通过式固相萃取与液相色谱串联质谱和气相色谱串联质谱结合测定加热卷烟中多种农药残留  

Determination of multiple pesticide residues in heated cigarettes by liquid chromatography tandem mass spectrometry and gas chromatography tandem mass spectrometry combined with pass-through solid phase extraction

作　　者：杨飞[1] 纪元 刘珊珊[1] 王颖[1] 范子彦[1] 邓惠敏[1] 边照阳[1] 陈晓水[2] 唐纲岭[1] YANG Fei;JI Yuan;LIU Shanshan;WANG Ying;FAN Ziyan;DENG Huimin;BIAN Zhaoyang;CHEN Xiaoshui;TANG Gangling(China National Tobacco Quality Supervision&Test Center,Zhengzhou 450001,China;Technology Center of China Tobacco Zhejiang Industrial Co.,Ltd.,Hangzhou 310024,China)

机构地区：[1]国家烟草质量监督检验中心,郑州450001 [2]浙江中烟工业有限责任公司技术中心,杭州310024

出　　处：《中国烟草学报》2021年第3期1-10,共10页Acta Tabacaria Sinica

摘　　要：【目的】实现加热卷烟中多种农药残留的测定。【方法】样品经乙腈提取,以PRiME HLB通过式固相萃取柱净化后,分别以液相色谱-串联质谱(LC-MS/MS)和气相色谱-串联质谱(GC-MS/MS)分析。【结果】①PRiME HLB通过式固相萃取净化效率高,操作简便。②在高、中、低三个不同添加浓度水平下,所有分析物的回收率在77.36%~108.28%之间,相对标准偏差(RSD)小于8.0%。所有农药均获得了良好的线性相关系数(r≥0.9977),检出限(LOD)和定量限(LOQ)范围分别为0.31~10.88μg/kg和1.11~36.21μg/kg。③采用该方法对25个实际样品进行了检测,所有样品均检出有杀菌剂。【结论】该方法操作简便,结果准确可靠,可用于测定加热卷烟中的多种农药残留。[Objective]In order to realize the determination of multiple pesticide residues in heated cigarettes.[Methods]The samples were extracted with acetonitrile,purified by PRiME HLB pass-through solid phase extraction,and analyzed by LC-MS/MS and GC-MS/MS,respectively.[Results]①The purification efficiency of PRiME HLB pass-through solid phase extraction is high and the operation is simple.②Under high,medium and low levels of addition concentration of,the recoveries of all compounds were 77.36%-108.28%,with relative standard deviations(RSDs)less than 8.0%.Good linear correlation coefficients were obtained(r≥0.9977)for all studied analytes.The LOD for all analytes varied from 0.31-10.88μg/kg and the LOQ varied from 1.11-36.21μg/kg.③Twenty five actual samples were tested using this method,and all samples were found to be contaminated by fungicides.[Conclusion]The method is simple to operate,accurate and reliable,and can be used for the determination of multiple pesticide residues in heated cigarettes.

关 键 词：加热卷烟 农药残留 通过式固相萃取 气相色谱-串联质谱 液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] TS411[理学—化学]