固相萃取-高效液相色谱-质谱法检测大豆中氯嘧磺隆除草剂的残留量

Determination of chlorimuron-ethyl residue in soybean by solid phase extraction-high performance liquid chromatography-mass spectrometry

实验建立了固相萃取-高效液相色谱-质谱分析检测方法,对大豆中氯嘧磺隆除草剂的残留量进行了研究。样品经甲醇-超声波提取、正己烷液-液分配、固相萃取柱净化,将处理好的样品进行液相色谱定量分析、采用液相色谱-质谱进行定性检测。实验结果表明:氯嘧磺隆在0.1～200.0mg/L范围内浓度与峰面积具有良好的线性关系,相关系数为0.9997(n=3);在2.0～100.0μg/kg范围内,加标回收率为92.6%～95.2%;RSD为1.27%～2.64%;最低检测限为10.0μg/kg(S/N=3)。本方法具有简便、快速、准确、净化效果好等特点,适用于大豆中氯嘧磺隆除草剂的残留分析检测。

A solid phase extraction-high performance liquid chromatography-mass spectrometry method was established for determination the residue of chlorimuron-ethyl herbicide in soybean.Samples were extracted by methanol with ultrasonic,then liquid-liquid partitioned with normal hexane and purified by solid phase extraction. The sample was quantitatively analyzed by high performance liquid chromatography and qualitatively analyzed by high performance liquid chromatography-mass spectrometry.Results showed that： a good linear range from 0.1- 200.0μg/L with correlation coefficient of above 0.9997 （n = 3）was obtained.The extraction recovery were 92.6% 95.2% and the relative standard deviation were 1.27%-2.64%.The limit of detection was10.0μg/kg （S/N = 3）.The described method was simple,sensitive and accurate.