在线中心切割二维液相色谱-串联质谱法(2DLC-MS/MS)测定主流烟气烟草特有亚硝胺(TSNAs)
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- 英文论文题名：On-line analysis of four tobacco-specific N-nitrosamines(TSNAs) in mainstream cigarette smoke by using heart-cutting two dimensional liquid chromatography–tandem mass spectrometry(2DLC-MS/MS)
- 论文作者：陈敏 ; 王磊君 ; 戚大伟 ; 刘百战 ; 吴达
- 英文论文作者：CHEN Mina ; WANG Leijuna ; QIDawei ; LIUBaizhan ; WU Da ; Technology R&D Center ; Shanghai Tobacco Group Co. ; Ltd.
- 年：2016
- 作者机构：上海烟草集团有限责任公司技术研发中心;
- 论文关键词：主流烟气 ; 烟草特有亚硝胺 ; 二维液相色谱 ; 液质联用 ; 中心切割
- 英文论文关键词：Mainstream Smoke ; TSNAs ; 2DLC ; LC-MS/MS ; Heart-cutting
- 会议召开时间：2016-12-01
- 会议录名称：中国烟草学会2016年度优秀论文汇编——烟草工业主题
- 语种：中文
- 分类号：TS411;O657.63
- 学会代码：ZGYG
- 学会名称：中国烟草学会
- 页数：16
- 文件大小：945k
- 原文格式：D
摘要
由于烤烟型卷烟主流烟气烟草特有亚硝胺(TSNAs)释放量较低,基质干扰相对严重、难以准确测定,本文建立了在线的中心切割二维液相色谱串联质谱法(2DLC-MS/MS)测定烟气TSNAs的方法。卷烟烟气经剑桥滤片捕集后用醋酸铵水溶液萃取后直接上样,第一维LC采用强阳离子交换色谱柱分离除杂,TSNAs段馏分经补偿流路在线稀释与中和后切割至捕集柱保留与除盐,最后经第二维反相液相色谱柱分离,三重串联四级杆在多反应检测模式下(MRM)扫描并以内标法定量。NNN、NAT、NAB和NNK的检测限分别为0.023、0.028、0.019和0.028 ng/cig),定量限为0.076、0.094、0.027和0.092 ng/cig),回收率在93.6%~108.6%之间,相对标准偏差在5.4%以内;并对市售卷烟和标准卷烟进行测试分析。新方法前处理简单,仪器自动运行,目标物几乎无干扰,方法灵敏度高,结果准确可靠,适用于卷烟尤其是烤烟型卷烟主流烟气TSNAs释放量的分析检测。
Due to low emission of tobacco-specific N-nitrosamines(TSNAs) in Virginia cigarettes and complicated matrix interference, we develop a method which appears to be high sensitive and low quantitation limit for determination of TSNAs in mainstream cigarette smoke: heart-cutting two dimensional liquid chromatography-tandem mass spectrometry(2DLC-MS/MS) system. 2DLC was performed utilizing two different separate mechanisms to clean-up the sample and minimize matrix effects on TSNAs. After mainstream cigarette smoke was collected on a cambridge filter pad, the particulate matter was extracted with 0.1M ammonium acetate aqueous solution, and injected into 2DLC-MS/MS system. The sample were separated in strong cationexchange(SCX) column first,heart-cutting to trap column with online dilution and neutralization.Then it is separated by RPLC systemafter desalination. Finally, it is the analytes were determined qualitatively and quantitatively under multi-reaction monitoring(MRM) mode and positive polarity mode. The limits of detection of NNN、NAT、NAB、NNK was 0.023、0.028、0.019和 0.028 ng/cig), spiked recoveries of NNN、NAT、NAB、NNK ranged from 93.6%~ 108.6% with RSDs within 5.4%. Main advantages of new method are fairly high selectivity, sensitivity, accuracy of results and minimum sample pre-treatment, fully automatic with almostno matrix interference. Themethod was applied perfect in determination of TSNAs in 12 market cigarette mainstream smoke and 2 standard cigarette smoke.
Due to low emission of tobacco-specific N-nitrosamines(TSNAs) in Virginia cigarettes and complicated matrix interference, we develop a method which appears to be high sensitive and low quantitation limit for determination of TSNAs in mainstream cigarette smoke: heart-cutting two dimensional liquid chromatography-tandem mass spectrometry(2DLC-MS/MS) system. 2DLC was performed utilizing two different separate mechanisms to clean-up the sample and minimize matrix effects on TSNAs. After mainstream cigarette smoke was collected on a cambridge filter pad, the particulate matter was extracted with 0.1M ammonium acetate aqueous solution, and injected into 2DLC-MS/MS system. The sample were separated in strong cationexchange(SCX) column first,heart-cutting to trap column with online dilution and neutralization.Then it is separated by RPLC systemafter desalination. Finally, it is the analytes were determined qualitatively and quantitatively under multi-reaction monitoring(MRM) mode and positive polarity mode. The limits of detection of NNN、NAT、NAB、NNK was 0.023、0.028、0.019和 0.028 ng/cig), spiked recoveries of NNN、NAT、NAB、NNK ranged from 93.6%~ 108.6% with RSDs within 5.4%. Main advantages of new method are fairly high selectivity, sensitivity, accuracy of results and minimum sample pre-treatment, fully automatic with almostno matrix interference. Themethod was applied perfect in determination of TSNAs in 12 market cigarette mainstream smoke and 2 standard cigarette smoke.
引文
[1]Hecht S.S.,Biochemistry,biology,and carcinogenicity of tobacco-specific N-nitrosamines,Chem.Res.Toxicol.1998(11):599–603.
[2]Ei-bayouny K,Iatropoulos M,Amin S,Increased expression of cyclooxygenase in rat lung tumors induce by the tobacco-specific nitrosamine4-(Methylnitrosamine)-4-(3-pyridyl)-1-buta-none:The impact of a high-fat diet[J].Cancer Res,1999(59):1400-1403.
[3]毛友安,魏新亮,钟科军,等.烟草特有亚硝胺分析方法研究进展[J],烟草科技,2004(7):33-35.
[4]Neurath G,Pirmann B,Wichem H.Zur Frage der N-Nitrosoverbindungenim Tabakrauch[J].Beitr.Tabak Int,1964(2);311-319.
[5]Neurath G,Pirmann B,Luttich W.Zurfrage der N-Nitrosoverbindungenim Tabakrauch,Ⅱ[J].Beitr Tabak Int,1965,(3);251-262.
[6]Morie G P,Sloan C H.Determination of N–nitrosodimethylamine in the smoke of high-nitrate tobacco cigarettes[J].Beitr Tabakforsch Int.,1973(7):61-66.
[7]Hoffmann D,Hecht S S,Ornaf R M,N’-Nitroso-nornicotine in tobacco[J].Science,1974(186):265-267.
[8]谢复炜,金永明,赵明月,国内外主要品牌卷烟主流烟气中烟草特有N-亚硝胺的对比分析[J].中国烟草学报,2004(10):8-15.
[9]K.D.,Brunnemann,D.Hoffmann,Analytical studies on N-nitrosamines in tobacco and tobacco smoke,American Health Foudation,Valhalla,New York 10595,71-112.
[10]Determination of Nitrosamines in Mainstream Tobacco Smoke,Health Canada-Official Method T-111,1999,1-9.
[11]顾文博,周宛虹,陆怡峰,林华清,吴达,气相色谱-三重四极杆串联质谱法测定卷烟烟气中的烟草特有亚硝胺,烟草科技,2013(10):40-44。
[12]Wagner,K.A.,N.H.Finkel,J.E.Fossett,and I.G.Gillman:Development of a quantitative method for the analysis of tobacco-specific nitrosamines in mainstream cigarette smoke using isotope dilution liquid chromatography/electrospray ionization tandem mass spectrometry;Anal.Chem.2005(77):1001–1006.
[13]Determination of Tobacco Specific Nitrosamines in Mainstream Cigarette Smoke by LC-MS/MS,CORESTA Recommended Method N°75,July 2014.
[14]UK SMOKE Part 8:Determination of March 2003 CONSTITUENTS STUDY Tobacco Specific Nitrosamines Yields in Cigarette Smoke.March 2003.
[15]Determination of tobacco-specific nitrosamines in mainstream smoke,British American Tobacco Group Research&Development,1-8.
[16]Baker R.R.A review of pyrolysis studies to unravel reaction steps in burning tobacco[J].J Anal Appl Pyrol,1987,11:555-573.
[17]Torikai K,Yoshida S,Takahashi H.Effects of temperature,atmosphere and p H on the generation of smoke compounds during tobacco pyrolysis[J].Food Chem Toxicol,2004,42(9):1409-1417.
[18]Jie Zhang,Ruoshi Bai,Xiaoli Yi,Zhendong Yang,Xingyu Liu,Jun Zhou,Wei Liang,Fully automated analysis of four tobacco-specifi c N-nitrosamines in mainstream cigarette smoke using two-dimensional online solid phase extraction combined with liquid chromatography–tandem mass spectrometry,Talanta,2016(146)216-224.
[19]Baizhan Liu,Wei Yao,Qingde Su,Racemization of S-(-)-nicotine during smoking and its relationship with pyrolysis process,J.Anal.Appl.Pyrolysis,2008,81(2):157-161.
[20]Baizhan Liu,Chaoying Chen,Da Wu,Qingde Su,Enantiomeric analysis of anatabine,nornicotine and anabasine in commercial tobacco by multi-dimensional gas chromatography and mass spectrometry,J.Chromatogr.B,2008(865):1213-1217.
[21]Jibao Cai,Baizhan Liu,Ping Lin,Qingde Su,Fast analysis of nicotine related alkaloids in tobacco and cigarette smoke by megabore capillary gas chromatography,J.Chromatogr.A,2002(947):267-275.
[22]Robert E.Murphy,Mark R.Schure,and Joe P.Foley,Effect of Sampling Rate on Resolution in Comprehensive Two-Dimensional Liquid Chromatography,Anal.Chem.1998(70):1585-1594.
[23]Giddings J.C.Two-dimensional separations-concept and promise.Anal.Chem.,1984(56):1258-1261.
[24]Wang SW,Wang C,Zhao X,Mao SL,Wu YT,Fan GR.Comprehensive two-dimensional high performance liquid chromatography system with immobilized liposome chromatography co lumn and monolithic column for separation of the traditional Chinese medicine Schisandrachinensis.Anal Chim Acta,2012(713):121-129.
[25]Dück R,Sonderfeld H,Schmitz OJ.A simple method for the determination of peak distribution in comprehensive two-dimensional Liquid chromatography.J Chromatogr A,2012(1246):69–75.
[26]王芳,陈再根,张威,唐纲岭,刘惠民,卷烟常规分析用吸烟机测定总粒相物和焦油,GB/T 19609-2004。
[2]Ei-bayouny K,Iatropoulos M,Amin S,Increased expression of cyclooxygenase in rat lung tumors induce by the tobacco-specific nitrosamine4-(Methylnitrosamine)-4-(3-pyridyl)-1-buta-none:The impact of a high-fat diet[J].Cancer Res,1999(59):1400-1403.
[3]毛友安,魏新亮,钟科军,等.烟草特有亚硝胺分析方法研究进展[J],烟草科技,2004(7):33-35.
[4]Neurath G,Pirmann B,Wichem H.Zur Frage der N-Nitrosoverbindungenim Tabakrauch[J].Beitr.Tabak Int,1964(2);311-319.
[5]Neurath G,Pirmann B,Luttich W.Zurfrage der N-Nitrosoverbindungenim Tabakrauch,Ⅱ[J].Beitr Tabak Int,1965,(3);251-262.
[6]Morie G P,Sloan C H.Determination of N–nitrosodimethylamine in the smoke of high-nitrate tobacco cigarettes[J].Beitr Tabakforsch Int.,1973(7):61-66.
[7]Hoffmann D,Hecht S S,Ornaf R M,N’-Nitroso-nornicotine in tobacco[J].Science,1974(186):265-267.
[8]谢复炜,金永明,赵明月,国内外主要品牌卷烟主流烟气中烟草特有N-亚硝胺的对比分析[J].中国烟草学报,2004(10):8-15.
[9]K.D.,Brunnemann,D.Hoffmann,Analytical studies on N-nitrosamines in tobacco and tobacco smoke,American Health Foudation,Valhalla,New York 10595,71-112.
[10]Determination of Nitrosamines in Mainstream Tobacco Smoke,Health Canada-Official Method T-111,1999,1-9.
[11]顾文博,周宛虹,陆怡峰,林华清,吴达,气相色谱-三重四极杆串联质谱法测定卷烟烟气中的烟草特有亚硝胺,烟草科技,2013(10):40-44。
[12]Wagner,K.A.,N.H.Finkel,J.E.Fossett,and I.G.Gillman:Development of a quantitative method for the analysis of tobacco-specific nitrosamines in mainstream cigarette smoke using isotope dilution liquid chromatography/electrospray ionization tandem mass spectrometry;Anal.Chem.2005(77):1001–1006.
[13]Determination of Tobacco Specific Nitrosamines in Mainstream Cigarette Smoke by LC-MS/MS,CORESTA Recommended Method N°75,July 2014.
[14]UK SMOKE Part 8:Determination of March 2003 CONSTITUENTS STUDY Tobacco Specific Nitrosamines Yields in Cigarette Smoke.March 2003.
[15]Determination of tobacco-specific nitrosamines in mainstream smoke,British American Tobacco Group Research&Development,1-8.
[16]Baker R.R.A review of pyrolysis studies to unravel reaction steps in burning tobacco[J].J Anal Appl Pyrol,1987,11:555-573.
[17]Torikai K,Yoshida S,Takahashi H.Effects of temperature,atmosphere and p H on the generation of smoke compounds during tobacco pyrolysis[J].Food Chem Toxicol,2004,42(9):1409-1417.
[18]Jie Zhang,Ruoshi Bai,Xiaoli Yi,Zhendong Yang,Xingyu Liu,Jun Zhou,Wei Liang,Fully automated analysis of four tobacco-specifi c N-nitrosamines in mainstream cigarette smoke using two-dimensional online solid phase extraction combined with liquid chromatography–tandem mass spectrometry,Talanta,2016(146)216-224.
[19]Baizhan Liu,Wei Yao,Qingde Su,Racemization of S-(-)-nicotine during smoking and its relationship with pyrolysis process,J.Anal.Appl.Pyrolysis,2008,81(2):157-161.
[20]Baizhan Liu,Chaoying Chen,Da Wu,Qingde Su,Enantiomeric analysis of anatabine,nornicotine and anabasine in commercial tobacco by multi-dimensional gas chromatography and mass spectrometry,J.Chromatogr.B,2008(865):1213-1217.
[21]Jibao Cai,Baizhan Liu,Ping Lin,Qingde Su,Fast analysis of nicotine related alkaloids in tobacco and cigarette smoke by megabore capillary gas chromatography,J.Chromatogr.A,2002(947):267-275.
[22]Robert E.Murphy,Mark R.Schure,and Joe P.Foley,Effect of Sampling Rate on Resolution in Comprehensive Two-Dimensional Liquid Chromatography,Anal.Chem.1998(70):1585-1594.
[23]Giddings J.C.Two-dimensional separations-concept and promise.Anal.Chem.,1984(56):1258-1261.
[24]Wang SW,Wang C,Zhao X,Mao SL,Wu YT,Fan GR.Comprehensive two-dimensional high performance liquid chromatography system with immobilized liposome chromatography co lumn and monolithic column for separation of the traditional Chinese medicine Schisandrachinensis.Anal Chim Acta,2012(713):121-129.
[25]Dück R,Sonderfeld H,Schmitz OJ.A simple method for the determination of peak distribution in comprehensive two-dimensional Liquid chromatography.J Chromatogr A,2012(1246):69–75.
[26]王芳,陈再根,张威,唐纲岭,刘惠民,卷烟常规分析用吸烟机测定总粒相物和焦油,GB/T 19609-2004。
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