采用LC/MS/MS测定侧流卷烟烟气中挥发性羰基化合物的方法研究  

Quantitative analysis of volatile carbonyls in side-stream cigarette smoke by LC/MS/MS

作　　者：严莉红 易小丽[1] 周骏[1] 白若石[1] 何爱军[1] 

机构地区：[1]北京卷烟厂,北京市朝阳区管庄西里42号100024

出　　处：《中国烟草学报》2008年第5期7-14,26,共9页Acta Tabacaria Sinica

基　　金：北京卷烟厂重点科研项目2005-2

摘　　要：挥发性羰基化合物是卷烟烟气中的一类重要有害物质,准确测定卷烟烟气中,特别是侧流卷烟烟气中的挥发性羰基化合物还有许多问题有待解决。实验中采用2,4-二硝基苯肼(DNPH)酸性溶液捕集侧流烟气中的羰基化合物,乙腈水溶液稀释后,以对羟基苯甲酸丁酯为内标物,用带有负离子电喷雾的LC/MS/MS定量分析侧流烟气中8种挥发性羰基化合物。实验证明,此方法有较好的重复性:对8种羰基化合物测定的相对标准偏差在6%以下;具有较高的灵敏度:8种挥发性羰基化合物的检出限均低于2.8ng/cig;较高的准确性:8种挥发性羰基化合物的回收率在87.2%～104.7%之间。与以往的分析方法相比,该方法具有更高的选择性,实现了烟气中巴豆醛、2-丁酮的DNPH衍生物的同分异构体的分离,对巴豆醛、2-丁酮定量更为准确,分析方法的灵敏度也明显提高。Volatile carbonyls are possible sources of careinogenicity in cigarette smoke. There are still many problems to be solved in the accurate determination of volatile carbonyls in cigarette smoke, especially in side-stream smoke. In the experiment, cigarette smoke was collected using a Cambridge filter connected to an impinger with acidic solution of 2, 4-dinitrophenylhydrazine. The collected volatile carbonyls were extracted with acetonitrile/water solution and analyzed by reversedphase liquid chromatography coupled with quadrupole tandem mass spectrometry in negative electro-spray ionization mode using butyl paraben as internal standard. Results showed that this method achieved excellent reproducibility and the relative standard deviations were generally below 6%. Limit of detection for every carbonyl was less than 2.8ng/cig. The recoveries and accuracies were in the range of 87.2% to 104.7% and 90.1% to 103.3%, respectively. This new method had higher selectivity and sensitivity compared to conventional methods, and achieved the separation of DNPH-crotonaldehyde and DNPH-methylethyl-ketone isomers successfully.

关 键 词：LC/MS/MS 侧流烟气 挥发性羰基化合物 测定 

分 类 号：TS411.2[农业科学—烟草工业]