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Headspace solid-phase microextraction coupled to comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry for the analysis of aerosol from tobacco heating product
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2017-09-07 , DOI: 10.1016/j.chroma.2017.09.014
Benjamin Savareear , Radoslaw Lizak , Michał Brokl , Chris Wright , Chuan Liu , Jean-Francois Focant

A method involving headspace solid-phase microextraction (HS-SPME) and comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOFMS) was developed and optimised to elucidate the volatile composition of the particulate phase fraction of aerosol produced by tobacco heating products (THPs). Three SPME fiber types were studied in terms of extraction capacity and precision measurements. Divinylbenzene polydimethylsiloxane appeared as the most efficient coating for these measurements. A central composite design of experiment was utilised for the optimization of the extraction conditions. Qualitative and semi-quantitative analysis of the headspace above THP aerosol condensate was carried out using optimised extraction conditions. Semi-quantitative analyses of detected constituents were performed by assuming that their relative response factors to the closest internal standard (itR) were equal to 1. Using deconvoluted mass spectral data (library similarity and reverse match >750) and linear retention indices (match window of ±15 index units), 205 peaks were assigned to individual compounds, 82 of which (including 43 substances previously reported to be present in tobacco) have not been reported previously in tobacco aerosol. The major volatile fraction of the headspace contained ketones, alcohols, aldehydes, alicyclic hydrocarbons alkenes, and alkanes. The method was further applied to compare the volatiles from the particulate phase of aerosol composition of THP with that of reference cigarette smoke and showed that the THP produced a less complex chemical mixture. This new method showed good efficiency and precision for the peak areas and peak numbers from the volatile fraction of aerosol particulate phase for both THP and reference cigarettes.



中文翻译:

顶空固相微萃取结合全面的二维气相色谱-飞行时间质谱分析烟草加热产品中的气溶胶

建立并优化了一种涉及顶空固相微萃取(HS-SPME)和全面二维气相色谱-飞行时间质谱分析(GC×GC-TOFMS)的方法,以阐明颗粒相级分的挥发性成分烟草加热产品(THP)产生的气溶胶的数量。研究了三种SPME纤维的提取能力和精确度测量。二乙烯基苯聚二甲基硅氧烷似乎是这些测量中最有效的涂料。实验的中央复合设计被用于优化提取条件。使用优化的提取条件对THP气溶胶冷凝物上方的顶部空间进行了定性和半定量分析。ř)等于1。使用去卷积质谱数据(库相似度和反向匹配> 750)和线性保留指数(匹配窗口的±15个索引单位),将205个峰分配给各个化合物,其中82个峰(先前包括43种物质) (据报道存在于烟草中)以前没有在烟草气雾剂中报道过。顶部空间的主要挥发性部分包含酮,醇,醛,脂环族烃,烯烃和烷烃。将该方法进一步应用于比较THP气溶胶组合物颗粒相和参考香烟烟雾的颗粒相中的挥发物,结果表明THP生成的混合物不太复杂。

更新日期:2017-09-07
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