在线凝胶渗透色谱-气相色谱-串联质谱联用检测烟叶中的农药残留

Determination of Pesticide Residues in Tobacco Using Modified Qu ECh ERS Procedure Coupled to On-line Gel Permeation Chromatography-Gas Chromatography /Tandem Mass Spectrometry

采用改进Qu ECh ERS方法,以石墨化炭黑/乙二胺-N-丙基键合硅烷/磁性四氧化三铁复合材料为吸附剂,对烟叶提取物进行净化,结合在线凝胶渗透色谱-气相色谱-串联质谱联用仪,建立了烟叶中10种农药残留的检测方法。优化了影响实验结果的参数,最终凝胶渗透色谱在线收集时间选取为3.30~5.30 min、磁性吸附剂用量为80 mg、净化时间为1.0 min。目标物的检出限在0.940~100 ng/L之间,线性相关系数R2≥0.9989,日内和日间相对标准偏差分别小于15.1%和19.8%,实际样品的加标回收率为68.8%~132.2%。本方法成功应用于实际烟叶样品的检测,检测结果与现行标准方法相吻合。

Magnetic graphitized carbon black / primary secondary amine / magnetite（ GCB / PSA / Fe3O4）composite material was used as modified Qu ECh ERS adsorbent for the clean-up of tobacco extract. A method for the determination of 10 pesticide residues in tobacco was proposed by coupling the modified Qu ECh ERS procedure to on-line gel permeation chromatography（ GPC）-gas chromatography / tandem mass spectrometry.Several parameters affecting the clean-up efficiency were investigated,and 3. 30- 5. 30 min of on-line GPC collection time,80 mg of adsorbent amount and 1. 0 min of clean-up time were adopted as the optimized conditions. The detection limit of the proposed method for targeted analytes ranged from 0. 940 to 100 ng / L.And the linearities of the proposed method were obtained with correlation coefficients not less than 0. 9989 for all target analytes. The relative standard deviations（ RSDs） for both intra- and inter-day were less than15. 1% and 19. 8%,respectively. The recoveries were in the range of 68. 8%- 132. 2% for real samples.The method was successfully applied to the analysis of pesticide residues in real samples,and the results were in agreement with those from the current standard method.