高效液相色谱_____高效液相色谱，芳胺，在线固相萃取

在线固相萃取和高效液相色谱法测定卷烟主流烟气中几种芳胺

http://www.100md.com 《分析化学》 2006年第5期

高效液相色谱,,高效液相色谱，芳胺，在线固相萃取,摘要,关键词,1引言,2实验部分,3结果与讨论,References

     摘要

    研究了用在线固相萃取富集和高效液相色谱法测定卷烟主流烟气中的几种芳胺 (苯胺、对甲基苯胺、2,4二甲基苯胺、1萘胺、2萘胺和4氨基联苯)的方法，样品中的芳胺用邻甲氧基酚衍生生成偶氮染料，偶氮染料用Waters XterraTM RP18色谱柱在线固相萃取富集，然后以Waters XterraTM RP18色谱柱为固定相，75%的甲醇(内含0.01 mol/L pH=8的四氢吡咯醋酸缓冲液)为流动相分离，二极管矩阵检测器检测；苯胺、对甲基苯胺、2,4二甲基苯胺、4氨基联苯、1萘胺、2萘胺的检出限分别为005、0.08、0.08、0.06、0.03和0.03 μg/L。几种芳胺的相对标准偏差在2.2%~3.4%之间；标准回收率在89%～106%之间，方法用于卷烟主流烟气中几种芳胺的测定，结果令人满意。

     关键词 高效液相色谱，芳胺，在线固相萃取

    Study on Determination of Aromatic Amine in Mainstream Tobacco Smoke by Online Solid Phase Extraction and High Performance Liquid Chromatography

    Cheng Zhangyu1，2, Yang Guangyu2, Miao Mingming2, Su Qingde1

    1(School of Chemistry & Material Science, University of Science & Technology of China Hefei 230026)

    2(Laboratory of Chemistry, Yunnan Academy of Tobacco Science, Kunming 650106)

    Abstract A new method for the determination of aromatic amines (aniline, pmethylaniline, 2,4dimethylaniline, 4aminobiphenyl, 1naphthylamine, 2naphthylamine) in mainstream tobacco smoke by online solid phase extraction and high performance liquid chromatography was described. The aromatic amines were precolumn derived with omethoxyphenol to form azo dyes. The azo dyes were enriched by online solid phase extraction with Waters XterraTM RP18(3.9 mm×20 mm, 5 μm), and separated on a Waters XterraTM RP18 chromatographic column (3.9 mm×150 mm, 5 μm), with 75% methanol (containing 0.01 mol/L pyrrolidineacetic acid buffer salt (pH=8)) as mobile phase at rate of 0.5 mL/min. Each aromatic amine was monitored at its maximum absorption wavelength with photodiode array detector. The detection limits of aniline, pmethylaniline, 2,4dimethylaniline, 4aminobiphenyl, 1naphthylamine, 2naphthylamine are 005 ......

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