大体积顶空-气相色谱-质谱法半定量分析卷烟开包气息化合物  

Semi-Quantitative Analysis of Cigarette Unpacking Breath Compounds by Large Volume Headspace-Gas Chromatography-Mass Spectrometry

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作  者:吴秉宇 周梦茜 刘彦穹 刘百战[1] 费婷[1] 罗辰[1] 吴达[1] 束茹欣 WU Bingyu;ZHOU Mengxi;LIU Yanqiong;LIU Baizhan;FEI Ting;LUO Chen;WU Da;SHU Ruxin(Technical Center,Shanghai Tobacco Group Co.,Ltd.,Shanghai 201315,China)

机构地区:[1]上海烟草集团有限责任公司技术中心,上海201315

出  处:《理化检验(化学分册)》2024年第11期1104-1109,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基  金:中国烟草总公司科技重点项目(110201802004)。

摘  要:改进了商品化大体积顶空进样系统,用保温棉包裹冷阱使其维持在220℃作为高温模块,将分流口移至高温模块,在密闭条件下将多维捕集阱预加热至210℃,使顶空成分脱附后瞬时进样。将卷烟小盒包装顶部拆封后,迅速放入大体积顶空样品瓶,加入含0.4 mg·L^(-1)氘代苯乙烯的甲醇溶液(内标)1 m L,拧盖密封后在平衡温度40℃下平衡40 min,在DB-Heavy WAX色谱柱上按照柱升温程序分离,质谱分析采用电子轰击离子(EI)源,全扫描(SCAN)模式。结果表明,大部分化合物测定值的相对标准偏差(n=6)小于6.0%;方法用于分析不同类型卷烟样品,不同类型的卷烟开包气息化合物的差异明显,主要差异性化合物为吡嗪类、萜烯类、酯类和酸类。The commercial large volume headspace sampling system was improved.The cold trap was wrapped with insulation cotton to keep at 220℃as a high temperature module,and the diversion port was moved to the high temperature module.The multidimensional trap was pre-heated to 210℃under sealed condition to allow the headspace components to desorb and inject the sample instantly.The top of the cigarette packaging in a small box was opened,and quickly placed into a large volume headspace sample bottle.1 mL of methanol solution containing 0.4 mg·L^(−1) deuterated styrene(internal standard)was added,and the bottle was sealed.The mixture was heated and equilibrated at 40℃for 40 min,and separated on a DB-HeavyWAX chromatographic column according to the column heating program.Electron impact ion(EI)source and full scan(SCAN)mode were adopted in mass spectrometry analysis.As shown by the results,the RSDs(n=6)of the determined values of most compounds were less than 6.0%.This method was used for analysis of different types of cigarette samples,and there were significant differences in unpacking breath compounds of different types of cigarettes,with the main differential compounds of pyrazines,terpenes,esters,and acids.

关 键 词:大体积顶空 气相色谱-质谱法 卷烟 开包气息化合物 

分 类 号:O657.63[理学—分析化学]

 

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