色谱

色谱 ›› 2010, Vol. 28 ›› Issue (12): 1200-1203.DOI: 10.3724/SP.J.1123.2010.01200

• 技术与应用 • 上一篇    下一篇

微波辅助-顶空液相微萃取在线联用-高效液相色谱法测定环境水样中的敌敌畏

孔娜1, 邹小兵1,2*, 黄锐2,3, 夏之宁1,2, 魏欣旸1   

  1. 1. 重庆大学化学化工学院, 重庆 400030; 2. 重庆大学生物工程学院, 重庆 400030; 3. 西南政法大学刑事侦查学院, 重庆 401120
  • 收稿日期:2010-08-20 修回日期:2010-10-20 出版日期:2010-12-28 发布日期:2010-08-28
  • 通讯作者: 邹小兵,博士,讲师,主要研究方向为分析化学和药物合成. E-mail: zxbygl@yahoo.com.cn.
  • 基金资助:

    中央高校基本科研业务费项目(No. CDJXS10220004)、重庆市科学委员会自然科学基金项目(No. CSTC2008BB9266)和重庆市教育委员会科学技术研究项目(No. KJ100102).

Determination of dichlorvos in water by microwave-assisted-headspace-liquid-phase microextraction coupled with high performance liquid chromatography

KONG Na1, ZOU Xiaobing1,2*, HUANG Rui2,3, XIA Zhining1,2, WEI Xinyang1   

  1. 1. College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030, China; 2. College of Bioengineering, Chongqing University, Chongqing 400030, China; 3. College of Criminal Investigation Law, Southwest University of Political Science and Law, Chongqing 401120, China
  • Received:2010-08-20 Revised:2010-10-20 Online:2010-12-28 Published:2010-08-28

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摘要： 基于微波辅助-顶空液相微萃取联用(MAE-HS-LPME)这一样品前处理方法,采用高效液相色谱法(HPLC)对水样中的敌敌畏残留量进行了测定。对影响萃取的因素如萃取剂、微波辐射功率、萃取时间、离子强度和样品基质的pH值等进行了考察。萃取条件为: 选用二甲苯作萃取剂,萃取时间为15 min,微波辐射功率300 W,NaCl含量为5%,pH为2.5。在最佳条件下,敌敌畏的检出限(信噪比为3时)为0.96 μg/L,定量限(信噪比为10时)为3.20 μg/L,萃取富集倍数为54,实际水样的加标回收率为87.4%～103%。与传统的前处理方法相比,本方法具有简便、快速、高效、节省溶剂、选择性好、应用范围广的特点。

关键词: 敌敌畏, 顶空液相微萃取, 高效液相色谱, 环境水样, 微波辅助萃取

Abstract: A novel method for the determination of dichlorvos in environmental water samples has been developed using microwave-assisted-headspace-liquid-phase microextraction (MAE-HS-LPME) coupled with high performance liquid chromatography (HPLC). The influences of extraction parameters in the sample matrix were investigated. Under optimized experimental conditions, the detection limit (S/N=3), the quantification limit (S/N=10) and the enrichment factor of the proposed method for the target analyte were 0.96 μg/L, 3.20 μg/L and 54, respectively. The recoveries of target analyte spiked in real water samples were 87.4%~103%. The extraction performance of MAE-HS-LPME to the target analyte was also compared with liquid-liquid extraction (LLE). The results indicated that the developed method is simple, rapid, efficient, solvent-saving, highly selective and widely applicable.

Key words: dichlorvos, environmental waters, high performance liquid chromatography (HPLC), headspace-liquid-phase microextraction (HS-LPME), microwave-assisted extraction (MAE)