卷烟主流烟气中的4种重要杂环胺的SPE-GC/MS法测定研究

采用酸性溶剂萃取卷烟主流烟气剑桥滤片捕集物,目标分析物经固相萃取小柱分离富集后,应用气质联用仪进行定量分析,从而建立卷烟主流烟气中4种杂环胺的测定方法.4种待测物的检出限在0.14～0.24ng/支之间,样品加标回收率在79.7%至86.2%之间.工作曲线的相关系数均大于0.997.应用该方法测定了国内在售的10个重点品牌卷烟样品,结果显示1-甲基-吡啶并[3,4-b]吲哚(Harman)、9H-吡啶并[3,4-b]吲哚(Norharman)、2-胺基-9H-吡啶并[2,3-b]吲哚(AαC)、2-胺基-3-甲基-9H-吡啶并[2,3-b]吲哚(MeAαC)的含量范围分别为433.0～959.1ng/支、1220.4～2796.4ng/支、55.0～82.8ng/支、3.0～24.1ng/支.相关性分析结果表明Harman、Norharman和MeAαC分别与实测焦油量存在一定的线性相关性,且卷烟主流烟气中4种杂环胺的含量同卷烟类型无明显关联.

Analysis of four heterocyclic aromatic amines in cigarettes mainstream smoke by SPE-GC/MS

For the analysis of heterocyclic aromatic amines in the mainstream smoke condensate from Chinese brand cigarettes,the smoke condensates were collected on a filter pad,the analytes were isolated by using solid-phase extraction (SPE),and quantified on a Gas Chromatography-Mass(GC/MS).The relative index of working curves were 0.997,and the detection limits of four compounds ranged from 0.14 to 0.24 ng/cig.Relative standard deviation were 8.6%—13.6% (n=6).The recoveries of sample were 79.7%—86.2%.The method is suitable for determination of heterocyclic aromatic amines in smoke.Ten Chinese brand cigarettes which were sold popularly in China were determined,and the results showed that the contents of Harman,Norharman,AαCand MeAαCwere between 433.0—959.1 ng/cig,1220.4—2796.4 ng/cig,55.0—82.8 ng/cig,3.0—31.6 ng/cig,respectively.The relationship between the contents of heterocyclic aromatic amines and Tar was analyzed by SPSS,and the results showed that the contents of Harman,Norharman,AαCwere relative with realistic contents of tar,and the index were 0.8222,0.7918,0.7442,respectively.