QuEChERS-超高效液相色谱-串联质谱法同时测定蔬菜废弃物中70种农药残留

Simultaneous determination of 70 kinds of pesticide residues in vegetable wastes by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  蔬菜废弃物  农药残留  QuEChERS  超高效液相色谱-串联质谱

英文关键词:vegetable wastes  pesticide residues  QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立一种基于QuEChERS (Quick Easy Cheap Effective Rugged and Safe)前处理技术和超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定蔬菜废弃物中70种农药残留的分析方法。方法 蔬菜废弃物样品采用QuChERS方法提取净化, UPLC-MS/MS测定, 采用电喷雾电离源扫描, 多反应监测模式检测, 基质匹配标准曲线, 外标法定量。结果 70种农药在2.0~200.0 μg/L质量浓度范围内线性关系良好, 相关系数均大于0.99; 3个添加水平(0.002、0.004和0.020 mg/kg)下的平均回收率为61.7%~109.9%, 相对标准偏差为0.4%~9.7%; 检出限为0.0001~0.0020 mg/kg, 定量限为0.0003~0.0060 mg/kg。结论 该方法简单、快速、准确、灵敏度高, 可用于大批蔬菜废弃物中农药残留快速检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 70 kinds of pesticide residues in vegetable wastes by QuChERS (Quick Easy Cheap Effective Rugged and Safe) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Vegetable wastes samples were extracted 第 3 期 杜远芳, 等: QuEChERS-超高效液相色谱-串联质谱法同时测定蔬菜废弃物中 70 种农药残留 155 and purified by QuChERS method, then the samples were detected by UPLC-MS/MS, and the electrospray ionization source was used simultaneous scanning, detected under multiple reaction monitoring mode, matrix-matched calibration curve, and quantified by external standard method. Results The 70 kinds of target pesticides exhibited great linear relationships within the concentration range of 2.0–200.0 μg/L, with linear correlation coefficients were all greater than 0.99. The average recoveries ranged from 61.7% to 109.9%, the relative standard deviations were 0.4%–9.7%, with 3 addition levels at 0.002, 0.004 and 0.020 mg/kg. The limits of detection were in the range of 0.0001 to 0.0020 mg/kg, and the limits of quantification were in the range of 0.0003–0.0060 mg/kg. Conclusion This method is easy operation, fast, accurate, and good sensitivity, which is suitable for the simultaneous detection of pesticide residues in a large number of vegetable wastes samples.