QuEChERS结合UPLC-MS/MS测定菠菜中5种氨基甲酸酯类农药残留

Determination of Residues of Five Carbamate Pesticides in Spinach by Qu ECh ERS Coupled with UPLC-MS/MS

建立了基于QuEChERS技术的超高效液相色谱-串联质谱法(UPLC-MS/MS),对菠菜中的5种氨基甲酸酯类农药残留量进行测定。样品均质后,以乙腈-水(体积比50∶50)提取后,盐析离心,乙腈层用N-丙基乙二胺净化后供UPLC-MS/MS测定。采用电喷雾离子源ESI正离子模式电离,质谱多反应监测模式对目标母离子和子离子进行扫描测定。5种氨基甲酸酯类农药在0.1~20.0μg/L的基质曲线范围内呈良好线性关系,相关系数r大于0.9991,3个水平的平均加标回收率为91.0%~101.0%,方法检出限和定量限分别为0.10~0.20μg/kg和0.25~0.50μg/kg,相对标准偏差为2.15%~5.57%。该方法具有操作简便、快速高效、回收率高、灵敏度高、重复性好等优点,可用于测定菠菜中的5种氨基甲酸酯类农药残留量。

An ultra performance liquid chromatography-tandem mass spectrometry (UPL C- MS /MS) method for the determination of five carbamate pesticides in spinach was established. Samples were homogenized and extracted by ultrasonic with acetonitrile-water(50 ∶50 in volume ratio), and then salted out and purified with primary secondary amine sorbent. Under the electrospray ionization (ESI+mode), data of the target parent ions and product ions were collected with mass spectrometric multi-response monitoring scanning detection. The matrix calibration curves of five carbamate pesticides showed the good linearity within the concentrations of 0.1-20.0 μg/L with the good correlation coefficient ( r >0.999 1). The average recoveries of three spiked levels ranged from 91.0%-101.0%, while the limits of detection and limits of quantitation were 0.10-0.20 μg/kg and 0.25-0.50 μg/kg, respectively. The relative standard deviations were 2.15%-5.57%. This method has good sensitivity and high precision, which is suitable for practical determination of five carbamate pesticides in spinach.