在线凝胶色谱-气质联用测定卷烟主流烟气中的苯并a芘-烟草科技.PDFVIP

烟草科技/ Tobacco Science Technology 烟草化学/ Tobacco Chemistry 2014 年第9 期（总第326 期） 在线凝胶色谱-气质联用测定卷烟主流烟气中的苯并[a]芘 段沅杏，王昆淼，刘志华，张 霞，杨光宇，韩敬美，赵 伟，缪明明* 云南中烟工业有限责任公司技术中心，昆明市五华区红锦路367 号 650032 摘要：建立了准确测定卷烟主流烟气中苯并[a] 芘（B[a]P ）的在线凝胶色谱- 气质联用（在线GPC-GC/MS ）分 析方法。卷烟主流烟气依次经剑桥滤片捕集、环己烷萃取后进行在线GPC-GC/MS 测定，以苯并[a] 芘-d12 2 （B[a]P-d ）为内标进行定量。结果表明：B[a]P 在0.4~50 ng/mL 浓度范围内线性关系良好（R =0.9995 ），3 个 12 加标水平的回收率在95.6%~97.2% 之间，平均相对标准偏差（RSD）2.18% ，检出限0.28 ng/ 支。该方法灵敏 度高、定性定量结果可靠，适用于卷烟主流烟气中B[a]P 的测定。 关键词：在线GPC-GC/MS ；苯并[a] 芘；卷烟；主流烟气 中图分类号：TS411.2 文献标识码：A 文章编号：1002-0861 （2014 ）09-0039-05 Determination of Benzo[a]pyrene in Mainstream Cigarette Smoke by Online Gel Permeation Chromatography-Gas Chromatography/Mass Spectrometry DUAN Yuanxing, WANG Kunmiao, LIU Zhihua, ZHANG Xia, YANG Guangyu, HAN Jingmei, ZHAO Wei, and MIAO Mingming* Technology Center, China Tobacco Yunnan Industrial Co., Ltd., Kunming 650032, China Abstract: In order to accurately determine the benzo[a]pyrene (B[a]P) in mainstream cigarette smoke, an online gel permeation chromatography-gas chromatography/mass spectrometry (online GPC-GC/MS) method was developed. The B[a]P in mainstream cigarette smoke was collected by a Cambridge filter pad, then the pad was extracted with cyclohexane, the extract was quantitatively analyzed by online GPC-GC/MS with B[a]P-d12 2 as an internal standard. The results showed that: B[a]P displayed good linearity (R=0.9995) in the range of 0.4 to 50 ng/mL. The recoveries at three spiked levels ranged from 95.6% to 97.2% with the mean relative standard deviation of 2.18% and the limit of detection of 0.28 ng/cig. This method is reliable, sensitive