超高效液相色谱-串联质谱法同时测定蔬菜中阿维菌素和氟吡菌酰胺的残留

Determination of Abamectin and Fluopyram Residues in VegetablesUsing Ultra-high Performance Liquid Chromatography-tandem MassSpectrometry

为建立同时测定蔬菜中阿维菌素和氟吡菌酰胺残留的超高效液相色谱-串联质谱(UPLC-MS/MS)方法,采用乙腈高速匀浆提取蔬菜样品中的阿维菌素和氟吡菌酰胺,利用无水硫酸镁和PSA吸附剂进行净化,在UPLC-MS/MS的正离子电离和多反应离子监测模式下进行测定。结果表明,阿维菌素和氟吡菌酰胺的检出限分别为1.0、0.2μg/kg;在0.005~0.200 mg/L浓度范围内,其线性相关系数均大于0.999。阿维菌素和氟吡菌酰胺在3个试验水平(0.01、0.02和1.0 mg/kg)的添加回收率分别为83%~106%和90%~108%,相对标准偏差分别在0.5%~5.2%和1.2%~8.4%。本方法前处理过程快速简单,仪器分析灵敏度好,方法准确度高,可用于蔬菜样品中阿维菌素和氟吡菌酰胺农药残留量的检测分析。

To determine the residues of abamectin and fluopyram in vegetable samples,a method was established using the ultra-high performance liquid chromatography-tandem mass spectrometry.The vegetable samples were extracted with acetonitrile and purified with MgSO4 and PSA adsorbents.The target compounds were separated by a C18 UPLC column,then detected by electro-spray ionization(ESI+)and multiple reaction monitoring(MRM)mode.Quantification was performed by peak area external standard methods using matrix-matched calibration curves.In the range of 0.005 to 0.200 mg/L with good linear relationships,the correlation coefficients were better than 0.999.The limit of detection(LOD)of abamectin and fluopyram was 1.0 and 0.2μg/kg,respectively.At 0.01 to 1.0 mg/kg spiked levels for vegetable samples,the recovery of abamectin was between 83%and 106%,and the relative standard deviation(RSD)was in range of 0.5%to 5.2%;the recovery of fluopyram was between 90%and 108%,and the relative standard deviation(RSD)was in range of 1.2%to 8.4%.This method is simple,quick,accurate,and could be applied to the determination of the four pesticides residues in vegetable samples.