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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。②8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。
A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS / MS) was developed for the determination of 8 volatile carbonyl compounds (formaldehyde, acetaldehyde, acetone, acrolein, Butanone and butanal). A mixed solvent of acetonitrile and water (1: 1 by volume) was used to shake the extraction filter. The carbonyl group was detected by LC-ESI-MS / MS negative ion mode after derivatization with 2,4-dinitrophenylhydrazine. Four kinds of filters (cellulose acetate, activated carbon, fibril and paper filter) were selected for the optimization of conditions and the characterization of the method. The retention efficiency of the filter for eight carbonyls was also investigated. The results show that: ① the sample pretreatment is simple, high sensitivity. The detection limits of eight carbonyls ranged from 0.0044 to 0.0430 μg / branch. ② The recoveries of eight carbonyls were 92.8% ~ 118.4%. ③ The method for the complete and part of the filter day precision and daytime precision are less than 10%. ④ The retention efficiency of the eight carbonyls from high to low was activated carbon> cellulose acetate> paper> cellulose fiber filter. The retention efficiencies of all eight carbonyls were less than 5% and the retention efficiencies were high The carbonyls are formaldehyde and crotonaldehyde.