Development of New Capillary Separation and Extraction Methods for Analysis of Complicated Biological and Environmental Samples

博士 === 國立成功大學 === 化學系 === 88 === Accelerated solvent extraction (ASE) and capillary electrophoresis are two new techniques which are developing popular recently in analytical chemistry. For the former, the extraction is achieved at high temperature and pressure in short time. Well recoveries are fou...

Full description

Bibliographic Details
Main Authors: WeiChao Lin, 林維炤
Other Authors: Chun-Hsiung Kuei
Format: Others
Language:zh-TW
Published: 2000
Online Access:http://ndltd.ncl.edu.tw/handle/60023611173143893414
Description
Summary:博士 === 國立成功大學 === 化學系 === 88 === Accelerated solvent extraction (ASE) and capillary electrophoresis are two new techniques which are developing popular recently in analytical chemistry. For the former, the extraction is achieved at high temperature and pressure in short time. Well recoveries are found in a lot of studies compared with traditional extraction technique. This technique is not only saving time but also decreasing the solvent consumption. For the later, the chromatographic separation was performed at high electric field. The theoretic plate is high enough to give a well separatiion efficiency. The extraction of heavy metal in environmental solid matrix was investigated in this study. Three topics were composed of this study. The first is to study the extraction of three metal ions by ASE from four solid matrixes. Diethyl ammonium diethyldithiocarbamate was added in chloroform as extraction solvent. Well recoveries were found when cellulose、sea sand and silical gel were used as matrixes. The recovery was near 70% for zinc when aluminum oxide was used as the matrix. The second is to evaluate the suitability of ASE in real soil sample. The amount of extracted metal ions was proportional with extraction temperature. The result shows that this method is similar to traditional 0.1N HCl extraction and 0.05 M EDTA extraction for soil. The third is to investigate the extraction of butyltins from sediment by ASE. The recoveries for three butyltins were dependent on different solvents. When hexane was used as extraction solvent,only tributyltin gives well recovery. The recovery can be improved for dibutyltin and monobutyltin when tropolone was added in hexane. The use of tetrahydrofuran as extraction solvent is also give good recovery for butyltins. Three separation studies by capillary electrophoresis for biochemical and environmental interested compounds are also demonstrated in this thesis. The first is to separate the atropisomeric polychlorinated biphenyls by cyclodextrin modified micellar electrokinetic chromatography. Seven PCB rotimers was sucessful separated. The second is to study the temperature effect on the separation of DNA fragments by capillary electrophoresis in hydroxyethyl cellulose solution. A possible mechanism was also proposed in this study. The third is to separate seven anabolic steroids with similar structures by MECC. The effect of organic modifier was also discussed in this article.