超低温溶剂提取-全二维气相色谱/飞行时间质谱法测定卷烟主流烟气中有机酸成分  

Determination of Organic Acids from Mainstream Cigarette Smoke using Ultra Low Temperature Solvent Extraction Followed by Comprehensive Two-Dimensional Gas Chromatography /Time-of-Flight Mass Spectrometry

作　　者：张权[1] 向章敏 蔡凯 周淑平 耿召良 郭玉双 陈文生[1] 

机构地区：[1]贵州师范大学贵州省山地环境信息系统与生态环境保护重点实验室,贵阳550001 [2]贵州省烟草科学研究院,贵阳550081

出　　处：《分析化学》2014年第8期1124-1130,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.31360431);贵州省烟草专卖局(公司)项目(No.201112;201307);贵州省科学技术基金(黔科合J字[2011]2143号)共同资助项目~~

摘　　要：建立了超低温溶剂提取结合全二维气相色谱/飞行时间质谱（GC×GC-TOF/MS）测定卷烟主流烟气中有机酸类成分的方法。首先利用乙醚为提取溶剂的超低温溶剂提取装置对卷烟主流烟气进行捕集,然后将提取液通过液液萃取、N,O-双（三甲基硅烷）三氟乙酰胺（BSTFA）衍生化后,以DB-1（30 m×0.25 mm,1.0μm）为一维色谱柱、DB-wax（1.5 m×0.1 mm,0.1μm）为二维色谱柱组成的柱系统对目标物进行分离,在调制周期为6 s、质量扫描范围为m/z 45~450的条件下,卷烟主流烟气中12种有机酸成分可以在58 min内得到准确的检测。实验结果表明,卷烟主流烟气中12种有机酸标准曲线相关系数R2〉0.99,加标回收率为80.2%~107.8%,相对标准偏差（RSD）的范围为0.4%~12.1%（n=5）,方法检出限为1.3~24.5μg/kg,定量限为4.1~77.1μg/kg。A new method for the determination of organic acids from mainstream cigarette smoke using ultra low temperature solvent extraction-comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry（GC×GC-TOF/MS）was established. The mainstream smoke was directly trapped by ethyl ether with ultra low temperature solvent extraction device, and cleaned up with liquid-liquid extraction. The concentrated extracts were further derived by N,O-bis（trimethylsily）trifluoroacetamide （BSTFA）. The good separation of silanized product was achieved by the column set of DB-1 （30 m × 0. 25 mm, 1. 0 μm） as the 1st column and DB-wax （1. 5 m × 0. 1 mm, 0. 1 μm） as the 2nd column with modulation period of 6 s and scan range of m/z 45-450 . The results showed that linearity correlation coefficients were larger than 0 . 99 , and the average recoveries were between 80. 17% and 107. 81% with the relative standard deviations （RSD） in the range of 0 . 4%-12 . 1% （ n=5 ） . The detection limit and the quantitation limit were 1 . 3-24 . 5 μg/kg and 4. 1-77. 1 μg/kg, respectively.

关 键 词：全二维气相色谱-飞行时间质谱 超低温溶剂提取 卷烟 主流烟气 有机酸 

分 类 号：O657.63[理学—分析化学] TS411[理学—化学]