摘要
建立了液相色谱-电喷雾电离串联质谱(LC—ESI—MS/MS)测定卷烟滤嘴中8种挥发性羰基化合物(甲醛、乙醛、丙酮、丙烯醛、丙醛、巴豆醛、2-丁酮和丁醛)的方法。采用乙腈:水为1:1(体积比)的混合溶剂振荡萃取滤嘴,羰基物与2,4-二硝基苯肼衍生化反应后用LC.ESI-MS/MS负离子模式检测。选取4种类型滤嘴(醋纤、活性炭、丙纤和纸滤嘴)进行条件优化和方法表征,并考察了滤嘴对8种羰基物的截留效率。结果表明:①该方法样品前处理简单,灵敏度高。8种羰基物的检测限在0.0044-0.0430μg/支之间。⑦8种羰基物的加标回收率为92.8%~118.4%。③该方法对于完整和部分滤嘴的日内精密度和日间精密度均小于10%。④滤嘴对8种羰基物的截留效率由高到低的顺序为活性炭〉醋纤〉纸〉丙纤滤嘴,对8种羰基物总量的截留效率均〈5%,截留效率较高的羰基物为甲醛和巴豆醛。
For determining the eight volatile carbonyl compounds (formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butanone, and butyraldehyde) in cigarette filter, a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) method was developed. The cigarette filters were extracted by shaking with acetonitrile aqueous solution (1:1, V/V), then the extract derivatively reacted with 2, 4-dinitrophenylhydrazine. The derivatives were analyzed by LC-ESI-MS/MS in negative ion mode. Four types of cigarette filter (i.e. cellulose acetate filter, activated carbon filter, polypropylene fiber filter, and paper filter) samples were selected for the optimization and characterization of analytical method, and their filtration efficiencies to the eight carbonyl compounds were also investigated. The results showed that: 1) The developed method featured simple pretreatment and high sensitivity, and the detection limit for the eight carbonyl compounds ranged from 0.0044 to 0.0430 μg/cig. 2) The recoveries of standard addition of the eight carbonyl compounds were from 92.8% to 118.4%. 3) The precisions of intra-day and inter-day were all less than 10% for whole or part of cigarette filters. 4) The filters in the order of filtration efficiency to the eight carbonyl compounds were activated carbon filter 〉 cellulose acetate filter 〉 paper filter 〉 polypropylene fiber filter. The filtration efficiencies of the said four filters to the total content of the eight carbonyl compounds were all less than 5%, though their filtration efficiencies to formaldehyde and crotonaldehyde were higher.
出处
《烟草科技》
EI
CAS
北大核心
2013年第9期39-46,共8页
Tobacco Science & Technology
基金
郑州烟草研究院科技项目"基于滤嘴分析的吸烟者烟气主要有害成分暴露量评估方法研究"(312011CZ0590)
关键词
液相色谱-电喷雾电离串联质谱法
卷烟滤嘴
挥发性羰基化合物
Liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS)
Cigarette filter
Volatile carbonyl compound