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土壤中13种磺酰脲类除草剂多残留的超高效液相色谱-串联质谱法测定
Determination of Multi-residues of Thirteen Sulfonylurea Herbicides in Soil by Ultra Performance Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry
【摘要】 建立了超高效液相色谱-串联质谱法同时检测土壤中13种磺酰脲类除草剂多残留量的方法。样品经磷酸缓冲液(pH7.8)-甲醇(体积比1∶1)振荡提取,Oasis HLB固相萃取小柱净化后,采用多反应监测模式测定,外标法定量。13种磺酰脲类除草剂在5~200μg/L范围内线性关系良好,相关系数为0.999 1~0.9999。13种除草剂在5、20μg/kg水平下的平均加标回收率为89%~103%,相对标准偏差为1.1%~11.2%。方法的检出限(S/N=3)为0.020~0.092μg/kg,定量下限(S/N=10)为0.07~0.31μg/kg。
【Abstract】 A UPLC-MS/MS method was established for the simultaneous determination of thirteen sulfonylurea herbicides multiresidues in soil.Samples were extracted from soil with phosphate buffer(pH 7.8)-methanol(1∶1,by volume) in oscillator and purified by Oasis HLB solid phase extraction cartridge.The extracts were determined under multiple reaction monitoring mode.The quantification was performed by the external standard method.The results indicated that the linear ranges of thirteen sulfonylureas were in the range of 5-200 μg/L,with correlation coefficients of 0.999 1-0.999 9.The average recoveries of thirteen sulfonylurea herbicides from the soil sample at two spiked levels of 5 and 20 μg/kg ranged from 89% to 103% with relative standard deviations of 1.1%-11.2%.The limits of detection(LOD) were in the range of 0.020-0.092 μg/kg,and the limits of quantitation(LOQ) were 0.07-0.31 μg/kg.
【Key words】 UPLC-MS/MS; sulfonylurea herbicide; soil; multi-residue; solid phase extraction;
- 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2010年11期
- 【分类号】X833
- 【被引频次】31
- 【下载频次】409