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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
引用本文:邹月利,陶波.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[J].食品工业科技,2012,33(17):291-294.
作者姓名:邹月利  陶波
作者单位:东北农业大学理学院,黑龙江哈尔滨,150030
基金项目:哈尔滨市科技攻关计划项目(2007GG002544)
摘    要: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。

关 键 词:固相萃取  高效液相色谱-质谱法  氯嘧磺隆除草剂  残留检测

Determination of chlorimuron-ethyl residue in soybean by solid phase extraction-high performance liquid chromatography-mass spectrometry
ZOU Yue-li,TAO Bo.Determination of chlorimuron-ethyl residue in soybean by solid phase extraction-high performance liquid chromatography-mass spectrometry[J].Science and Technology of Food Industry,2012,33(17):291-294.
Authors:ZOU Yue-li  TAO Bo
Affiliation:(College of Science,Northeast Agricultural University,Harbin 150030,China)
Abstract: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~ 200.0mg/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 was 10.0μg/kg(S/N=3).The described method was simple,sensitive and accurate.
Keywords:solid phase extraction  high performance liquid chromatography-mass spectrometry  chlorimuron-ethyl herbicide  residue detection
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