索氏提取-气相色谱-质谱法测定卷烟主流烟气中苯并[a]芘  

Determination of benzo[a]pyrene in mainstream cigarette smoke by Soxhlet extraction-gas chromatography-mass spectrometry

作　　者：申钦鹏 刘春波 张凤梅 何沛 司晓喜 荆磊磊 王晋 缪明明 刘志华 杨光宇 

机构地区：[1]云南中烟工业有限责任公司技术中心云南省烟草化学重点实验室,昆明市五华区红锦路367号650231 [2]昆明理工大学化学工程学院

出　　处：《烟草科技》2016年第5期63-68,共6页Tobacco Science & Technology

基　　金：国家自然科学基金项目"液相-气相二维色谱新技术研究多环芳烃和亚硝胺在吸烟者体内的代谢"(21365026);云南省科学技术厅科技项目"用超临界-气相二维色谱新方法研究卷烟主流烟气中的香气成分"(2014FD078);云南中烟工业有限责任公司技术中心项目"SFC-GC-MS的联用及其在卷烟烟气香气成分中的应用研究"(JSZX2014JC04)

摘　　要：为简化样品前处理操作步骤,减小分析误差,设计了一种带有柱层析净化功能的索氏提取装置,基于该装置建立了测定卷烟主流烟气中苯并[a]芘(B[a]P)释放量的索氏提取-气相色谱-质谱(GC/MS)方法,并采用该方法对肯塔基参比卷烟2R4F和14个不同类型的卷烟样品进行了测定。结果表明:1利用该装置可直接对捕集卷烟主流烟气总粒相物后的剑桥滤片进行提取、净化和浓缩,浓缩液用GC/MS在选择离子监测模式下进行测定。2方法的线性范围为5~500 ng/mL(R^2=0.999 5),B[a]P的加标回收率为95.4%~104.2%,平均相对标准偏差(RSD)2.32%,检测限0.12 ng/支。32R4F参比卷烟和14个不同类型卷烟样品主流烟气中B[a]P的测定结果与采用GB/T 21130—2007方法的测定结果基本一致。该方法操作简便,灵敏度和准确度较高,适用于卷烟主流烟气中B[a]P的测定。To simplify sample preparation and reduce analysis errors, a Soxhlet extraction system combined with column chromatography purification was established to determine the levels of benzo[a]pyrene（B[a]P） in mainstream cigarette smoke. Kentucky 2R4 F reference cigarette and 14 cigarette samples were determined by the developed method. The results showed that： 1）The total particulate matter of mainstream cigarette smoke collected by a Cambridge filter pad was directly extracted, purified and concentrated by the improved Soxhlet extraction system. The extract was analyzed by gas chromatography-mass spectrometry under selected ion monitoring mode.2）B[a]P displayed a good linearity（R-2=0.999 5）in the range of 5 to 500 ng/mL, and the detection limit was 0.12ng/cig（S/N=3）. The developed method had recoveries of 95.4%-104.2% with relative standard deviations（RSD）of 2.32%. 3）The B[a]P in 2R4 F reference cigarette and the 14 cigarette samples determined by the new method basically agreed with those determined by the GB/T 21130—2007 method. This method is simple, sensitive,reliable and suitable for detecting B[a]P in mainstream cigarette smoke.

关 键 词：索氏提取 气相色谱-质谱法(GC/MS) 卷烟 主流烟气 苯并[a]芘(B[a]P) 

分 类 号：TS411.2[农业科学—烟草工业]