基质固相分散萃取-超高效液相色谱-串联质谱法快速测定蔬菜中的农药多残留

Simultaneous Determination of Multi-residue Pesticides in Vegetables by Matrix Solid-phase Dispersion Extraction and Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometer

[目的]建立蔬菜中17种农药多残留的超高效液相色谱一串联质谱（JPLC-MS-MS）检测方法。[方法]样品采用基质固相分散萃取技术进行提取和净化,超高效液相色谱分离、二级质谱检测器测定。[结果]17种农药在0.005~0.5 mg/L范围内线性关系良好、相关系数r≥0.999 5,检出限0.001~0.004 mg/L;添加水平在0.025~0.25 mg/kg范围内,平均添加回收率为73.44%~101.58%、相对标准偏差为0.73%~11.09%。[结论]该方法快速、准确、简便、经济、高效、安全,可用于蔬菜样品中农药多残留确证检测。

[Aims] The ultra-high performance liquid chromatography-tandem mass spectrometric （UPLC-MS/MS） method was developed for the simultaneous determination of seventeen pesticide residues in vegetables. [Methods]The samples were extracted and cleaned up by matrix solid-phase dispersion extraction, separated by UPLC and detected by mass spectrometry detector. [Results] The correlation coefficients were between 0.999 5 and 0.999 9 with the linear range of 0.005-0.5 mg/L. The limit of detection were 0.001-0.004 mg/L. When the spiked levels were between 0.025 and 0.5 mg/kg, the average recoveries of seventeen pesticides in vegetables ranged from 73.44 to 101.58% and the relative standard deviations were between 0.73 and 11.09%. [Conclusions] The method is simple, precise, cheap, high sensitivity and selectivity, which fits the determination needed for the multi residue pesticides in vegetables.