QuEChERS结合气相色谱-质谱联用法检测蔬菜中10种农药残留

Determination of 10 kinds of pesticides residues in vegetables by QuEChERS coupled with gas chromatography-mass spectrometry

中文关键词:  QuEChERS  气相色谱-质谱联用法  蔬菜  农药残留

英文关键词:QuEChERS  gas chromatography-mass spectrometry  vegetables  pesticide residues

中文摘要:

      目的 建立QuEChERS结合气相色谱-质谱联用法(gas chromatography-mass spectrometry, GC-MS)同时测定蔬菜中10种农药残留的分析方法。方法 样品加入乙腈后使用漩涡混合和超声波提取, 应用 QuEChERS 方法进行净化处理。浓缩定容后用GC-MS在选择离子监测模式(select ion monitoring, SIM)下进行测定, 外标法定量。结果 10种农药在0.005~1.0 μg/mL范围内线性良好, 相关系数r2均大于0.997, 方法的检出限为0.0001~0.002 mg/kg, 方法的定量限为0.0001~0.007 mg/kg。在0.02、0.05和0.1 mg/kg添加水平的回收率为62.6%~151.2%, 相对标准偏差为0.1%~6.0% (n=6)。结论 该方法简单、准确、灵敏高, 适合用于蔬菜中农药多残留的测定。

英文摘要:

      Objective To establish a method for the simultaneous determination of 10 pesticide residues in vegetables by QuEChERS combined with gas chromatography-mass spectrometry(GC-MS). Methods The samples were extracted by vortex mixing and ultrasonic wave after adding acetonitrile, and purified by the modified QuEChERS method. After concentration and dissolution, the compounds were analyzed by GC-MS under selected ion monitoring (SIM) mode. The external standard method was used for quantitative analysis. Results The 10 pesticides had good linear relationships in the range of 0.005–1.0 μg/mL, and the correlation coefficients were larger than 0.997. The detection limits of the method were 0.0001-0.002 mg/kg, the limits of quantitation were 0.0001–0.007 mg/kg. The recoveries of 10 pesticides at 0.02, 0.05 and 0.1 mg/kg levels ranged from 62.6%–151.2%, and the relative standard deviation were 0.1%–6.0% (n=6). Conclusion This method is simple, accurate and sensitive, which is suitable for detecting 10 pesticide residues in vegetables.