细支卷烟中5种树苔香味物质的气相色谱-质谱法测定
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摘要
为了评价细支卷烟中树苔香味物质从烟丝向烟气的迁移情况,建立了气相色谱-质谱联用(GC-MS)选择离子法测定卷烟烟丝和烟气中苔黑酚单甲醚、苔黑酚、β-苔黑酚羧酸甲酯、苔黑酚羧酸乙酯和十六酸乙酯的检测方法。考察了萃取溶剂、萃取时间和基质效应对分析结果的影响,最终确定以乙酸乙酯作为萃取溶剂,并使用基质匹配标准溶液进行外标法定量。5个目标物在0. 02～2. 0 mg/L的质量浓度范围内线性关系良好(r~2> 0. 996)。在烟丝中,检出限(S/N=3)和定量下限(S/N=10)分别为0. 79～3. 0 ng/m L和2. 6～10. 0 ng/m L,平均加标回收率为90. 5%～103%,相对标准偏差(RSDs,n=6)为2. 3%～12%;在烟气中,检出限(S/N=3)和定量下限(S/N=10)分别为0. 60～2. 9 ng/m L和2. 0～9. 6 ng/m L,平均加标回收率为85. 6%～104%,相对标准偏差(RSD,n=6)为1. 6%～9. 3%。结果表明,该方法简便、灵敏、线性关系好,能满足卷烟烟丝和烟气中5种目标物质的测定要求。运用该方法对烟丝和烟气中5种树苔成分的含量进行测定,并评价了其由细支卷烟的烟丝向烟气的迁移率。
To evaluate the migration of treemoss flavoring compounds in slim cigarettes from cut tobaaco to tobacco smoke,a gas chromatography – mass spectrometry( GC-MS) in selected ion monitoring mode was developed for the determination of orcinol monomethyl,orcinol,methyl atratate,ethyl hexadecanoate and ethyl orsellinate in cut tobacco and tobacco smoke. The influences of solvent,extraction time and matrix effect were investigated. The tobacco sample was extracted with ethyl acetate,and quantified externally with matrix matched standard solution. Under the optimized conditions,there were good linear relationships for 5 selected analytes in the range of 0. 02-2. 0 mg/L with their correlation coefficients( r~2) larger than 0. 996. For cut tobacco,the limits of detection( LODs) and limits of quantitation( LOQs) were in the ranges of 0. 79-3. 0 ng/m L and 2. 6-10. 0 ng/m L,respectively,with spiked recoveries of 90. 5%-103% and relative standard deviations( RSDs,n = 6) of 2. 3%-12%. For tobacco smoke,LODs and LOQs were in the ranges of 0. 60-2. 9 ng/m L and 2. 0-9. 6 ng/m L,respectively,with average spiked recoveries of 85. 6%-104% and RSDs( n = 6) of 1. 6%-9. 3%. The proposed method was applied in the determination of 5 analytes in cut tobacco and tobacco smoke followed by the evaluation of the migration of treemoss components from cut tobacco to tobacco smoke. The results showed that the method was handy,sensitive and reliable,and could satisfy the requirements for the determination of the 5 analytes both in cut tobacco and tobacco smoke.
To evaluate the migration of treemoss flavoring compounds in slim cigarettes from cut tobaaco to tobacco smoke,a gas chromatography – mass spectrometry( GC-MS) in selected ion monitoring mode was developed for the determination of orcinol monomethyl,orcinol,methyl atratate,ethyl hexadecanoate and ethyl orsellinate in cut tobacco and tobacco smoke. The influences of solvent,extraction time and matrix effect were investigated. The tobacco sample was extracted with ethyl acetate,and quantified externally with matrix matched standard solution. Under the optimized conditions,there were good linear relationships for 5 selected analytes in the range of 0. 02-2. 0 mg/L with their correlation coefficients( r~2) larger than 0. 996. For cut tobacco,the limits of detection( LODs) and limits of quantitation( LOQs) were in the ranges of 0. 79-3. 0 ng/m L and 2. 6-10. 0 ng/m L,respectively,with spiked recoveries of 90. 5%-103% and relative standard deviations( RSDs,n = 6) of 2. 3%-12%. For tobacco smoke,LODs and LOQs were in the ranges of 0. 60-2. 9 ng/m L and 2. 0-9. 6 ng/m L,respectively,with average spiked recoveries of 85. 6%-104% and RSDs( n = 6) of 1. 6%-9. 3%. The proposed method was applied in the determination of 5 analytes in cut tobacco and tobacco smoke followed by the evaluation of the migration of treemoss components from cut tobacco to tobacco smoke. The results showed that the method was handy,sensitive and reliable,and could satisfy the requirements for the determination of the 5 analytes both in cut tobacco and tobacco smoke.
引文
[1] Zhao C N. Light Ind. Sci. Technol.(赵宸楠.轻工科技),2017,10:12-13.
[2] McAdam K,Eldridge A,Fearon I M,Liu C,Manson A,Murphy J,Porter A. Regul. Toxicol. Pharm.,2016,82:111-126.
[3] Sun H D. Flavor Fragrance Cosmetics(孙汉董.香料香精化妆品),1990,1:1-10.
[4] Joulain D,Tabacchi R. Flavour Fragr. J.,2009,24(3):105-116.
[5] GB/T 2760-2014. National Food Safety Standard for Uses of Food Additives. National Standards of the People's Repub-lic of China(食品安全国家标准食品添加剂使用标准.中华人民共和国国家标准).
[6] Liu Q,Mao D S,Hou C,Wang D. Tobacco Sci. Technol.(刘强,冒德寿,侯春,王笛.烟草科技),2005,3:18-21.
[7] Mao D S,Liu Q,Hou C,Wang D. Chin. J. Chromatogr.(冒德寿,刘强,侯春,王笛.色谱),2005,23(3):323.
[8] Zhu H Y,Zhuang Y D,Wan M,Zhang Y,Xiong X M. Phys. Test. Chem. Anal.:Chem. Anal.(朱怀远,庄亚东,万敏,张映,熊晓敏.理化检验-化学分册),2012,48(6):699-701,704.
[9] Manrique E,López F. Bryologist,1991,94(2):207-212.
[10] Hiserodt R D,Swijter D F H,Mussinan C J. J. Chromatogr. A,2000,888(1):103-111.
[11] Bossi R,Rastogi S C,Bernard G,Gimenez-Arnau E,Johansen J D,Lepoittevin J P,MennéT. J. Sep. Sci.,2004,27(7/8):537-540.
[12] Cui H T,Li H,Tang S Y,Liu C B,Gao X H,Li Z J,Zhang F M,Yang G Y,Jiang W,Liu Z H,Miao M M,HeP,Shen Q P. J. Instrum. Anal.(崔婷惠,李恒,唐石云,刘春波,高晓华,李振杰,张凤梅,杨光宇,蒋薇,刘志华,缪明明,何沛,申钦鹏.分析测试学报),2018,37(7):766-771.
[13] Zhang X,Liu Z H,Yang G Y,Yang L,Duan Y X,Liu C B,Chen Y K,Miu M M. J. Instrum. Anal.(张霞,刘志华,杨光宇,杨柳,段沅杏,刘春波,陈永宽,缪明明.分析测试学报),2014,33(5):545-550.
[14] Li Y G,Wu Q M,Kou T S,Zhao B,Zhang Y F,He A M,Su G S. J. Instrum. Anal.(李远根,吴穹曼,寇天舒,赵彬,张艳芳,何爱民,苏国岁.分析测试学报),2018,37(6):708-713.
[15] GB/T 6682-2008. Water for Analytical Use-Specification and Test Methods. National Standards of the People's Repub-lic of China(分析实验室用水规格和试验方法.中华人民共和国国家标准).
[16] GB/T 19609-2004. Cigarettes—Determination of Total and Nicotine-free Dry Particulate Matter Using a Routine Analy-cial Smoking Machine. National Standards of the People's Republic of China(卷烟用常规分析用吸烟机测定总粒相物和焦油.中华人民共和国国家标准).
[17] Ding Z H,Ding J K. Acta Botania Yunnanica(丁智慧,丁靖垲.云南植物研究),1990,12(1):99-106.
[18] Li B,Lin Z W,Sun H D. Acta Botania Yunnanica(李波,林中文,孙汉董.云南植物研究),1991,13(1):81-84.
[19] Guo F Q,You J,Zhong K J,Huang J G,Liang Y Z,Huang L F. J. Central South Univ.:Sci. Technol.(郭方遒,尤健,钟科军,黄建国,梁逸曾,黄兰芳.中南大学学报:自然科学版),2005,36(5):828-832.
[20] Chen X S,Bian Z Y,Tang G L,Hu Q Y. Chin. J. Chromatogr.(陈晓水,边照阳,唐纲岭,胡清源.色谱),2012,30(10):1043-1055.
[21] MatovskáK,Lehotay S J,Anastassiades M. Anal. Chem.,2005,77(24):8129-8137.
[22] Poole C F. J. Chromatogr. A,2007,1158(1):241-250.
[2] McAdam K,Eldridge A,Fearon I M,Liu C,Manson A,Murphy J,Porter A. Regul. Toxicol. Pharm.,2016,82:111-126.
[3] Sun H D. Flavor Fragrance Cosmetics(孙汉董.香料香精化妆品),1990,1:1-10.
[4] Joulain D,Tabacchi R. Flavour Fragr. J.,2009,24(3):105-116.
[5] GB/T 2760-2014. National Food Safety Standard for Uses of Food Additives. National Standards of the People's Repub-lic of China(食品安全国家标准食品添加剂使用标准.中华人民共和国国家标准).
[6] Liu Q,Mao D S,Hou C,Wang D. Tobacco Sci. Technol.(刘强,冒德寿,侯春,王笛.烟草科技),2005,3:18-21.
[7] Mao D S,Liu Q,Hou C,Wang D. Chin. J. Chromatogr.(冒德寿,刘强,侯春,王笛.色谱),2005,23(3):323.
[8] Zhu H Y,Zhuang Y D,Wan M,Zhang Y,Xiong X M. Phys. Test. Chem. Anal.:Chem. Anal.(朱怀远,庄亚东,万敏,张映,熊晓敏.理化检验-化学分册),2012,48(6):699-701,704.
[9] Manrique E,López F. Bryologist,1991,94(2):207-212.
[10] Hiserodt R D,Swijter D F H,Mussinan C J. J. Chromatogr. A,2000,888(1):103-111.
[11] Bossi R,Rastogi S C,Bernard G,Gimenez-Arnau E,Johansen J D,Lepoittevin J P,MennéT. J. Sep. Sci.,2004,27(7/8):537-540.
[12] Cui H T,Li H,Tang S Y,Liu C B,Gao X H,Li Z J,Zhang F M,Yang G Y,Jiang W,Liu Z H,Miao M M,HeP,Shen Q P. J. Instrum. Anal.(崔婷惠,李恒,唐石云,刘春波,高晓华,李振杰,张凤梅,杨光宇,蒋薇,刘志华,缪明明,何沛,申钦鹏.分析测试学报),2018,37(7):766-771.
[13] Zhang X,Liu Z H,Yang G Y,Yang L,Duan Y X,Liu C B,Chen Y K,Miu M M. J. Instrum. Anal.(张霞,刘志华,杨光宇,杨柳,段沅杏,刘春波,陈永宽,缪明明.分析测试学报),2014,33(5):545-550.
[14] Li Y G,Wu Q M,Kou T S,Zhao B,Zhang Y F,He A M,Su G S. J. Instrum. Anal.(李远根,吴穹曼,寇天舒,赵彬,张艳芳,何爱民,苏国岁.分析测试学报),2018,37(6):708-713.
[15] GB/T 6682-2008. Water for Analytical Use-Specification and Test Methods. National Standards of the People's Repub-lic of China(分析实验室用水规格和试验方法.中华人民共和国国家标准).
[16] GB/T 19609-2004. Cigarettes—Determination of Total and Nicotine-free Dry Particulate Matter Using a Routine Analy-cial Smoking Machine. National Standards of the People's Republic of China(卷烟用常规分析用吸烟机测定总粒相物和焦油.中华人民共和国国家标准).
[17] Ding Z H,Ding J K. Acta Botania Yunnanica(丁智慧,丁靖垲.云南植物研究),1990,12(1):99-106.
[18] Li B,Lin Z W,Sun H D. Acta Botania Yunnanica(李波,林中文,孙汉董.云南植物研究),1991,13(1):81-84.
[19] Guo F Q,You J,Zhong K J,Huang J G,Liang Y Z,Huang L F. J. Central South Univ.:Sci. Technol.(郭方遒,尤健,钟科军,黄建国,梁逸曾,黄兰芳.中南大学学报:自然科学版),2005,36(5):828-832.
[20] Chen X S,Bian Z Y,Tang G L,Hu Q Y. Chin. J. Chromatogr.(陈晓水,边照阳,唐纲岭,胡清源.色谱),2012,30(10):1043-1055.
[21] MatovskáK,Lehotay S J,Anastassiades M. Anal. Chem.,2005,77(24):8129-8137.
[22] Poole C F. J. Chromatogr. A,2007,1158(1):241-250.
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