在线液相-气相二维色谱测定卷烟主流烟气中的苯并[a]芘  

Determination of Benzo[a]pyrene in Mainstream Cigarette Smoke by Online Comprehensive Two-dimensional Liquid-Gas Chromatography

作　　者：刘春波 申钦鹏 张凤梅 张安丰 何沛 司晓喜 刘志华 杨光宇 缪明明 

机构地区：[1]云南省烟草化学重点实验室,云南中烟工业有限责任公司技术中心,昆明650231

出　　处：《分析化学》2016年第2期241-246,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21365026)资助项目~~

摘　　要：建立了在线液相-气相二维色谱测定卷烟主流烟气中的苯并[a]芘方法。采用剑桥滤片捕集烟气粒相物,环己烷萃取,以D12-苯并[a]芘为内标,然后用在线液相-气相二维色谱测定：样品直接进样进入液相色谱,经微型硅胶柱分离,含苯并[a]芘的部位切割进入气相色谱,排干溶剂后启动气相色谱升温,经毛细管柱进行分离,用质谱检测。本方法将烟气苯并[a]芘测定中的硅胶柱层析和气相色谱-质谱分析在线连接起来,可不经样品前处理净化直接进样分析;而且每次进样可达40#L,与常规气相色谱-质谱分析最大进样2.0#L相比,分析灵敏度提高了20倍。方法线性范围达0.08~50 ng/L,相关系数为r2=0.999,回收率为94.2%~105.5%;检出限和定量限分别为0.09和0.30 ng/支,应用本方法对14个不同类型市售卷烟和2R4F标准烟进行了测定,结果与GB/T21130-2007测定结果相符合。An online comprehensive two-dimensional liquid-gas chromatography method was developed to determine the benzo [ a] pyrene （ B [ a ] P） in mainstream cigarette smoke. The B [ a ] P in mainstream cigarette smoke was collected by a cambridge filter pad, then the pad was extracted with cyclohexane and the extract was quantitatively analyzed by online LC-GC/MS with B [ a] P-D12 as an internal standard. After direct injection into the performance liquid chromatography, the benzo[ a] pyrene in the samples were separated by micro silica gel column and cut into the gas chromatography. After draining the solvent, the benzo[ a] pyrene was separated by capillary column gas chromatography warming and detected by mass spectrometry detection. By using silica gel column chromatography and gas chromatography-mass spectrometry in combination, the benzo ~ a] pyrene in the mainstream cigarette smoke was directly detected without any sample pretreatment. The sample injection volume of the method could reach 40 p,L each time, which was far greater than that of conventional gas chromatography-mass spectrometry （2.0 p,L of sample injection volume ） , resulting in an increasing analysis sensitivity of 20 times. The linearity range of the method （R：2= 0. 999） was in the range of 0.08 ng/L to 50 ng/L. The recoveries at three spiked levels ranged from 94.2% to 105.5% and the limit of detection was 0.09 ng/cig. This method was applied for the determination of benzo [a ] pyrene in 14 kind cigarettes in Chinese marked and the reference cigarettes 2R4F, and the determination results were consistent with GB/T21130-2007 method.

关 键 词：在线液相-气相二维色谱 苯并[A]芘 卷烟 主流烟气 

分 类 号：O657.63[理学—分析化学] TS411[理学—化学]