分散液液微萃取-GC-MS/MS法测定卷烟主流烟气粒相物中的农药残留

Determination of pesticide residues in particulate matter of mainstream cigarette smoke by dispersive liquid-liquid microextraction and gas chromatography-tandem mass spectrometry

为测定卷烟主流烟气粒相物中的农药残留,通过考察优化萃取剂种类、萃取剂体积、萃取时间等因素,建立了检测卷烟主流烟气粒相物中63种农药残留的分散液液微萃取(DLLME)-气相色谱-串联质谱(GC-MS/MS)方法。用乙腈振荡萃取捕集主流烟气粒相物后的剑桥滤片,萃取液进行DLLME处理,取四氯化碳相进行GC-MS/MS测定,内标法定量。结果表明:63种农药在各自的线性范围内线性关系良好(R2=0.994 9~1.000 0),目标物定量限均≤10 ng·支-1;在高、中、低3个加标水平下,农药的平均回收率为75.6%~127.5%,相对标准偏差为0.5%~19.0%。该方法简单、准确,灵敏度高,适用于卷烟主流烟气粒相物中63种农药残留的测定。

In order to quantify the pesticide residues in particulate matter of mainstream cigarette smoke, a procedure using acetonitrile-based extraction combined with dispersive liquid-liquid microextraction （DLLME） and gas chromatography-tandem mass spectrometry （GC-MS/MS） detection was developed for determining the residues of 63 pesticides. The effects of extraction solvent type and volume, extraction time were investigated and optimized. The total particulate matter of mainstream cigarette smoke collected by a Cambridge filter pad was extracted with acetonitrile under oscillation, the extract was further disposed by DLLME, the obtained tetrachloromethane extract was analyzed by GC-MS/MS and quantified by internal standard method. The results showed that good linearity was observed for all 63 analytes with the correlation coefficients ranged from 0.994 9 to 1.000 0. The limits of quantification were no more than 10 ng/cig, and the average recoveries were 75.6%-127.5% with RSD from 0.5% to 19.0% at three different spiked levels. This method is simple, accurate, sensitive and suitable for the determination of 63 pesticide residues in particulate matter of mainstream cigarette smoke.