QuEChERS-超高效液相色谱-串联四级杆质谱法快速检测番茄酱中19种常见农药残留量

摘要

Objective To develop a fast and accurate method for simultaneous determination of 19 pesticide residues in tomato paste by ultra performance liquid chromatography-tandem mass spectrometry. Methods Tomato paste was firstly dispersed by water and extracted with acetonitrile containing 1% acetic acid by ultra-sonic, and the extracts were purified by dispersive solid phase extraction using GCB and PSA as the sorbents. After centrifugation and concentrated by nitrogen flushing, samples were detected by UPLC-MS/MS.ResultsThe method showed a good linearity in the range of 0.001~0.10 mg/L for 19 pesticides withr>0.994. The recoveries were in the range of 72.2%~116.8% at 3 spiked levels of 0.010, 0.050, and 0.10 mg/kg for 19 pesticides, and the relative standard deviations (RSDs) were less than 13%. The limits of detections were in the range of 0.016~3.96μg/kg.Conclusion The method is simple, fast and reliable, with a good repeatability, which could meet the detection requirements of these 19 pesticide residues in tomato paste at home and abroad. The method is suitable for quality control and food safety risk control in factory.%目的：建立同时、快速、准确检测番茄酱中19种常见农药残留量的超高效液相色谱-串联四级杆质谱(UPLC-MS/MS)分析方法。方法番茄酱原料样品经水分散后用含1%乙酸的乙腈超声辅助提取,应用GCB和PSA 等吸附填料进行分散式固相萃取净化,离心后浓缩定容,最后使用超高效液相色谱-串联四级杆质谱仪进行定性和外标法定量。结果19种农药在0.001~0.10 mg/L浓度范围内呈现良好线性关系,r>0.994；在0.010、0.050、0.10 mg/kg三个添加浓度上回收率为72.2%~116.8%,相对标准偏差小于13%,检出限在0.016~3.96μg/kg。结论该方法操作简单,快速可靠,重复性好,可满足国内外对番茄酱中19种农药检测的要求。