超高效液相色谱-串联质谱法同时测定玉米及土壤中烟嘧磺隆和2甲4氯残留
Simultaneous determination of nicosulfuron and MCPA residues in corn and soil by ultraperformance liquid chromatography-tandem mass spectrometry
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摘要: 采用分散固相萃取法进行样品前处理,建立了超高效液相色谱-电喷雾串联四极杆质谱(UPLC-MS/MS)同时快速检测玉米及其土壤中烟嘧磺隆和2甲4氯残留的方法。样品经乙腈-甲酸V(乙腈):V(甲酸)=99.9:0.1提取,C18基质固相分散(DSPE)净化后,采用UPLC-MS/MS、多反应监测模式(MRM)检测,外标法定量。结果显示,烟嘧磺隆和2甲4氯进样质量浓度与峰面积间线性关系良好,在0.005～0.1 mg/kg添加水平范围内,烟嘧磺隆和2甲4氯在不同基质中的平均回收率分别为74.6%～98.0%和81.3%～100.1%,相对标准偏差(RSD)分别为1.1%～3.4%和1.7%～10.5%,定量限(LOQ)均为0.005 mg/kg。Abstract: A rapid method for the simultaneous determination of nicosulfuron and MCPA residues in corn and soil was devoloped based on dispersive solid-phase extraction and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).The samples were extracted into acetonitrile containing 0.1% formic acid and then purified on C18.The nicosulfuron and MCPA were analyzed by UPLC-MS/MS under multiple reaction monitoring mode.External standard calibration curves were used for the quantitative analysis.There were good linear correlations between the responses and concentrations of nicosulfuron and MCPA.The recoveries of nicosulfuron and MCPA in different samples were in range of 74.6%-98.0% and 81.3%-100.0% with the relative standard deviations(RSDs) of 1.1%-3.4% and 1.7%-10.5%.The limit of quantitation of this method was 0.005 mg/kg.
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