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研究生： 郭廷洋
論文名稱： 毛細管電泳層析微胞濃縮掃集法結合77K低溫螢光光譜分析對螢光增白劑DSBP之分析研究
指導教授： 林震煌
學位類別： 碩士
Master
系所名稱： 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： 108
中文關鍵詞： 毛細管電泳 、sweeping-MEKC 、77K低溫螢光 、DSBP
論文種類： 學術論文
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    • 本研究成功結合線上濃縮技術和毛細管電泳層析/77 K低溫螢光光譜偵測法，並針對在市售洗衣樣品中的E,E-DSBP進行77 K低溫光譜鑑定的研究。
    本實驗使用Sweeping-MEKC掃集法，可成功的於毛細管電泳中進行線上濃縮與分離DSBP的異構物，同時也結合77 K低溫螢光技術，在DSBP樣品抵達偵測窗口時，瞬間將溫度降至77 K，測量分別異構物的on-line螢光光譜，並比較真實樣品以及標準品的指紋比對。此方法可避免真實樣品上單純只依靠遷移時間或添加標準品來確定分析物，所導致的不準確性，此外，本實驗更進一步的研究DSBP光轉換以及異構物之分離的機制。

    The feasibility of combining the techniques of online concentration and capillary electrophoresis/low temperature fluorescence spectroscopy in the detection and identification of E,E-DSBP in synthetic detergent at 77 K is demonstrated. This technique, which involves the use of sweeping-MEKC, was used for the initial on-line concentration and separation, after which, a cryogenic molecular fluorescence experiment was performed at 77 K. The proposed method permits, not only the separation and detection of E,E-DSBP in a synthetic detergent sample, but also ensures that the on-line spectrum is readily distinguishable and can be un-ambiguously assigned at 77 K. The photo-conversion and isomer-separation of DSBP were also descried.

    中文摘要………………………………………………………………..Ⅰ 英文摘要………………………………………………………………..Ⅱ 目錄……………………………………………………………………..Ⅲ 圖目錄…………………………………………………………………..Ⅴ 表目錄…………………………………………………………………..Ⅶ 第一章 緒論………………...……………………………….……….01 1-1 分析物簡介……..………..………………………….…………..01 1-2 High Intensive Discharge (HID)氙氣燈……………...……….03 1-3 研究目的………………………………..………….…..………..05 第二章 研究原理和方法……………..……...………..........……….07 2-1 毛細管電泳層析法的發展……………….....……………..……07 2-2 毛細管電泳層析法的分離原理……………...…………..…..…12 2-2.1 電泳的分離與遷移率……………………………....…....12 2-2.2 Zeta電位與電滲流………..…….….…….……...…......14 2-2.3 電分散作用…………………………..……...…...….......20 2-2.4 分離效率及解析度…………………..………….….…....22 2-3 毛細管電泳層析法的分離模式…………..…...…………..….….23 2-3.1 毛細管區帶電泳層析法（CZE）………………………....23 2-3.2 微胞電動毛細管層析法（MEKC）…………….…….....24 2-4 毛細管電泳線上濃縮技術…………………………………..….28 2-4.1 毛細管電泳掃集法………………......…………………..30 2-5 77 K低溫螢光光譜分析法………………….…………………..32 2-6 固相萃取法………………………………….…………………..35 第三章 實驗儀器及藥品…………………….……..….…………….38 3-1 自組式毛細管電泳螢光分析儀…….….…...…………………..38 3-2 自組式毛細管電泳／低溫（77 K）螢光偵測系統……………..41 3-3 使用儀器及週邊設備列表………………………………………..45 3-4 藥品………………………..…………………….………………..48 第四章 毛細管電泳/HID氙氣燈誘導螢光法對DSBP 之偵測分析研究……………………………………….…....49 4-1 DSBP的標準品確認..............................................................49 4-2 DSBP光譜性質的測量..........................................................51 4-3 HID氙氣燈發光光譜的測量...................................................53 4-4 HID氙氣燈與DSBP光譜的比較............................................55 4-5 微胞電動層析法(MEKC)測試................................................59 4-5.1 MEKC最佳化電泳條件之確立……….… .……….…...59 4-1.2 MEKC檢量線的製作以及再現性的探討……...…..…..62 4-6 線上濃縮掃集法(Sweeping-MEKC)測試...............................65 4-6.1 Sweeping-MEKC最佳化電泳條件之確立…….….......65 (一) 背景溶液佐以添加有機修飾劑…… …..…....………..…65 (二) 背景溶液的調校………………....………….………....…69 (三) 最佳進樣長度的測量……………………...……….……..71 4-6.2 Sweeping-MEKC檢量線的製作以及再現性的探討…73 4-7 Normal-MEKC與Sweeping-MEKC之比較...........................76 4-8 萃取回收率探討....................................................................77 4-8 洗衣用清潔劑之檢測.............................................................81 第五章 毛細管電泳/Online 77 K 螢光光譜法鑑定 DSBP光轉換異構物……………………………………....84 5-1 吸收光譜偵測法鑑定DSBP及其異構物……….……………..87 5-2 螢光光譜法偵測DSBP………………….….…………………..90 5-2.1 室溫螢光光譜性質測量…………………………………90 5-2.2 77K低溫螢光光譜及低溫效應對螢光強度的影響...….92 5-2.3 毛細管電泳/螢光偵測法進行DSBP異構物的分離..….94 4-2.4 低溫77 K on-line 光譜鑑定E,E-DSBP、E,Z-DSBP..96 5-3清潔樣品毛細管電泳掃集結合on-line 77 K螢光光譜鑑定…..100 第六章 結論………………………………..…………………........102 參考資獻……………………………………………………………...103 論文發表………………………………………………………….…..108 附錄：期刊論文

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