超高压液相色谱串联质谱法测定小油菜中3种农药残留

Determination of abamectin,chlorantraniliprole and difenoconazole residues in rape by ultra performance liquid chromatography-tandem mass spectrometry

建立了小油菜中阿维菌素、氯虫苯甲酰胺和苯醚甲环唑3种农药残留的超高效液相色谱-串联质谱检测方法。样品经乙腈提取,SPE氨基固相萃取柱净化,超高效液相色谱-串联质谱(UPLC-MS/MS)同时进行检测。3种农药在小油菜样品中均存在程度不同的基质效应,因此,采用空白基质匹配的校准曲线外标法定量。3种农药均在0.5~500μg/L范围内具有良好的线性关系,相关系数均大于0.9996。在0.02~0.2 mg/kg范围内,平均添加回收率为84.0%~110.0%,相对标准偏差为1.2%~1.5%。阿维菌素、氯虫苯甲酰胺和苯醚甲环唑的检出限(LOD)分别为1.87,0.0115和0.0110μg/kg,定量限(LOQ)分别为6.24,0.0384和0.0366μg/kg。

An ultra performance liquid chromatography-tandem mass spectrometry（ UPLC/MS/MS）method was developed for the determination of abamectin,chlorantraniliprole and difenoconazole residues in rape. The analytes were extracted from sample with acetonitrile,and purified by a solid phase extraction（ SPE） column containing amino,and then analyzed by UPLC/MS/MS. The matrix effect was observed in the analysis of the analytes in sample. The interference of matrix was reduced which quantified by an external standard of the matrix-matched calibration standards. The linear range was from 0. 5 to 500 μg/L for abamectin,chlorantraniliprole and difenoconazole with the good coefficients（ r ! 0. 9996）. The recoveries of rape added abamectin,chlorantraniliprole and difenoconazole from 0. 02 to 0. 2 mg/kg were 84. 0 % ~ 110. 0 %,with relative standard deviations（ RSD） of 1. 2 % ~ 1. 5 %. The limits of determination（ LODs）（ S/N = 3） were 1. 87,0. 0115 and0. 0110 μg/kg,and the limits of quantification（ LOQs）（ S/N = 10） were 6. 24,0. 0384 and0. 0366 μg/kg for abamectin,chlorantraniliprole and difenoconazole,respectively.