超声萃取-气相色谱-质谱法测定卷烟主流烟气中的6种挥发酚
GC-MS Determination of 6 Volatile Phenols in Mainstream Smoke of Cigarettes with Ultrasonic Extraction
摘 要
采用气相色谱-质谱法测定卷烟主流烟气中的苯酚、对甲酚、间甲酚、邻甲酚、对苯二酚和间苯二酚等6种挥发酚的含量。用剑桥滤片在标准抽吸条件下采集5支卷烟烟气粒相物,用甲醇超声萃取10 min。所得萃取液用DB-624毛细管色谱柱(30 m×0.25 mm,1.4 μm)为固定相进行分离,在质谱分析中采用全扫描和选择离子监测模式。以苯酚-D5为内标物。方法的检出限(3S/N)在10~16 ng·支-1之间,测定下限(10S/N)在28~40 ng·支-1之间。加标回收率在84.6%~99.1%之间,测定值的相对标准偏差(n=6)在2.1%~6.4%之间。
超声萃取
挥发酚
卷烟
主流烟气
GC-MS
Ultrasonic extraction
Volatile phenols
Cigarette
Mainstream smoke
Abstract
GC-MS was applied to the determination of 6 volatile phenols, i.e. phenol, o-cresol, p-cresol, m-cresol, hydroquinone, and resorcinol, in mainstream smoke of cigarettes. The total particulate matter in mainstream smoke of 5 cigarettes were trapped by Cambridge filter pad under standard smoking condition and extracted ultrasonically with methanol for 10 min. The extract was separated on DB-624 capillary column (30 m×0.25 mm, 1.4 μm). Full-scanning mode and selected ion monitoring mode were adopted in MS determination. Phenol-D5 was used as internal standard. Detection limits (3S/N) of the method found were in the range of 10-16 ng·cig-1 each cigarette and lower limits of determination (10S/N) of the method found were in the range of 28-40 ng·cig-1 each cigarette. Values of recovery found by standard addition method were in the range of 84.6%-99.1%, and values of RSD′s (n=6) were found in the range of 2.1%-6.4%.
中图分类号 O657.63 文献标志码： A 文章编号： DOI 10.11973/lhjy-hx201604009
所属栏目 工作简报
基金项目 贵州中烟工业有限责任公司科技项目(201019)
收稿日期 2015/4/13
修改稿日期
网络出版日期
作者单位点击查看
联系人作者刘剑(liuj1208@163.com)
备注姬厚伟(1978-),男,河南新乡人,工程师,硕士,主 要从事烟用材料及烟草化学分析研究。
引用该论文: JI Hou-wei,ZHANG Li,LIU Jian,LIU Na-na,HUANG Xi-juan,MAN Jie,WANG Fang,YANG Jing-guo. GC-MS Determination of 6 Volatile Phenols in Mainstream Smoke of Cigarettes with Ultrasonic Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(4): 412～416
姬厚伟,张 丽,刘 剑,刘纳纳,黄锡娟,满 杰,王 芳,杨敬国. 超声萃取-气相色谱-质谱法测定卷烟主流烟气中的6种挥发酚[J]. 理化检验－化学分册, 2016, 52(4): 412～416
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参考文献
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【2】HOFFMANN D, HOFFMANN I, EL-BAYOUMY K. The less harmful cigarette: a controversial issue. A tribute to Ernst L. Wynder［J］. Chem Res Toxicol, 2001,14(7):767-791.
【3】WALTERS D B. Monitoring phenolics in cigarette smoke condensate fractions by micro-polyamide thin-layer chromatography［J］. Journal of Analytical Toxicology, 1977,1(5):218-220.
【4】HOSHIKA Y, MUTO G. Sensitive gas chromatographic determination of phenols as bromophenols using electron capture detection［J］. J Chromatogr, 1979,179:105-111.
【5】KUWATA K, UEBORI M, YAMAZAKI Y. Reversed-phase liquid chromatographic determination of phenols in auto exhaust and tobacco smoke as p-nitrobenzeneazophenol derivatives［J］. Anal Chem, 1981,53:1531-1534.
【6】赵明月,周富臣.卷烟主流烟气中酚类物质的毛细管气相色谱分析［J］.中国烟草学报, 1992(1):1-14.
【7】毛多斌,马宇平,张峻松,等.国内外混合型卷烟主流烟气中酚类物质的分析［J］.烟草科技, 2002(4):17-20.
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【9】RISNERT C H, CASK S L. A high performante liquid chromatographic determination of major phenolic compounds in tobacco smoke［J］. J Chromat Sci, 1990,28:239-244.
【10】SNOOK M E. Spectrophotometric determination of phenol in tobacco smoke［J］. Anal Chem, 1991,339(3):199-200.
【11】陈章玉,张承明,徐若飞.快速高效液相色谱法测定卷烟主流烟气中的酚［J］.色谱, 2006,24(2):209-210.
【12】刘芳,杨柳,倪朝敏,等.超声萃取-快速HPLC法测定卷烟主流烟气中的苯酚、甲酚和苯二酚［J］.烟草科技, 2007(10):31-35.
【13】张婕,彭黔荣,杨敏,等.β-环糊精在卷烟主流烟气中简单酚类分析中的应用［J］.烟草科技, 2008(12):47-51.
【14】WU Jing-cun, RICKERT W S, MASTERS A. An improved high performance liquid chromatography-fluorescence detection method for the analysis of major phenolic compounds in cigarette smoke and smokeless tobacco products［J］. Journal of Chromatography A, 2012,1264:40-47.
【15】李中皓,唐纲岭,庞永强,等.超高效液相色谱β-环糊精流动相添加剂法分析卷烟主流烟气中7种酚类化合物［J］.色谱, 2010,28(8):790-794.
【16】杨继,杨柳,鲁媛,等.吸收瓶捕集-超高效液相色谱法测定卷烟侧流烟气中的酚类化合物［J］.分析试验室, 2010(12):105-108.
【17】颜权平,王昇,丁丽,等.二维液相色谱法测定卷烟主流烟气中的间-苯二酚及其他酚类化合物［J］.烟草科技, 2011(12):56-60.
【18】刘秀明,王庆忠.超高效液相色谱荧光法检测卷烟主流烟气中的挥发酚［J］.云南大学学报(自然科学版), 2011(增):305-309.
【19】黄朝章.超高效液相色谱快速测定卷烟主流烟气中7种挥发酚［J］.烟草科技, 2011(8):44-47.
【20】路鑫,蔡君兰,武建芳,等.全二维气相色谱-飞行时间质谱用于卷烟主流烟气中酚类化合物的表征［J］.化学学报, 2004,62(8):804-810.
【21】FOREHAND J B, DOOLY G L, MOLDOVEANU S C. Analysis of polycyclic aromatic hydrocarbons, phenols and aromatic amines in particulate phase cigarette smoke using simultaneous distillation and extraction as a sole sample clean-up step［J］. Journal of Chromatography A, 2000,898:111-124.
【22】MOLDOVEANU S C, KISER M. Gas chromatography/mass spectrometry versus liquid chromatography/fluorescence detection in the analysis of phenols in mainstream cigarette smoke［J］. Journal of Chromatography A, 2007,1141:90-97.
【23】SHA Yun-fei, HUANG Dan-ni, ZHENG Sai-jing, et al. Development of microwave-assisted headspace solid-phase microextraction followed by gas chromatography-mass spectrometry for the analysis of phenol in a cigarette pad［J］. Anal Methods, 2013,5:4655-4659.
【24】肖志翔,杨翠清,丁时超,等.卷烟主流烟气中酚类化合物的LC-MS/MS法测定［J］.湖南师范大学(自然科学学报), 2009(4):72-76.
【25】SAHA S, MISTRI R, RAY B C. A rapid and selective method for simultaneous determination of six toxic phenolic compounds in mainstream cigarette smoke using single-drop microextraction followed by liquid chromatography-tandem mass spectrometry［J］. Anal Bioanal Chem, 2013,405:9265-9272.
【26】YC/T 255-2008 卷烟 主流烟气中主要酚类化合物的测定 高效液相色谱法［S］.
【2】HOFFMANN D, HOFFMANN I, EL-BAYOUMY K. The less harmful cigarette: a controversial issue. A tribute to Ernst L. Wynder［J］. Chem Res Toxicol, 2001,14(7):767-791.
【3】WALTERS D B. Monitoring phenolics in cigarette smoke condensate fractions by micro-polyamide thin-layer chromatography［J］. Journal of Analytical Toxicology, 1977,1(5):218-220.
【4】HOSHIKA Y, MUTO G. Sensitive gas chromatographic determination of phenols as bromophenols using electron capture detection［J］. J Chromatogr, 1979,179:105-111.
【5】KUWATA K, UEBORI M, YAMAZAKI Y. Reversed-phase liquid chromatographic determination of phenols in auto exhaust and tobacco smoke as p-nitrobenzeneazophenol derivatives［J］. Anal Chem, 1981,53:1531-1534.
【6】赵明月,周富臣.卷烟主流烟气中酚类物质的毛细管气相色谱分析［J］.中国烟草学报, 1992(1):1-14.
【7】毛多斌,马宇平,张峻松,等.国内外混合型卷烟主流烟气中酚类物质的分析［J］.烟草科技, 2002(4):17-20.
【8】刘春波,陆舍铭,刘正聪,等.吹扫捕集-气相色谱法测定卷烟主流烟气中挥发酚［J］.理化检验-化学分册, 2009,45(3):349-351.
【9】RISNERT C H, CASK S L. A high performante liquid chromatographic determination of major phenolic compounds in tobacco smoke［J］. J Chromat Sci, 1990,28:239-244.
【10】SNOOK M E. Spectrophotometric determination of phenol in tobacco smoke［J］. Anal Chem, 1991,339(3):199-200.
【11】陈章玉,张承明,徐若飞.快速高效液相色谱法测定卷烟主流烟气中的酚［J］.色谱, 2006,24(2):209-210.
【12】刘芳,杨柳,倪朝敏,等.超声萃取-快速HPLC法测定卷烟主流烟气中的苯酚、甲酚和苯二酚［J］.烟草科技, 2007(10):31-35.
【13】张婕,彭黔荣,杨敏,等.β-环糊精在卷烟主流烟气中简单酚类分析中的应用［J］.烟草科技, 2008(12):47-51.
【14】WU Jing-cun, RICKERT W S, MASTERS A. An improved high performance liquid chromatography-fluorescence detection method for the analysis of major phenolic compounds in cigarette smoke and smokeless tobacco products［J］. Journal of Chromatography A, 2012,1264:40-47.
【15】李中皓,唐纲岭,庞永强,等.超高效液相色谱β-环糊精流动相添加剂法分析卷烟主流烟气中7种酚类化合物［J］.色谱, 2010,28(8):790-794.
【16】杨继,杨柳,鲁媛,等.吸收瓶捕集-超高效液相色谱法测定卷烟侧流烟气中的酚类化合物［J］.分析试验室, 2010(12):105-108.
【17】颜权平,王昇,丁丽,等.二维液相色谱法测定卷烟主流烟气中的间-苯二酚及其他酚类化合物［J］.烟草科技, 2011(12):56-60.
【18】刘秀明,王庆忠.超高效液相色谱荧光法检测卷烟主流烟气中的挥发酚［J］.云南大学学报(自然科学版), 2011(增):305-309.
【19】黄朝章.超高效液相色谱快速测定卷烟主流烟气中7种挥发酚［J］.烟草科技, 2011(8):44-47.
【20】路鑫,蔡君兰,武建芳,等.全二维气相色谱-飞行时间质谱用于卷烟主流烟气中酚类化合物的表征［J］.化学学报, 2004,62(8):804-810.
【21】FOREHAND J B, DOOLY G L, MOLDOVEANU S C. Analysis of polycyclic aromatic hydrocarbons, phenols and aromatic amines in particulate phase cigarette smoke using simultaneous distillation and extraction as a sole sample clean-up step［J］. Journal of Chromatography A, 2000,898:111-124.
【22】MOLDOVEANU S C, KISER M. Gas chromatography/mass spectrometry versus liquid chromatography/fluorescence detection in the analysis of phenols in mainstream cigarette smoke［J］. Journal of Chromatography A, 2007,1141:90-97.
【23】SHA Yun-fei, HUANG Dan-ni, ZHENG Sai-jing, et al. Development of microwave-assisted headspace solid-phase microextraction followed by gas chromatography-mass spectrometry for the analysis of phenol in a cigarette pad［J］. Anal Methods, 2013,5:4655-4659.
【24】肖志翔,杨翠清,丁时超,等.卷烟主流烟气中酚类化合物的LC-MS/MS法测定［J］.湖南师范大学(自然科学学报), 2009(4):72-76.
【25】SAHA S, MISTRI R, RAY B C. A rapid and selective method for simultaneous determination of six toxic phenolic compounds in mainstream cigarette smoke using single-drop microextraction followed by liquid chromatography-tandem mass spectrometry［J］. Anal Bioanal Chem, 2013,405:9265-9272.
【26】YC/T 255-2008 卷烟 主流烟气中主要酚类化合物的测定 高效液相色谱法［S］.
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