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利用固相微萃取及液相微萃取法分析超微量有機物質之研究
Dissertation

利用固相微萃取及液相微萃取法分析超微量有機物質之研究

賈侃融
Doctor of Philosophy (PHD), 國立清華大學, 化學系
2004

Abstract

微量分析 固相微萃取 液相微萃取 溶劑棒微萃取 單滴微萃取 氣相層析 質譜儀 戴奧辛 安非他命 有機氯 化學衍生 中空纖維 Trace Analysis Solid-Phase Microextraction Liquid-Phase Microextraction Solvent Bar Microextraction Single-Drop Microextraction Gas-Chromatography Mass Spectrometer Dioxins Amphetamine Organochlorine Chemical Derivatization Hollow Fiber
The development of faster, simpler and economic sample-preparation techniques is an important issue in chemical analysis. In this work, four analytical methods based on solid-phase microextraction and liquid-phase microextraction were described. The developed methods have been applied to the analysis of trace organic pollutants in different sample matrices such as soil, human urine or wine. Solid-phase microextraction (SPME), discovered and developed by Pawliszyn and co-workers, has emerged as a versatile solvent-free alternative to conventional liquid–liquid extraction and solid-phase extraction procedures. It involves the partitioning of analytes between the fiber coating and the sample matrix. The first topic describes the development of HS-SPME technique by cooling the headspace where the fiber is suspended, and heating / ultrasonic activated of the sample area simultaneously. It was applied to the screening of soil sample by high contamination with dioxins. Second topic describes the development of SPME technique where the extraction and derivatization were carried out in one step. In this work, the glass insert containing the derivatizing reagent was introduced into the sample vial so that the fiber can absorb the reagents and analytes at the same time. This technique was applied to the analysis of amphetamine-like drugs in urine sample from abusers. Liquid-phase microextraction (LPME) methods, which included the sing-drop microextraction (SDME), hollow fiber liquid-phase microextraction (HF-LPME), and solvent bar microextraction (SBME) were investigated in the chapter four and chapter five. This methodology proved to be an extremely simple, low cost and virtually solvent-free sample-preparation technique, which provided a high degree of selectivity and enrichment with the partitioning of analytes in organic and aqueous phase. The results show that these sample-preparation techniques coupled with mass spectrometric detection could determinate the trace organic pollutants in the low ppb or ppt level.

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