枪头式分散固相微萃取柱方法结合气相色谱-串联质谱测定果蔬中9种农药多残留

Determination of 9 kinds of pesticide residues in fruits and vegetables using disposable pipette extraction and gas chromatography–tandem mass spectrometry

中文关键词:  枪头式分散固相微萃取柱方法  气相色谱-串联质谱法  农药残留  水果  蔬菜

英文关键词:dispersive pipette extraction  gas chromatography-tandem mass spectrometry  pesticide residue  fruits  vegetables

中文摘要:

      目的 建立枪头式分散固相微萃取柱(disposable pipette extraction, DPX)结合气相色谱-串联质谱法同时测定番茄、苹果、小青菜3种水果蔬菜中的9种农药残留的方法。方法 水果蔬菜样品经均质, 乙腈抽提, 采用DPX-RP枪头式分散固相微萃取柱进行净化。采用气相色谱-串联质谱法-多反应模式监测(multiple reaction monitoring, MRM)测定, 内标法定量。结果 9种农药化合物在10~800 μg/kg浓度范围内呈现良好的线性关系, 相关系数均大于0.995, 方法的检出限为0.3~4.7 μg/kg, 定量限为1.2~13.5 μg/kg。分别在番茄、苹果、小青菜中添加水平为50、250、500 μg/kg的混标, 平均回收率为72.8%~115.9%, 方法的相对标准偏差(relative standard deviation, RSD)为0.29%~9.9%, 通过与DPX多通道半自动前处理仪结合使用可在10 min内净化处理1~48个样品, 有效缩短了样品前处理的时间。结论 本方法简便、省时, 并且高通量, 适用于水果蔬菜中农药残留的测定。

英文摘要:

      Objective To establish a method for the determination of 9 pesticide and fungicide residues in tomato, apple and green lettuce by dispersive pipette extraction (DPX) technology with gas chromatography tandem mass spectrometry (GC-MS/MS). Methods Fruit and vegetable samples were extracted with acetonitrile solution. And then the extracts were purified and concentrated by DPX-RP tips. The extracts were analyzed with GC-MS/MS and quantified by internal standard method. Results The 9 pesticides had good linear relationships in the range of 10?800 μg/kg, and coefficients of determination were greater than 0.995. The limits of detection were 0.3?4.7 g/kg and limit of quantitation were 1.2?13.5 g/kg. The average recoveries from spiked tomato, apple and green lettuce sample matrices at three concentration levels of 50, 250, 500 μg/kg varied from 72.8% to 115.9%, with the relative standard deviations of 0.29%?9.9%. The extraction of 1?48 samples was less than 10 min using DPX tips with a semi-automated level extractor. Conclusion This method is rapid, accurate, time-saving, high-throughput, which is suitable for the analysis of pesticide residues in fruit and vegetable samples.