微波萃取-高效液相色谱法测定稻谷中敌敌畏的残留量
投稿时间:2007-11-05    点此下载全文
引用本文:汪涛,柴逸峰,范国荣,宓鹤鸣.微波萃取-高效液相色谱法测定稻谷中敌敌畏的残留量[J].药学实践杂志,2008,(3):194~196
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作者单位E-mail
汪涛 第二军医大学药学院药物分析教研室,上海200433 mhm19470718@sina.com 
柴逸峰 第二军医大学药学院药物分析教研室,上海200433  
范国荣 第二军医大学药学院药物分析教研室,上海200433  
宓鹤鸣 第二军医大学药学院药物分析教研室,上海200433  
中文摘要:目的:建立了微波辅助萃取-高效液相色谱法测定稻谷中敌敌畏残留量的方法。方法:以丙酮-乙腈(体积比3:7)为提取剂,采用微波辅助萃取稻谷中残留的敌敌畏,经弗罗里硅土及中性氧化铝柱层析净化,以乙腈-水为流动相,流速1.0 mL/min,200 nm检测。结果:敌敌畏在2.0-25.0μg/mL范围内呈良好的线性关系,检测限为0.5μg/mL,稻壳添加平均回收率为81.1%,RSD为3.9%;糙米添加平均回收率为78.9%,RSD为4.0%。结论:该方法简便、快速,可用于稻谷中敌敌畏残留量的测定。
中文关键词:微波辅助萃取  高效液相色谱法  敌敌畏  稻壳  糙米
 
Determination of dichlorovos residue in rice by microwave-assisted extraction/HPLC
Abstract:Objective: To develop a method of microwave-assisted extraction(MAE)followed by HPLC for the determination of the residue of dichlorovos in rice.Methods:Pesticide residues were extracted from rice samples with a solvent mixture.Extracts were cleaned up with a column filled with Florisil and neutral aluminum oxide.Nova-Pak C18 column(4 μm,3.9×150 mm)was used with acetonitrile:water(3070,V/V)solution as mobile phase,and the flow speed was 1.0mL/min.The ultraviolet detection wavelength was 200nm.Results:Good linear correlation for dichlorovos was found in the concentration range of 2.00-25.00 μg/mL.The detection limit was 0.5 μg/mL for dichlorovos(S/N=3).The average recovery rate of rice hull and brown rice were 81.1%(RSD3.9%) and 78.9%(RSD4.0%),respectively.Conclusion:This method is simple and rapid.It can be used for the determination of dichlorovos residue in rice with satisfactory results.
keywords:microwave-assisted extraction  HPLC  dichlorovos  rice hull  brown rice
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