色谱 ›› 2016, Vol. 34 ›› Issue (11): 1120-1125.DOI: 10.3724/SP.J.1123.2016.06012

• 研究论文 • 上一篇    

悬浮固化分散液液微萃取-毛细管电泳法测定水中磺酰脲类除草剂

朱婧1, 李明昕1, 王倩1, 任琳2, 郑波1, 雍莉2, 邹晓莉1   

  1. 1. 四川大学华西公共卫生学院卫生检验与检疫系, 四川 成都 610041;
    2. 四川省疾病预防控制中心, 四川 成都 610041
  • 收稿日期:2016-06-08 出版日期:2016-11-08 发布日期:2016-11-03
  • 通讯作者: 邹晓莉
  • 基金资助:

    四川省卫生与计划生育委员会项目(14H1236).

Solidification of floating organic drop dispersive liquid-liquid microextraction combined with capillary electrophoresis for the determination of sulfonylurea herbicides in water

ZHU Jing1, LI Mingxin1, WANG Qian1, REN Lin2, Zheng Bo1, YONG Li2, ZOU Xiaoli1   

  1. 1. Department of Sanitary Technology, West China School of Public Health, Sichuan University, Chengdu 610041, China;
    2. Center for Disease Control and Prevention of Sichuan Province, Chengdu 610041, China
  • Received:2016-06-08 Online:2016-11-08 Published:2016-11-03
  • Supported by:

    Health and Family Planning Commission Project of Sichuan Province (No. 14H1236).

摘要:

建立了悬浮固化分散液液微萃取-毛细管电泳法同时测定水中磺酰脲类除草剂残留的方法。以十二醇为萃取剂、甲醇为分散剂,采用悬浮固化分散液液微萃取技术对水样进行分离提取,并结合毛细管电泳法进行测定。该方法可以有效提取、分离、检测水中残留的微量苯磺隆、吡嘧磺隆、苄嘧磺隆等9种磺酰脲类除草剂,各待测物在10.0~1000 μg/L范围内线性关系良好,相关系数r≥0.992,方法检出限为2.40~7.50 μg/L,方法精密度为6.55%~13.9%。将该方法用于实际水样的测定,取得了较满意的结果,加标回收率为82.0%~104%。该方法简便快速,适合水中磺酰脲类除草剂的同时测定。

关键词: 磺酰脲类除草剂, 毛细管电泳, 水样, 悬浮固化分散液液微萃取

Abstract:

A novel method of solidification of floating organic drop dispersive liquid-liquid microextraction for the simultaneous determination of sulfonylurea herbicides in water samples by capillary electrophoresis was established. Sulfonylurea herbicides in water samples were extracted by solidification of floating organic drop dispersive liquid-liquid microextraction using dodecanol as extractant and methanol as dispersive solvent, and were determined with capillary electrophoresis. Nine kinds of sulfonylurea herbicides such as tribenuron-methyl, pyrazosulfuron-methyl, bensulfuron-methyl and so on were detected by this method. The good linearities were obtained in the range of 10.0-1000 μg/L. The correlation coefficiencies were not less than 0.992. The method detection limits (MDLs) ranged from 2.40 to 7.50 μg/L. The relative standard derivations (RSDs) of the method were 6.55%-13.9%. The method was applied for the determination of water samples and showed satisfactory results. The spiked recoveries ranged from 82.0% to 104%. The method is quick, sensitive and suitable for the batch analysis of sulfonylurea herbicides in water samples.

Key words: capillary electrophoresis (CE), solidification of floating organic drop dispersive liquid-liquid microextraction (SFO-DLLME), sulfonylurea herbicides, water sample

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