HPLC-MS/MS法测定水和土壤中四氟甲醚菊酯残留量

Determination of dimefluthrin residues in water and soils by HPLC-MS/MS

采用HPLC-MS/MS法建立了一种测定水和土壤中四氟甲醚菊酯残留量的方法。通过直接提取水和土壤中的四氟甲醚菊酯,采用高效液相色谱-三重四级杆质谱联用仪,以甲醇-0.1%甲酸水溶液(体积比90∶10)为流动相,使用Eclipse Plus C18色谱柱和MSD检测器,对水和土壤中的四氟甲醚菊酯进行测定,外标法定量。结果表明,四氟甲醚菊酯在0.2~100.0μg/L质量浓度范围内具有良好的线性关系,线性相关系数为0.9993。当水中添加浓度为0.1μg/L和10.0μg/L时,四氟甲醚菊酯在不同水中的平均回收率为95.6%~107.8%,相对标准偏差为2.1%~9.8%;当土壤中添加浓度为1.0μg/kg和100.0μg/kg时,四氟甲醚菊酯在不同土壤中的平均回收率为88.0%~109.2%,相对标准偏差为1.9%~8.7%。说明该方法具有操作简单、灵敏度高、快速准确等特点,可用于水和土壤中四氟甲醚菊酯残留量的检测。

A HPLC-MS/MS method for the determination of dimefluthrin residues in water and soils was established.The dimefluthrin residues extracted directly from water and soil samples were detected using HPLC-MS/MS with methanol and 0.1%formic acid(90:10,by vol)as the mobile phase.The eclipse plus C18 column and MSD were utilized.The external standard method was used for quantification.The results showed that there was a good linear relationship between the concentrations and their responding values when the concentration of dimefluthrin was in the range of 0.2-100.0μg/L,and the linear correlation coefficient was 0.9993.The average recovery of dimefluthrin in different water samples was 95.6%-107.8%and the relative standard deviation was 2.1%-9.8%when the spiked concentration levels were 0.1μg/L and 10.0μg/L,respectively.The average recovery of dimefluthrin in different soil samples was 88.0%-109.2%and the relative standard deviation was 1.9%-8.7%when the spiked levels were 1.0μg/kg and 100.0μg/kg,respectively,which indicated that it should be an ideal method for the detection of dimefluthrin residues in water and soils with the characteristics of simple operation,high sensitivity,fast and accuracy.