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

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...

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Bibliographic Details
Published in分析化学 Vol. 43; no. 10; pp. 1538 - 1544
Main Author 罗彦波 郑浩博 姜兴益 李雪 张洪非 朱风鹏 庞永强 冯钰锜
Format Journal Article
LanguageChinese
Published 国家烟草质量监督检验中心,郑州,450001%武汉大学化学与分子科学学院,武汉,430072 2015
Subjects
ECh
ERS方法
Qu
农药残留
凝胶渗透色谱
在线
气相色谱-串联质谱
烟叶
QuEChERS方法
农药残留
Tobacco
Pesticide residues
QuEChERS
Gas chromatography/tandem mass spectrometry
烟叶
在线
凝胶渗透色谱
On-line
气相色谱-串联质谱
Gel permeation chromatography
Online AccessGet full text
ISSN0253-3820
DOI10.11895/j.issn.0253-3820.150114

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Summary: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。
Bibliography:LUO Yan-Bo , ZHENG Hao-Bo , JIANG Xing-Yi , LI Xue , ZHANG Hong-Fei , ZHU Feng-Peng , PANG Yong-Qiang, FENG Yu-Qi（ China National Tobacco Quality Supervision and Test Center, Zhengzhou 450001, China） 2（ College of Chemistry and Molecular Science, Wuhan University, Wuhan 430072, China）
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 line
ISSN:0253-3820
DOI:10.11895/j.issn.0253-3820.150114