QuEChERS净化-高效液相色谱串联质谱法测定菠菜中16种农药残留

Determination of 16 Pesticides in Spinach by QuEChERS-HPLC-MS/MS

采用高效液相色谱-串联质谱联用仪(HPLC-MS/MS)技术建立了同时检测菠菜中16种农药多残留的快速检测方法。样品经过QuEChERS法提取净化,以Agilent Eclipse Plus C18色谱柱分离,0.1%甲酸水-甲醇乙腈(1:1)作为液相色谱流动相进行梯度洗脱,多反应监测模式进行定量分析。考察了不同净化剂的净化效果,研究了菠菜样品的基质效应。结果表明:16种农药在0.01~0.10μg/mL浓度范围内均具有良好的线性关系,相关系数均大于0.996。对高、中、低3个不同加标浓度的平均回收率均在82.3%~104.2%,相对标准偏差RSD(n=6)小于11.8%,且在菠菜样品基质中,16种目标农药均为弱基质效应。因此该方法简单、快速、准确度高,灵敏可靠,可满足菠菜中16种农药多残留检测要求。

An high performance liquid chromatography-tandem mass spectrometric method (HPLC-MS/MS) has been developed for the simultaneous determination of 16 kinds of pesticide residues in Spiniach. After purification with QuEChERS method, the analytes were analyzed by HPLC-MS/MS on an Agilent Eclipse Plus C18 column with a mixture of 0.1% formic acid-acetonitrile and methanol(1:1)as mobile phase by fradient elution. The mass spectrometer was opertated in multiple reactions monitoring (MRM) mode in positive or negative mode. The purifying effects of different purifying agent and the matrix effects of Spinach were studied. The 16 pesticides had good linearities in the range of 0.01~0.10 μg/mL, with correlation coefficient not less than 0.996. The average recoveries at low, intermediate and high concentration levels were in the range of 82.3%~104.2%, with relative standard deviations (RSDs) not more than 11.8%, and in the sample matrix, it was showed weak matrix effect for 16 pesticides. The method is simple, efficient, accurate, reliable and sensitive, and was satisfied the requirements for detection of 16 pesticides in spinach.