色谱

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固相萃取-高效液相色谱法测定环境水样中的三嗪类化合物

李竺 陈 玲 郜洪文 董丽娴 赵建夫   

  1. 1.State Key Laboratory of Pollution Control and Resources Reuse, Tongji University, Shanghai 200092, China; 2.Key Laboratory of Yangtze Aquatic Environment, Ministry of Education, Tongji University, Shanghai 200092, China
  • 收稿日期:2005-08-02 修回日期:2005-12-07 出版日期:2006-05-30 发布日期:1987-03-25
  • 通讯作者: 陈 玲

Determination of Triazines in Surface Water Using Solid Phase Extraction-High Performance Liquid Chromatography

LI Zhu, CHEN Ling, GAO Hongwen, DONG Lixian, ZHAO Jianfu   

  1. 1.State Key Laboratory of Pollution Control and Resources Reuse, Tongji University, Shanghai 200092, China; 2.Key Laboratory of Yangtze Aquatic Environment, Ministry of Education, Tongji University, Shanghai 200092, China
  • Received:2005-08-02 Revised:2005-12-07 Online:2006-05-30 Published:1987-03-25
  • Contact: Chen Ling

摘要: 建立了固相萃取-高效液相色谱法(SPE-HPLC)测定地表水中三嗪类化合物的方法。考察了4种不同固相萃取柱对三嗪类化合物的吸附效果,最终选择ENVI-18固相萃取柱用于萃取地表水中的三嗪类化合物;系统研究了环境水样中三嗪类化合物的最佳固相萃取条件,选择洗脱溶剂为甲醇,洗脱溶剂用量5 mL,水样在萃取前不需要添加甲醇,不调节pH值。测定了方法的检测限,结果表明,扑草净、莠去津、西玛津、脱乙基莠去津、羟基化莠去津和脱异丙基莠去津的最低检测限依次为0.14 μg/L,0.12 μg/L,0.08 μg/L,0.08 μg/L,0.10 μg/L和0.18 μg/L。将该法应用于实际环境水样的分析测定,结果表明某湖水中扑草净的含量为(9.33±0.27) μg/L,某江水中莠去津和扑草净的含量分别为(5.28±0.43) μg/L和(7.12±0.54) μg/L。

关键词: 高效液相色谱, 固相萃取, 三嗪类化合物, 预富集

Abstract: A method was developed to monitor triazines in surface water using the combination of solid phase extraction (SPE) and high performance liquid chromatography. Four different SPE cartridges were tested for extracting six triazines, including atrazine (A), simazine (S), prometryn (P), desethylatrazine (DEA), 2-hydroxyatrazine (OHA) and desisopropylatrazine (DIA), and finally ENVI-18 was selected as optimal. The method for solid phase extraction was further systematically studied for details. Optimal results of orthogonal design were determined as follows: pH 6, 5 mL methanol as eluting solvent, and no methanol added into water sample before extraction. The detection limits of six triazines were 0.14 μg/L for P, 0.12 μg/L for A, 0.08 μg/L for S, 0.08 μg/L for DEA, 0.10 μg/L for OHA and 0.18 μg/L for DIA. This method was applied for environmental aquatic samples, and the results showed that the concentration of prometryn in a lake was detected as (9.33±0.27) μg/L, as well as the concentrations of atrazine and prometryn in a river were detected as (5.28±0.43) μg/L and (7.12±0.54) μg/L respectively.

Key words: high performance liquid chromatography (HPLC), preconcentration , solid phase extraction (SPE), s-triazine compounds