浊点萃取-高效液相色谱法检测牛奶中的六种农药  被引量:21

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

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作  者:王健[1] 崔艳梅[1] 刘伟[1] 杨明敏[1] 陈建波[1] 

机构地区:[1]南京农业大学理学院,江苏南京210095

出  处:《色谱》2007年第6期853-856,共4页Chinese Journal of Chromatography

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60g/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20~10000μg/L、苯噻草胺在30~10000μg/L、苄嘧磺隆和烟嘧磺隆在50~10000μg/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%~95.74%,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。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 - 10 000 μg/L for tralkoxydim, metribuzin and bromoxynil, 30 - 10 000 μg/L for mefenacet, and 50 - 10 000 μg/L for bensulfuron-methyl and nicosulfuron. The correlation coefficients were 0. 998 1 - 0. 999 7. 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.

关 键 词:浊点萃取 高效液相色谱 除草剂 牛奶 

分 类 号:O658[理学—分析化学]

 

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