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研究生： 賈侃融
Kan-Jung Chia
論文名稱： 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
Analysis of trace organic pollutants based on a solid-phase microextraction and liquid-phase microextraction technique
指導教授： 黃賢達
Shang-Da Huang
口試委員:
學位類別： 博士
Doctor
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2005
畢業學年度： 93
語文別： 中文
論文頁數： 173
中文關鍵詞： 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
外文關鍵詞： 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
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    • 近年來在化學分析方法上，強調快速、簡便與環保的分析技術，傳統的液液相萃取法或固相萃取法等，對於分析環境中之微量污染物有著花費大量時間或有機溶劑的缺點。因此本論文的研究動機是發展兩套分析方法，一為改良式的固相微萃取技術、一為液相微萃取技術，配合氣相層析質譜儀之分析方法，並將其運用在自然界中超微量有機物之測定。 以下為各章節的主題與概要說明。
    第一章為緒論，說明在發展經濟同時環境保護的重要性，提出本論文研究之目的，並介紹各章節中運用之分析技術的原理與特性。
    第二章為利用改良式的固相微萃取法分析土壤中之戴奧辛。研究中探討一般的固相微萃取裝置，在萃取受污染土壤中之戴奧辛時會遭遇到的問題，而利用本實驗之改良裝置可以加以克服。文中說明了利用自行設計的冷卻系統結合固相微萃取裝置，配合超音波震盪樣品，可將與土壤結合強的戴奧辛化合物揮發至樣品瓶中頂空部分，再以吸附纖維萃取後，以串聯質譜技術分析。與文獻之分析戴奧辛方法比較，樣品分析時間由24小時縮減為2小時，可大幅降低人力與時間的耗費。
    第三章為同步衍生-萃取的固相微萃取技術應用在人體尿液中的安非他命類藥物之分析。研究中說明一般分析濫用藥物的萃取方法，並討論本研究開發出之同時衍生/萃取的實驗裝置所達到的良好結果，除了分析時間的縮短，方法的簡便與靈敏度的提升外，並探討各項萃取參數之最佳化條件，與此技術之實際應用性，顯示可分析尿液中超微量濃度之濫用藥物。
    第四章之內容為化學衍生法結合液相微萃取技術，並應用於水溶液樣品中微量一級胺之分析。液相微萃取法是近年來新興的一種樣品前處理方法，萃取相為微量有機溶劑，相較於商業化固相微萃取之吸附纖維的價格低廉許多，同時也具有樣品前濃縮的效果，為一十分快速簡便之前處理方法。研究中探討中空液相微萃取法的最佳化參數，並與單滴微萃取法加以比較。
    第五章之內容是開發溶劑棒微萃取技術與其應用。溶劑棒微萃取法是2004年發表的一項萃取技術，利用聚丙烯材質的中空纖維包覆溶劑形成一「溶劑棒」，與水溶液樣品一起攪動達成萃取。本研究中討論了各項最佳化參數，以及應用在酒類樣品中有機氯農藥的分析。
    第六章則將上述開發的數種分析方法做簡單的整理，並展望未來分析技術可能的進展與應用。

    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.

    中文摘要 Abstract 第一章 緒論 1-1前言 ………………………………………………………………1 1-2研究目的 …………………………………………………………3 1-2-1開發簡單快速檢測土壤中高度污染的戴奧辛之分析方法 …3 1-2-2以同步萃取/衍生之固相微萃取法分析尿液中安非他命類 之濫用藥物 …………………………………………………4 1-2-3以液相微萃取法分析水樣中之一級胺 ………………………4 1-2-4以溶劑棒微萃取法分析酒類中之有機氯農藥 ………………5 1-3固相微萃取法 ……………………………………………………6 1-3-1萃取原理 ………………………………………………………6 1-3-2直接浸入式固相微萃取法 ……………………………………7 1-3-3頂空固相微萃取法 ……………………………………………7 1-3-4固相微萃取法的特點與應用 …………………………………8 1-4液相微萃取法 ……………………………………………………10 1-4-1單滴微萃取 ……………………………………………………10 1-4-2中空纖維薄膜液相微萃取 ……………………………………11 1-4-3中空纖維液相微萃取 …………………………………………12 1-4-4溶劑棒微萃取 …………………………………………………13 1-4-5萃取原理 ………………………………………………………14 1-4-6液相微萃取法的特點與發展 …………………………………14 1-5氣相層析離子阱質譜儀 …………………………………………16 第二章 開發簡單快速檢測土壤中嚴重污染戴奧辛之分析方法 2-1前言 ………………………………………………………………26 2-1-1戴奧辛性質 ……………………………………………………26 2-1-2戴奧辛的影響 …………………………………………………27 2-1-3開發一快速檢測土壤中高度污染戴奧辛之分析方法 ………29 2-2實驗部分 …………………………………………………………31 2-2-1試藥 ……………………………………………………………31 2-2-2器材 ……………………………………………………………31 2-2-3分析儀器 ………………………………………………………32 2-2-4樣品配置 ………………………………………………………34 2-2-5萃取步驟 ………………………………………………………34 2-3結果與討論 ………………………………………………………35 2-3-1靜相纖維之選擇 ………………………………………………35 2-3-2樣品溫度 ………………………………………………………35 2-3-3不同萃取裝置之效果 …………………………………………36 2-3-4添加有機溶劑的影響 …………………………………………37 2-3-5定量方法 ………………………………………………………37 2-3-6絕對回收率、偵測極限與精密度 ……………………………38 2-4結論 ………………………………………………………………40 第三章 以同步萃取/衍生之固相微萃取法分析尿液中安非他命類 化合物 3-1前言 ………………………………………………………………50 3-1-1安非他命類藥物之性質 ………………………………………50 3-1-2分析方法 ………………………………………………………52 3-1-3固相微萃取結合化學衍生法 …………………………………52 3-2實驗部分 …………………………………………………………54 3-2-1試藥與器材 ……………………………………………………54 3-2-2分析儀器 ………………………………………………………55 3-2-3萃取步驟 ………………………………………………………56 3-3結果與討論 ………………………………………………………58 3-3-1靜相纖維之選擇 ………………………………………………58 3-3-2衍生劑體積 ……………………………………………………58 3-3-3萃取時間 ………………………………………………………59 3-3-4萃取溫度 ………………………………………………………60 3-3-5樣品攪拌程度 …………………………………………………60 3-3-6離子強度 ………………………………………………………61 3-3-7檢量線與偵測極限 ……………………………………………62 3-3-8回收率與精密度 ………………………………………………62 3-3-9真實樣品的測試 ………………………………………………63 3-4與文獻分析方法的比較 …………………………………………64 3-5結論 ………………………………………………………………65 第四章 以液相微萃取法分析水樣中之一級胺 4-1前言 ………………………………………………………………87 4-2實驗部分 …………………………………………………………88 4-2-1試藥 ……………………………………………………………88 4-2-2器材 ……………………………………………………………89 4-2-3分析儀器 ………………………………………………………89 4-2-4衍生化反應過程 ………………………………………………90 4-2-5中空纖維液相微萃取 …………………………………………91 4-2-6單滴微萃取 ……………………………………………………91 4-3結果與討論 ………………………………………………………93 4-3-1化學衍生法 ……………………………………………………93 4-3-2萃取溶劑的選擇 ………………………………………………93 4-3-3樣品攪動程度 …………………………………………………94 4-3-4萃取時間 ………………………………………………………94 4-3-5萃取溫度 ………………………………………………………95 4-3-6離子強度的影響 ………………………………………………95 4-3-7檢量線與精密度 ………………………………………………96 4-3-8溪水樣品 ………………………………………………………96 4-3-9與單滴微萃取法的比較 ………………………………………96 4-4文獻分析方法的比較 ……………………………………………98 4-5結論 ………………………………………………………………99 第五章 以溶劑棒微萃取法分析酒類樣品中微量有機氯農藥 5-1前言 ………………………………………………………………116 5-1-1有機氯農藥簡介 ………………………………………………116 5-1-2實驗架構 ………………………………………………………117 5-2實驗部分 …………………………………………………………118 5-2-1試藥 ……………………………………………………………118 5-2-2器材 ……………………………………………………………118 5-2-3分析儀器 ………………………………………………………119 5-2-4溶劑棒微萃取 …………………………………………………120 5-2-5中空纖維液相微萃取 …………………………………………121 5-3結果與討論 ………………………………………………………122 5-3-1萃取溶劑的選擇 ………………………………………………122 5-3-2樣品攪動程度 …………………………………………………122 5-3-3萃取時間 ………………………………………………………123 5-3-4萃取溫度 ………………………………………………………123 5-3-5離子強度的影響 ………………………………………………124 5-3-6樣品溶液中添加乙醇的影響 …………………………………124 5-3-7有機相/水相之體積比 ………………………………………125 5-3-8檢量線 …………………………………………………………126 5-3-9與中空纖維液相微萃取法的比較 ……………………………127 5-3-10酒類樣品的檢測 ……………………………………………128 5-4與文獻分析方法的比較 …………………………………………129 5-5結論 ………………………………………………………………130 第六章 結論與未來展望 6-1前處理技術的演進 ………………………………………………154 6-2分析方法的選擇 …………………………………………………156 6-3未來展望 …………………………………………………………158 參考文獻 ……………………………………………………………159

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