^(-1).The preprocessing method is simple,rapid,repeatable and precise,so that it is suitable for the detection of organochlorine pesticide residuesin dried lily bulb.