超高效液相色谱质谱法测定水中除草剂的残留量
Determination of Residual Content of Herbicides by the Method of Ultra-high Performance Liquid Chromatography-mass Spectrometry
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摘要:目的 建立超高效液相色谱串联质谱法同时测定水中多种除草剂残留量的检测方法。方法 水样经Oasis HLB柱净化浓缩, 用乙睛洗脱, 采用1.7 μm的C18色谱柱, 用乙腈和甲酸(0.1%)水为流动相, 进行线性梯度洗脱, 并在色谱质谱条件下进行检测。结果 该方法检测30种除草剂, 加标回收率为76.2%~101.3%%, 相对标准偏差(RSD)为3.2%~9.3%之间(n=6), 最低检测限(LOQ)在0.1~1.0 μg/L间, 线性范围在0.0~200 μg/L之间。结论 该方法操作简便, 快速准确, 提高了样品检出灵敏度, 能同时检测30种除草剂的残留量。Abstract:Objectives To establish a method for detecting the residual content of several kinds of herbicides in water using ultra-high performance liquid chromatography-mass spectrometry.Methods Water sample was purified and concentrated by Oasis HLB column and then eluted by acetonitrile. The determination by chromatography-mass spectrometry was performed on 1.7 μm C18 column, using acetonitrile, formic acid(0.1%) and water as mobile phase in linear gradient elution.Results The method can detect 30 kinds of herbicides. The spiked recovery rate varied in the range from 76.2% to 101.3%, with relative standard deviation in the range of 3.2% to 9.3% (n=6). The limit of operation was 0.1~1.0 μg/L with the linear range varying in the range of 0.0 to 200 μg/L.Conclusions The method is sensitive, specific and simple in operation. It can detect the residual content of 30 kinds of herbicides at the same time.
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