色谱

色谱

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高效液相色谱-高锰酸钾氧化化学发光法测定水中的痕量苯二酚

范顺利1,2,张立科1,魏彦林2,林金明2

  

  1. 1.Henan Key Laboratory for Environmental Pollution Control, College of Chemistry and Environmental Sciences, Henan Normal University, Xinxiang 453007, China; 2.State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, the Chinese Academy of Sciences, Beijing 100085, China
  • 收稿日期:2005-03-14 修回日期:2005-11-21 出版日期:2006-03-30 发布日期:1987-06-25
  • 通讯作者: 林金明

Determination of Dihydroxybenzenes Using High Performance Liquid Chromatography with Acidic Potassium Permanganate Chemiluminescence

FAN Shunli1,2, ZHANG Like1, WEI Yanlin2, LIN Jin-Ming2

  

  1. 1.Henan Key Laboratory for Environmental Pollution Control, College of Chemistry and Environmental Sciences, Henan Normal University, Xinxiang 453007, China; 2.State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, the Chinese Academy of Sciences, Beijing 100085, China
  • Received:2005-03-14 Revised:2005-11-21 Online:2006-03-30 Published:1987-06-25
  • Contact: LIN Jinmin

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摘要：

基于酸性介质中甲酸对高锰酸钾-苯二酚氧化发光反应的增敏作用建立了高效液相色谱-化学发光柱后检测苯二酚的新方法。优化了高锰酸钾-苯二酚氧化发光反应及高效液相色谱分离苯二酚的条件,用甲醇-0.1 mmol/L β-环糊精水溶液(体积比为30∶70) 作为流动相可实现对水中3种苯二酚异构体的分离,且能与高锰酸钾-苯二酚氧化化学发光反应条件很好地偶合。对所测定的苯二酚异构体,方法的线性范围达两个数量级;以信噪比为3测得邻、间、对苯二酚的检出限(n=3)分别为:5.2,4.7,3.2 μg/L,对质量浓度均为0.10 mg/L的3种苯二酚混合溶液连续测定11次,邻、间、对苯二酚的相对标准偏差分别为2.8%,3.4%,6.5%。将该方法与固相萃取技术相结合,对河水中的痕量苯二酚进行了测定,加标回收率为92.1%~95.4%。

关键词: 苯二酚 , 高锰酸钾, 高效液相色谱, 固相萃取, 化学发光检测

Abstract:

A sensitive, selective and simple post-column chemiluminescence (CL) detection method for simultaneously determining catechol, resorcinol, hydroquinone has been developed based on high performance liquid chromatography (HPLC) coupled with CL detection using reaction of dihydroxybenzenes with acidified potassium permanganate solution with the enhancing effect of formic acid. The optimal conditions for the CL detection and HPLC separation were achieved. Dihydroxybenzene isomers were baseline separated at column temperature of 25 ℃ using a mobile phase of methanol-0.1 mmol/L β-cyclodextrin aqueous solution (30/70, v/v) with an isocratic elution program and the mobile phase matched well the CL detection. For all compounds, the linear ranges of the CL detection were about two orders of magnitude. The detection limits were 3.2 μg/L for hydroquinone, 4.7 μg/L for resorcinol and 5.2 μg/L for catechol. Combining with solid phase extraction, the proposed method was successfully applied to the determination of dihydroxybenzenes in river water. The recoveries for the three dihydroxybenzenes were 92.1%-95.4%.

Key words: chemiluminescence (CL) detection, dihydroxybenzenes , potassium permanganate, solid phase extraction (SPE), high performance liquid chromatography (HPLC)