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基质固相分散-气相色谱法测定农药多残留的响应面优化

Response surface optimization for determination of pesticide multiresidues by matrix solid-phase dispersion and gas chromatography.

作者信息

Hu Yan-Yun, Zheng Ping, He You-Zhao, Sheng Guo-Ping

机构信息

Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026, China.

出版信息

J Chromatogr A. 2005 Dec 9;1098(1-2):188-93. doi: 10.1016/j.chroma.2005.09.093. Epub 2005 Nov 10.

Abstract

An optimized multiresidue analysis method based on matrix solid-phase dispersion (MSPD) and gas chromatography (GC) is proposed for the determination of organochlorines and pyrethroids in the tea samples. Response surface methodology (RSM) was used to optimize the extraction conditions of MSPD, such as the sorbent type, eluent composition, dichloromethane concentration and eluting volume. Desirability function approach was employed to optimize the pesticide recoveries and matrix cleanup. Compromising the recoveries and cleanup degree, MSPD was carried out with Florisil as the sorbent and n-hexane-dichloromethane (1:1, v/v) as the eluent. The pesticide recoveries in tea samples were better than 80% spiked in the concentration range of 0.01-0.05mg/kg and the relative standard deviations were lower than 7%. The quantification limits of the pesticides were in the range of 0.002-0.06mg/kg, which were lower than the maximum residue limits of the pesticides in tea samples established by the European Union.

摘要

提出了一种基于基质固相分散(MSPD)和气相色谱(GC)的优化多残留分析方法,用于测定茶叶样品中的有机氯和拟除虫菊酯。采用响应面法(RSM)优化MSPD的萃取条件,如吸附剂类型、洗脱液组成、二氯甲烷浓度和洗脱体积。采用可取性函数法优化农药回收率和基质净化效果。在回收率和净化程度之间进行折衷,以弗罗里硅土为吸附剂,正己烷-二氯甲烷(1:1,v/v)为洗脱液进行MSPD。茶叶样品中农药的回收率在0.01-0.05mg/kg加标浓度范围内优于80%,相对标准偏差低于7%。农药的定量限在0.002-0.06mg/kg范围内,低于欧盟规定的茶叶样品中农药的最大残留限量。

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