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卷烟主流烟气中氨释放量离子色谱测定方法的改进
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摘要
为了准确测定卷烟主流烟气中氨的释放量,解决使用CS12A色谱柱分离时干扰物的共流出问题和使用CS16柱分离时样品溶液中的一些强保留成分不易洗脱的缺点,对卷烟主流烟气中氨释放量的分析方法进行了研究和改进,建立了一种采用CS19柱测定卷烟主流烟气中氨的离子色谱(IC)分析方法。结果表明:方法的线性相关系数大于0.999,检出限为0.05μg/支,相对标准偏差为5.2%(n=5),加标回收率在92.3%~109.0%之间。样品溶液中的Na~+、甲胺离子、乙胺离子与NH_4~+的分离度良好,能够满足卷烟主流烟气中氨释放量的测定要求,烟气中的烟碱等强保留成分也能在短时间内洗脱下来,避免了色谱柱污染和对后续测定的干扰。该方法解决了采用CS12A和CS16柱分离时NH_4~+的色谱峰拖尾和强保留成分的干扰问题,适用于卷烟主流烟气中氨释放量的准确测定。
In order to determine the ammonia delivery in mainstream cigarette smoke accurately, an ion chromatography method is developed. This method uses a Dionex Ion Pac CS19 column to separate ammonium from other analytes, instead of Dionex Ion Pac CS12 A or CS16. The new method achieves better resolution of ammonium from sodium, methylamine and ethylamine present in mainstream cigarette smoke when compared to the method with CS12 A. When CS16 column is used to separate ammonium from other cationic species, some constituents in cigarette smoke(e.g., nicotine) can be adsorbed to ion chromatographic column strongly, affect separation or contaminate analytical column. This problem is also well resolved in the new method. The spiked recoveries for this method are in the range of 92.3% ~ 109.0%, and the linear correlative coefficients are better than 0.999. The relative standard deviation(RSD) and detection limit are 5.2%(n=5) and 0.05 μg/cig, respectively. The results of experiment show that the method can meet the requirements of determination of ammonia delivery in mainstream cigarette smoke.
引文
[1]牟世芬,刘克纳,丁晓静.离子色谱方法及应用[M].2版.北京.:化学工业出版社,2012:8 12.MOU Shifen,LIU Kena,DING Xiaojing.Ion chromatographic method and Its application,2nd ed.,Beijing:Chemical Industry Press,2005:8-12.
    [2]谢剑平,刘惠民,朱茂祥,等.卷烟烟气危害性指数研究[J].烟草科技,2009(2):5 15.XIE Jianping,LIU Huimin,ZHU Maoxiang,et al.Development of a novel hazard index of mainstream cigarette smoke and its application on risk evaluation of cigarette products[J].Tobacco Science&Technology,2009,(2):5-15.
    [3]Philip Morris USA Confidential Method M 12 A:1997.Analysis of mainstream smoke for total ammonia[S].
    [4]Health Canada-Official Method T 101:1999.Determination of ammonia in mainstream cigarette smoke[S].
    [5]UK Smoke Constitute Study,Part 5 Method:2003.Determination of Ammonia yields in mainstream cigarette smoke using the Dionex DX 500 ion chromatograph[R].
    [6]Huang C B,Bassfield R,Dabney B,et al.Determination of total ammonia in mainstream smoke[J].Beitr?ge zur Tabakforschung Intermational,2003,20(6):389 393.
    [7]王希琴.离子色谱在烟草与烟气分析中的应用研究[D].合肥.:中国科学技术大学,2005:25 41.WANG Xiqin.Study on application of ion chromatographic method in analysis of tobacco and cigarette smoke[D].Hefei:University of Science and Technology of China,2005:24-41.
    [8]彭慧敏.离子色谱法在卷烟主流烟气有害成分分析中的应用[D].长沙.:中南大学,2007:48 57.PENG Huimin.Application of ion chromatography in analysis of harmful components in mainstream cigarette smoke[D].Changsha:Central South University,2007:48-57.
    [9]British American Tobacco Group Research&Development Method:2008.Determination of ammonia in mainstream smoke[S].
    [10]Intorp M,Purkis S,Whittaker M,et al.Determination of“Hoffmann Analytes”in Cigarette Mainstream Smoke.The CORESTA 2006 Joint Experiment[J].Beitr?ge zur Tabakforschung Intermational,2009,23(4):161 202.
    [11]赵晓东,谢复炜,赵乐,等.国内外卷烟主流烟气中氨的分析比较[J].中国烟草学报,2010,16(5):1 5.ZHAO Xiaodong,XIE Fuwei,ZHAO Le,et al.Comparison of ammonium in mainstream smoke from demestic and foreign cigarettes[J].Acta Tabacaria Sinica,2010,16(5):1-5.
    [12]YC/T 377-2010卷烟主流烟气中氨的测定离子色谱法[S].YC/T 377-2010 Cigarettes-Determination of ammonia in mainstream cigarette smoke-Ion chromatography method[S].
    [13]张霞,许永,刘巍,等.离子色谱法测定卷烟主流烟气中氨含量的不确定度评定[J].化学分析计量,2011,20(4):16 19.ZHANG Xia,XU Yong,LIU Wei,et al.Evaluation of uncertainty in the determination of ammonia in cigarette mainstream smoke by ion chromatography[J].Chemical Analysis and Meterage,2011,20(4):16-19.
    [14]马雁军,易小丽,李娜,等.改进的离子色谱法用于卷烟主流烟气中氨的测定[J].中国烟草学报,2012,18(4):1 9.MA Yanjun,YI Xiaoli,LI Na,et al.Determination of ammonia in mainstream cigarette smoke by an improved method of ion chromatography[J]:Acta Tabacaria Sinica,2012,18(4):1-9.
    [15]施文庄,马青,曾静.离子色谱法测定卷烟主流烟气中氨含量的方法改进[J].烟草科技,2012(10):41 45.SHI Wenzhuang,MA Qing,ZENG Jing.Improvement of ion chromatographic method for determination of ammonis in mainstream cigarette smoke[J].Tobacco Science&Technology,2012,(10):41-45.
    [16]徐袆然,薛景娇,贺宾,等.离子色谱法测定卷烟烟气中氨[J].理化检验.:化学分册,2010,46(10):1152 1157.XU Yiran,XUE Jingjiao,HE Bin,et al.Determination of ammonia in mainstream of cigarette smoke by ion chromatography[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2010,46(10):1152-1157.
    [17]王颖,张威,胡清源,等.卷烟主流烟气中氨测定方法的改进及不同抽吸模式下的氨释放量比较[J].烟草科技,2012(7):50 53.WANG Ying,ZHANG Wei,HU Qingyuan,et al.Improvement of determination of ammonis in mainstream cigarette smoke and comparison of ammonia deliveries under different smoke regimes[J].Tobacco Science&Technology,2012,(7):50-53.
    [18]GB/T 16450-2004常规分析用吸烟机定义和标准条件[S].GB/T 16450-2004 Routine analytical cigarette-smoking machine-definitions and standard conditions[S].
    [19]Thermo Fisher Scientific Inc.Dionex Ion Pac CS19 Column Product Manual[EB/OL].[2015 04 27].http://www.dionex.com/en-us/index.html.
    [20]Thermo Fisher Scientific Inc.Dionex Ion Pac CS12A Column Product Manual[EB/OL].[2014 10 11].http://www.dionex.com/en-us/index.html.
    [21]Thermo Fisher Scientific Inc.Dionex Ion Pac CS16 Column Product Manual[EB/OL].[2014 11 23].http://www.dionex.com/en-us/index.html.
    [22]刘伟,张艳芳,李杰辉,等.离子色谱法测定卷烟侧流烟气中的甲胺和乙胺[J].烟草科技,2015,48(2):32 36,74.LIU Wei,ZHANG Yanfang,LI Jiehui,et al.determination of methylamine and ethylamine in sidestream cigarette smoke by ion chromatography[J].Tobacco Science&Technology,2015,48(2):32-36,74.

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