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分散固相萃取-高效液相色谱-质谱联用法测定水稻秸秆、糙米、稻壳和土壤中戊唑醇残留
引用本文:刘军,沈菁,刘建.分散固相萃取-高效液相色谱-质谱联用法测定水稻秸秆、糙米、稻壳和土壤中戊唑醇残留[J].分析科学学报,2010,26(1).
作者姓名:刘军  沈菁  刘建
作者单位:1. 湖北省农业科学院农业测试与科技信息中心,湖北武汉,430064
2. 湖北大学中药生物技术湖北省重点实验室,湖北武汉,430062
基金项目:农业部农药检定所农药登记残留试验项目(2007F056)
摘    要:建立了分散固相萃取-液相色谱-质谱法测定水稻秸秆、糙米、稻壳及土壤中戊唑醇残留量。方法以乙腈为萃取溶剂,N-丙基-乙二胺(PSA)为吸附剂,实现样品快速制备;在Zorbax Eclipse XDB-C18色谱柱上,以甲醇-5 mmol乙酸铵缓冲溶液(70/30,V/V)为流动相,采用电喷雾质谱检测器,选择离子监测模式,以m/z308为定量检测离子,戊唑醇保留时间在9.5 min左右,在0.005~2 mg/L范围内浓度与峰面积呈良好的线性关系,相关系数为0.9999。在4种样本中添加不同浓度戊唑醇其平均回收率在73.6%~105.8%,相对标准偏差(n=5)小于15%,检出限(S/N=5)为2.5×10-11g。该方法简单、快速、灵敏、准确。

关 键 词:戊唑醇  分散固相萃取  N-丙基-乙二胺  液相色谱-质谱法  

Determination of Tebuconazole in Straw, Rice, Rice Hull and Soil by Liquid Chromatography-Mass Spectrometry after Dispersive Solid Phase Extraction
LIU Jun,SHEN Jing,LIU Jian.Determination of Tebuconazole in Straw, Rice, Rice Hull and Soil by Liquid Chromatography-Mass Spectrometry after Dispersive Solid Phase Extraction[J].Journal of Analytical Science,2010,26(1).
Authors:LIU Jun  SHEN Jing  LIU Jian
Institution:1.Agricultural Testing Center & Information Center;Hubei Academy of AgriculturalScience;Wuhan 430064;2.Hubei Province Key Laboratory of Biotechnology ofChinese Traditional Medicine;Hubei University;Wuhan 430062
Abstract:A liquid chromatography mass(LC-MS) method was established for determination of tebuconazole in straw,rice,rice hull and soil samples by dispersive solid phase extraction using acetonitrile as extraction solvent and primary second amine(PSA) as sorbent.The HPLC conditions are as follows:Zorbax Eclipe XDB C18 column,methanol-5mmol/L acetate acid ammonium as mobile phase.Tebuconazole was detected in selected ion monitoring(SIM) mode with m/z308 for quantitation.Linear plot was obtained in the concentration of...
Keywords:Tebuconazole  Dispersive solid phase extraction  Primary secondary amine  Liquid-chromatography-mass spectrometry  
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