HS-SPME-GC/MS法测定主流烟气中8种香味成分的逐口释放量

Puff-by-puff release of 8 aroma compounds in mainstream cigarette smoke as determined by HS-SPME-GC/MS

建立了测定卷烟主流烟气粒相物中香味成分的顶空-固相微萃取-气相色谱-质谱（HS—SPME—GC／MS）方法，并采用该方法定量测定了卷烟主流烟气中8种香味成分（吡啶、吡咯、糠醛、5-甲基糠醛、3-甲基吡啶、D-柠檬烯、2,3，5，6-四甲基吡嗪和β-大马酮）的逐口释放量。结果表明：①选用85μm碳分子筛／聚二甲基硅氧烷（CAR／PDMS）的固相微萃取头、萃取温度及时间为60℃和60min、解吸温度及时间为250℃和8min时，固相微萃取的效率最高；②在优化条件下，8种香味成分标样的工作曲线线性相关系数、相对标准偏差及加标回收率分别为0．9698～0．9995、3．8％～9．0％和78％～105％；③在卷烟燃吸过程中香味成分与烟碱的主流烟气递送规律存在明显的区别。随着抽吸口序的增加，主流烟气中总粒相物和烟碱释放量呈上升趋势，而8种香味成分的逐口主流烟气释放量比较平稳。

An HS-SPME-GC/MS （Headspace solid-phase microextraction-gas chromatography-mass spectrometry） method was developed to analyze selected aroma compounds in the particulate matters of mainstream cigarette smoke. The puff-by-puff release of 8 aroma compounds, including pyridine, pyrrole, furfural, 5-methyl furfural, 3-methylpyridine, D-limonene, 2, 3, 5, 6-tetramethyl pyrazine and β-damascenone were quantitatively determined with this method. The results showed that： 1） The optimal experimental conditions are： extracting with 85 μm CAR/PDMS SPME column at 60 % for 60 min and desorbing at 250℃ for 8 min. These parameters gave the highest SPME efficiency. 2） Under the optimized conditions, the linear correlation coefficients of the calibration curve, relative standard deviations （RSDs） and recoveries of the 8 standard compounds were 0.969 8-0.999 5, 3.8%-9.0% and 78%-105%, respectively. 3） The release of aroma compounds in mainstream smoke during ISO smoking differed from that of nicotine. With each puff, the release of total particulate matter and nicotine in mainstream smoke was increased, while the puff-by-puff yields of the 8 compounds in mainstream smoke were relatively stable.