超高效液相色谱-串联质谱法测定水中双酰胺类杀虫剂的残留量

Determination of Diamide Insecticides Residues in Water by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了使用超高效液相色谱—串联质谱法(UPLC-MS/MS)测定水中5种双酰胺类杀虫剂残留量的检测方法。样品通过固相萃取柱富集后,用有机试剂洗脱,浓缩后测定。试验结果表明:在0.004~0.4mg/L范围内,氯虫苯甲酰啊等3种农药的质量浓度与相应的峰面积呈良好的线性关系,相关系数均>0.99,在0.1~5.0μg/L的添加水平下,添加回收率为85.1%~104.8%,相对标准偏差为1.7%~8.5%,定量限为0.1μg/L;在0.01~0.4mg/L范围内,环溴虫酰胺等2种农药的质量浓度与相应的峰面积呈良好的线性关系,相关系数均>0.99,在0.5~5.0μg/L的添加水平下,添加回收率为76.4%~107.9%,相对标准偏差为1.8%~10.7%,定量限为0.5μg/L。本方法简便、灵敏、准确。

A method for the determination of 5 diamide insecticides residues in water by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.Firstly,residues in water were enriched and purified by SPE cartridges.Then,the SPE cartridges were eluted with organic solvent.Finally,the samples were concentrated and determined.The results demonstrated that the concentrations of 3 pesticides including chlorantraniliprole had a good linear relationship with the corresponding peak area in the range of 0.004~0.4mg/L and the correlation coefficients were all above 0.99.The average recoveries ranged from 85.1%to 104.8%,with RSDs from 1.7%to 8.5%in the range of 0.1~5.0μg/L.The limit of quantification was 0.1μg/L.The concentrations of the other 2 pesticides including cyantraniliprole had a good linear relationship with the corresponding peak area in the range of 0.01~0.4mg/L and the correlation coefficients were all above 0.99.The average recoveries ranged from 76.4%to 107.9%,with RSDs from 1.8%to 10.7%in the range of 0.5~5.0μg/L.The limit of quantification was 0.5μg/L.The method showed good characteristics of simplicity,accuracy and time-saving.