QuEChERS-气相色谱-三重四极杆-串联质谱法测定果蔬中222种农药残留

Determination of 222 kinds of pesticide residues in vegetables and fruits by QuEChERS-gas chromatography-triple quadrupole-tandem mass spectrometry

中文关键词:  气相色谱-三重四极杆-串联质谱法  农药残留  QuEChERS  蔬菜  水果

英文关键词:gas chromatography-triple quadrupole tandem mass spectrometry  pesticide residues  QuEChERS  vegetables  fruit.

中文摘要:

      目的 建立一种QuEChERS前处理结合气相色谱-三重四极杆-串联质谱法(gas chromatography-triple quadrupole tandem mass spectrometry, GC-MS/MS)测定水果、蔬菜中222种农药残留的分析方法。方法 样品用乙腈均质提取, QuEChERS技术提取和净化, 经气相色谱分离, 用GC-MS/MS在动态多反应离子监测(dynamic multiple reaction monitoring, dMRM)模式下进行检测, 基质匹配标准溶液内标法定量。结果 220种农药在0.005~0.200 mg/L的质量浓度范围内线性关系良好, 相关系数(r2)均＞0.9900, 不同基质在0.01、0.05、 0.10 mg/kg的添加水平下216种农药的平均回收率在90%~120%之间, 相对标准偏差(relative standard deviation, RSD)为1.2%~8.9%, 方法的检出限为0.005~0.010 mg/kg, 定量限(limit of quantitation, LOQ)为0.01~0.02 mg/kg。结论 该法快速、准确、灵敏、重现性较好, 适用于大批量水果和蔬菜中农药残留的快速筛查分析。

英文摘要:

      Objective To establish a method for the rapid determination of 222 kinds of pesticide residues in vegetables and fruits by QuEChERS-gas chromatography-triple quadrupole-tandem mass spectrometry (GC-MS/MS). Methods Samples were extracted with acetonitrile, purified by QuEChERS, then separated by gas chromatography, detected by GC-MS/MS in the dynamic multi-reaction monitoring mode (dMRM). The analytes were quantified by matrix-matched standard solutions with internal standard method. Results The results showed that 222 kinds of pesticides had a good linear relationship in the range of 0.005?0.200 mg/L, and the correlation coefficients were greater than 0.9900. The average recoveries of 216 kinds of pesticides in different matrices were in the range of 90%?120% at the spiked level of 0.01, 0.05, 0.10 mg/kg, with relative standard deviations (RSDs) of 1.2%?8.9%. The limits of detection were 0.005?0.010 mg/kg, and the limits of quantification (LOQ) of the method were 0.01? 0.02 mg/kg. Conclution The method is rapid, accurate, sensitive and reproducible, and suitable for screening multiple pesticide residues in a wide variety of vegetables and fruits.