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目的建立同时测定蔬菜中29种农药残留的检测方法。方法样品使用乙腈萃取,Carb/NH2固相萃取柱(SPE)除杂,丙酮定容。采用HP-5MS分析柱,程序升温分离,以选择离子监测方式(SIM)监测目标化合物的特征离子进行定性定量分析。对提取条件、固相萃取模式、选择淋洗溶剂、色谱条件、质谱采集方式等进行优化,并对实际样品进行分析。结果 29种农药残留的加标回收率范围在72.7%~106.6%,相对标准偏差(RSD)为4.4%~11.6%,检出限(LOD)范围0.001~0.020 mg/kg,定量限(LOQ)范围0.003~0.060 mg/kg。结论本方法有效消除色素等复杂基质的干扰,实现一次进样多组分同时分析,准确度和灵敏度好,可满足蔬菜中多组分农药残留的同时测定。
Objective To establish a method for the simultaneous determination of 29 pesticide residues in vegetables. Methods Samples were extracted with acetonitrile, Carb / NH2 solid phase extraction (SPE), and acetone. HP-5MS analytical column was used, the program was temperature-controlled and separated, and the characteristic ions of the target compounds were monitored by selective ion monitoring (SIM) for qualitative and quantitative analysis. The extraction conditions, solid-phase extraction mode, selection of elution solvent, chromatographic conditions, mass spectrometry acquisition methods were optimized, and the actual samples were analyzed. Results The spiked recoveries ranged from 72.7% to 106.6%, the relative standard deviations (RSDs) ranged from 4.4% to 11.6%. The limit of detection (LOD) ranged from 0.001 to 0.020 mg / The range of 0.003 ~ 0.060 mg / kg. Conclusions This method can effectively eliminate the interference of complex matrix such as pigment, and achieve simultaneous analysis of multiple components in one injection. The method has the advantages of good accuracy and sensitivity, and can meet the simultaneous determination of multi-component pesticide residues in vegetables.