QuEChERS结合气相色谱－负化学源质谱法测定蔬菜水果中37种农药残留

Determination of 37 pesticide residues in vegetables and fruits by QuEChERS coupled with gas chromatography-negative chemical ionization mass spectrometry

中文关键词:  果蔬  QuEChERS  农药残留  气相色谱-负化学源质谱法

英文关键词:vegetables and fruits  QuEChERS  pesticide residues  gas chromatography-negative chemical ionization

中文摘要:

      目的 建立气相色谱－负化学源质谱法(gas chromatography-negative chemical ionization, GC-MS/NCI)测定果蔬中37种农药残留量的方法。方法 蔬菜水果样品由乙腈提取、QuEChERS净化, 采用GC-MS/NCI测定, 外标法定量。结果 在20~500 μg/L范围内37种农药的线性良好(相关系数r2>0.995), 所有农药的方法定量限在0.03~0.67 μg/kg之间; 芹菜和梨在0.01 mg/kg加标水平下, 37种农药的平均回收率范围为86.2%~110%且相对标准偏差(n=6)均小于10%。结论 该方法简便、快捷、回收率及精密度好, 可以成为检测果蔬中农药残留的常规检测技术, 其建立的质谱条件也可以成为农药确证的另一手段。

英文摘要:

      Objective To establish a gas chromatography-negative chemical ionization mass spectrometry (GC-MS/NCI) method for the determination of 37 pesticide residues in fruits and vegetables. Methods The fruit and vegetable samples were extracted with acetonitrile, cleaned up with QuEChERS, detected by GC-MS/NCI, and quantified by external standard method. Results The linearity of 37 pesticides was good in the range of 20–500 μg/L (correlation coefficient r2>0.995), and the quantitative limit of all pesticides was 0.03–0.67 μg/kg. The average recoveries of 37 pesticides in celery and pear were 86.2%–110% and relative standard deviations (n=6) were less than 10% at 0.01 mg/kg standard addition level. Conclusion The method is simple, rapid, and has good recovery and precision. It can be used as a routine detection technology for pesticide residues in fruits and vegetables, and the mass spectrometry conditions established by the method can also be used as another means for pesticide confirmation.