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
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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 the1st 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.
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 the1st 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.
引文
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7 XU Guo-Wang,YE Fen,KONG Hong-Wei,LU Xin,ZHAO Xin-Jie.Chinese Journal of Chromatography,2001,19(2):132 -136许国旺,叶芬,孔宏伟,路鑫,赵欣捷.色谱,2001,19(2):132-136
8 LU Xi-Mei,XIE Fu-Wei,LIU Hui,LI Jian-Jun,QU Ling-Bo,LIU Hui-Min.Tobacco Sci.Technol.,2006,(6):24-29鲁喜梅,谢复炜,刘晖,李建军,屈凌波,刘惠民.烟草科技,2006,(6):24-29
9 ZHENG Yue-Ming,FENG Feng,GUO Wei,CHU Xiao-Gang,PAN Jia-Rong,JIA Wei.Chinese Journal of Chromatography,2012,30(11):1166-1171郑月明,冯峰,国伟,储晓刚,潘家荣,贾玮.色谱,2012,30(11):1166-1171
10 WANG Yang,YU Zhi-Qiang,LUO Xiang-Fan,FENG Jia-Liang,ZHANG Dong-Ping,REN Guo-Fa.Chinese J.Anal.Chem.,2012,40(8):1187-1193汪洋,于志强,罗湘凡,冯加良,张东平,任国发.分析化学,2012,40(8):1187-1193
11 SHEN Bao-Jia,QIN Kun-Ming,LIU Qi-Di,CAI Hao,LIU Xiao,CAI Bao-Chang.Sci.Sin.Chim.,2013,43(11):1480-1489(in Chinese)沈保家,秦昆明,刘启迪,蔡皓,刘晓,蔡宝昌.中国科学:化学,2013,43(11):1480-1489
12 WU Jian-Fang,LU Xin,TANG Wan-Ying,KONG Hong-Wei,ZHOU Shen-Fan,XU Guo-Wang.Chinese J.Anal.Chem.,2004,32(5):582-586武建芳,路鑫,唐婉莹,孔宏伟,周申范,许国旺.分析化学,2004,32(5):582-586
13 JIANG Jun,LI Pei-Wu,XIE Li-Hua,DING Xiao-Xia,LI Ying,WANG Xiu-Pin,WANG Xue-Fang,ZHANG Qi,GUAN Di.Chinese J.Anal.Chem.,2011,39(1):72-76姜俊,李培武,谢立华,丁小霞,李英,王秀嫔,汪雪芳,张奇,管笛.分析化学,2011,39(1):72-76
14 ZHU Shuai,GAO Li-Rong,ZHENG Ming-Hui,LIU Hui-Min,ZHANG Bing,LIU Li-Dan,WANG Yi-Wen.Journal of Instrumental Analysis,2014,33(3):301-306朱帅,高丽荣,郑明辉,刘卉阂,张兵,刘立丹,王毅文.分析测试学报,2014,33(3):301-306
2 Rodgman R A,Perfetti T A.The Chemical Components of Tobacco and Tobacco Smoke.,2nd ed.New York:CRC Press,2009:1258-1259
3 ZHANG Ying-Chun,GUO Hai-Ning,YUE Hai-Bo.Journal of Analytical Science,2010,26(5):567-571张迎春,郭国宁,岳海波.分析科学学报,2010,26(5):567-571
4 WANG Jian,WENG Jun-Jie,JIA Liang-Yuan,PAN Yang.Chinese J.Anal.Chem.,2012,40(7):1048-1052王健,翁俊桀,贾良元,潘洋.分析化学,2012,40(7):1048-1052
5 TUO Su-Xing,YANG Hua-Wu,WU Ming-Jian,DAI Yun-Hui.Chinese J.Anal.Chem.,2012,40(7):1053-1058庹苏行,杨华武,吴名剑,戴云辉.分析化学,2012,40(7):1053-1058
6 LU Hong-Liang,ZHAO Ming-Yue,LIU Hui-Min,GONG An-Da,YU Jing,ZHENG Hu-Nan,LIANG Li-Li,LI Li,WEI Bu-Jian.Chinese Journal of Chromatography,2007,25(1):30-34鹿洪亮,赵明月,刘惠民,龚安达,于静,郑湖南,梁俐俐,李莉,魏步建.色谱,2007,25(1):30-34
7 XU Guo-Wang,YE Fen,KONG Hong-Wei,LU Xin,ZHAO Xin-Jie.Chinese Journal of Chromatography,2001,19(2):132 -136许国旺,叶芬,孔宏伟,路鑫,赵欣捷.色谱,2001,19(2):132-136
8 LU Xi-Mei,XIE Fu-Wei,LIU Hui,LI Jian-Jun,QU Ling-Bo,LIU Hui-Min.Tobacco Sci.Technol.,2006,(6):24-29鲁喜梅,谢复炜,刘晖,李建军,屈凌波,刘惠民.烟草科技,2006,(6):24-29
9 ZHENG Yue-Ming,FENG Feng,GUO Wei,CHU Xiao-Gang,PAN Jia-Rong,JIA Wei.Chinese Journal of Chromatography,2012,30(11):1166-1171郑月明,冯峰,国伟,储晓刚,潘家荣,贾玮.色谱,2012,30(11):1166-1171
10 WANG Yang,YU Zhi-Qiang,LUO Xiang-Fan,FENG Jia-Liang,ZHANG Dong-Ping,REN Guo-Fa.Chinese J.Anal.Chem.,2012,40(8):1187-1193汪洋,于志强,罗湘凡,冯加良,张东平,任国发.分析化学,2012,40(8):1187-1193
11 SHEN Bao-Jia,QIN Kun-Ming,LIU Qi-Di,CAI Hao,LIU Xiao,CAI Bao-Chang.Sci.Sin.Chim.,2013,43(11):1480-1489(in Chinese)沈保家,秦昆明,刘启迪,蔡皓,刘晓,蔡宝昌.中国科学:化学,2013,43(11):1480-1489
12 WU Jian-Fang,LU Xin,TANG Wan-Ying,KONG Hong-Wei,ZHOU Shen-Fan,XU Guo-Wang.Chinese J.Anal.Chem.,2004,32(5):582-586武建芳,路鑫,唐婉莹,孔宏伟,周申范,许国旺.分析化学,2004,32(5):582-586
13 JIANG Jun,LI Pei-Wu,XIE Li-Hua,DING Xiao-Xia,LI Ying,WANG Xiu-Pin,WANG Xue-Fang,ZHANG Qi,GUAN Di.Chinese J.Anal.Chem.,2011,39(1):72-76姜俊,李培武,谢立华,丁小霞,李英,王秀嫔,汪雪芳,张奇,管笛.分析化学,2011,39(1):72-76
14 ZHU Shuai,GAO Li-Rong,ZHENG Ming-Hui,LIU Hui-Min,ZHANG Bing,LIU Li-Dan,WANG Yi-Wen.Journal of Instrumental Analysis,2014,33(3):301-306朱帅,高丽荣,郑明辉,刘卉阂,张兵,刘立丹,王毅文.分析测试学报,2014,33(3):301-306