色谱

色谱

• 研究论文 • 上一篇    下一篇

浊点萃取-高效液相色谱法检测牛奶中的六种农药

王健,崔艳梅,刘伟,杨明敏,陈建波

  

  1. College of Science, Nanjing Agricultural University, Nanjing 210095, China
  • 收稿日期:2007-04-25 修回日期:2007-10-17 出版日期:2007-11-30 发布日期:1984-12-25
  • 通讯作者: 杨明敏

Determination of Six Pesticides in Milk Using Cloud Point Extraction-High Performance Liquid Chromatography

WANG Jian, CUI Yanmei, LIU Wei, YANG Mingmin, CHEN Jianbo   

  1. College of Science, Nanjing Agricultural University, Nanjing 210095, China
  • Received:2007-04-25 Revised:2007-10-17 Online:2007-11-30 Published:1984-12-25
  • Contact: YANG Mingmin

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摘要：

建立了应用浊点萃取法对牛奶中的残留除草剂进行萃取富集后用高效液相色谱(HPLC)检测的方法。以60 g/L的表面活性剂Tween 20或Triton X-100为萃取剂,在一定浓度的(NH4)2SO4或NaCl的存在下加热萃取。牛奶中6种不同的除草剂被胶束相富集后被HPLC分离检测。结果表明:肟草酮、嗪草酮和溴苯腈在20～10000 μg/L、苯噻草胺在30～10000 μg/L、苄嘧磺隆和烟嘧磺隆在50～10000 μg/L时其浓度和检测信号呈线性关系,相关系数为0.9981～0.9997,平均加标回收率为85.09%～96.74%,相对标准偏差为1.90%～3.98%。6种农药的定量检测限均小于国家规定的农药残留限量(MRL)。该方法简便、快速、灵敏、污染少,实际应用性好。

关键词: 除草剂, 高效液相色谱, 牛奶 , 浊点萃取

Abstract:

The feasibility of employing cloud point extraction (CPE) as extraction and preconcentration method for the recovery of herbicides from milk samples followed by high performance liquid chromatography (HPLC) analysis is demonstrated. An aqueous surfactant solution containing 60 g/L Tween 20 or Triton X-100 was heated with an appropriate concentration of (NH4)2SO4 or NaCl for the extraction of herbicides. The extract was analyzed by HPLC subsequently. Six herbicides in milk were analyzed simultaneously. The results showed that the linear dynamic ranges of detection were 20-10000 μg/L for tralkoxydim, metribuzin and bromoxynil, 30-10000 μg/L for mefenacet, and 50-10000 μg/L for bensulfuron-methyl and nicosulfuron.The correlation coefficients were 0.9981-0.9997. The average recoveries of the six herbicides ranged from 85.09% to 96.74%. The relative standard deviations for the six herbicides were in the range of 1.90%-3.98%. The limits of detection for the six pesticides were lower than the maximum residue limits (MRL) of China. The results indicate that the method is easier, faster, sensitive and produces less pollutants.

Key words: herbicide, high performance liquid chromatography (HPLC), milk , cloud point extraction (CPE)