UPLC-MS/MS测定卷烟烟气、滤嘴和烟灰中5种常用杀菌剂及其转移行为研究

Determination of five commonly uesd fungicides in cigarette smoke,filter and ash by UPLC-MS/MS and study on their migration behaviors

建立了UPLC-MS/MS测定主流烟气总粒相物、气相物、滤嘴、烟蒂烟丝和烟灰中霜霉威、多菌灵、稻瘟灵、三唑醇和三唑酮含量的方法,样品经乙腈或甲醇提取,分散固相萃取后,进行UPLC-MS/MS分析。5种杀菌剂在各基质中的检出限为0.325~1.832ng/cig,平均回收率为90.9%~111.8%,RSD为1.3%~10.1%。应用该方法研究了标准卷烟加标样品和自然高残留样品中杀菌剂的烟气转移率,结果表明:标准卷烟加标样品中,5种杀菌剂向主流烟气总粒相物、滤嘴中的平均转移率分别为29.4%和11.0%,向烟蒂烟丝和烟灰中平均转移率为1.6%和0.2%,主流烟气气相物中则未检出杀菌剂;主流烟气总粒相物中,多菌灵的转移率较低(<5%),其它4种杀菌剂则接近或超过30%。自然高残留卷烟样品中,5种杀菌剂向烟气总粒相物中平均转移率为3.7%,在滤嘴中平均转移率为2.2%。卷烟实际燃吸过程中5种杀菌剂向烟气总粒相物转移率明显低于加标研究结果;若采用加标研究结果,成品卷烟杀菌剂残留对吸烟者的健康风险将被高估。

A study was conducted for the determination of propamocarb, carbendazim, isoprothiolane, triadimenol and triadimefon in cigarette smoke total particulate matter(TPM), gas phase, filters, cut tobacco leaves in butts and cigarette ash by UPLC-MS/MS. Test samples were extracted with acetonitrile or methanol, prepared by matrix dispersive solid phase extraction, subsequently analyzed by UPLC-MS/MS. Results showed that the average recoveries ranged from 90.9% to 111.8% with relative standard deviation(RSD) of 1.3%-10.1%. Limit of detection(LOD) values ranged from 0.325ng/cig to 1.832ng/cig. This method was applied to study migration behaviors of five commonly uesd fungicides in standard cigarettes spiked with fungicides and homemade high fungicides residue cigarettes. In standard cigarettes spiked with fungicides, five fungicides were significantly transferred to TPM with mean migration ratio of 29.4% and cigarette filter with mean transfer ratio of 11.0%. as well as few fungicides transferred into cut tobacco leaves in cigarette butts and cigarette ash. No fungicides were found transferring into gas phase.. In homemade high fungicides residue cigarettes, mean migration ratios of five fungicides in TPM(3.7%) and cigarette filter(2.2%) were much lower than standard cigarettes spiked with fungicides. In summary, transfer ratios of carbendazim, isoprothiolane and triadimenol in actual smoking would be obviously lower than standard cigarettes spiked with fungicides. The health risk of fungicide residues in cigarettes might be overestimated from the test results.