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

2017年1月第50卷第1期

烟草科技

Tobacco Science&Technology

Jan.2017

V ol.50No.1

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

陈晓水，杨洋，汤晓东，蒋佳磊，赵路灿，张宸，朱书秀，陆明华*

浙江中烟工业有限责任公司技术中心,杭州市西湖区转塘镇科海路118号310024

摘要：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=0.9949~1.0000），目标物定量限均≤10ng·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。

关键词：卷烟；主流烟气；粒相物；分散液液微萃取（DLLME）；气相色谱-串联质谱（GC-MS/MS）；农药残留

中图分类号：TS411，S481+.8文献标志码：A文章编号：1002-0861（2017）01-0058-09 Determination of pesticide residues in particulate matter of mainstream cigarette smoke by dispersive liquid-liquid microextraction and gas chromatography-tandem mass spectrometry

CHEN Xiaoshui,YANG Yang,TANG Xiaodong,JIANG Jialei,ZHAO Lucan,ZHANG Chen,ZHU Shuxiu,LU Minghua*

Technology Center of China Tobacco Zhejiang Industrial Co.,Ltd.,Hangzhou310024,China

Abstract: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 of63pesticides.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 all63analytes with the correlation coefficients ranged from 0.9949to1.0000.The limits of quantification were no more than10ng/cig,and the average recoveries were 75.6%-127.5%with RSD from0.5%to19.0%at three different spiked levels.This method is simple,accurate, sensitive and suitable for the determination of63pesticide residues in particulate matter of mainstream cigarette smoke.

收稿日期：2016-06-17修回日期：2016-09-12

作者简介：陈晓水（1987—），硕士，工程师，主要从事烟叶与卷烟农残分析、烟气化学成分分析工作。E-mail：chenxiaoshui@ https://www.360docs.net/doc/6e1706912.html,；*通讯作者：陆明华，E-mail：lumh@https://www.360docs.net/doc/6e1706912.html,

引文格式：陈晓水，杨洋，汤晓东，等.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［J］.烟草科技, 2017，50（1）：58-66.（CHEN Xiaoshui，YANG Yang,TANG Xiaodong,et al.Determination of pesticide residues in

particulate matter of mainstream cigarette smoke by dispersive liquid-liquid microextraction and gas

chromatography-tandem mass spectrometry［J］.Tobacco Science&Technology，2017，50（1）：58-66.）DOI:10.16135/

j.issn1002-0861.2016.0286