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研究生： 劉學穎
Hsueh-Ying Liu
論文名稱： 應用毛細管電泳間接偵測方法分離四級銨鹽界面活性劑
Separation of homologues of quternary ammonium surfactants by capillary electrophoresis with indirect UV detection
指導教授： 丁望賢
Wang-Hsien Ding
口試委員:
學位類別： 碩士
Master
系所名稱： 理學院 - 化學學系
Department of Chemistry
畢業學年度： 91
語文別： 中文
論文頁數： 95
中文關鍵詞： 毛細管電泳 、間接偵測 、四級銨鹽界面活性劑
外文關鍵詞： capillary electrophoresis, quternary ammonium surfactants, indirect UV detection
相關次數： 點閱：12  下載：0 
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    • 摘要
    本研究應用毛細管電泳間接偵測的方法主要分離兩種未含有發色團的四級銨鹽界面活性劑，分別為直鏈式烷基三甲基銨鹽類( ATMACs )與直鏈式二烷基二甲基銨鹽類( DADMACs )。最有效的分離條件是緩衝溶液為10 mM磷酸鹽類，在pH值為4.35，添加有機修飾劑57.5%的四氫口夫口南( THF ) 與陰離子型界面活性劑修飾劑3 mM十二烷基硫酸鈉( SDS )，樣品利用水動式進樣法以壓力1 psi進樣20秒( 進樣體積約59.33 nL )，所施加電壓為25仟伏。為了改進波峰的定性與定量，針對發色團與內標準品的選擇做系統性的研究。其中氯化10-烷基苯基二甲基銨鹽( C10-BDMAC )為本實驗中最佳化的發色團，其與3 mM十二烷基硫酸鈉( SDS )結合對於此類的陽離子型界面活性劑可提供良好的偵測。毛細管電泳分析有良好的再現性，線性範圍為1.0到20.0 μg/mL，且線性關係係數( r2 )均大於0.999。本實驗的內標準品溴化8-四烷基銨鹽( TOA+B- )可增進遷移時間與定量上的再現性，其相對標準偏差( RSD )相對遷移時間均小於0.8%，與相對波峰面積其範圍為2.5~5.5%。此方法成功的應用到商業化的產品潤髮乳與衣物柔軟精中陽離子型界面活性劑的分析。本研究並利用電灑游離法質譜設備( ESI-MS )確認真實樣品中陽離子型界面活性劑之成分。

    Abstract
    This investigation describes the simultaneous separation of two major non-chromophoric quaternary ammonium surfactants, alkytrimethyl and dialkydimethyl ammonium compounds ( ATMACs and DADMACs, respectively ), by capillary electrophoresis ( CE ) with indirect UV detection. The most effective separation condition was 10 mM phosphate buffer with 57.5% tetrahydrofuran and 3 mM SDS at pH 4.35, and the sample hydrodynamic injection of up to 20 sec at 1 psi ( approximately 59.33 nL ), and an applied voltage 25 kV. The selection of appropriate chromophore and internal standard to improve the peak identification and quantitation was systematically investigated. Decylbenzyldimethyl ammonium chloride ( C10-BDMAC ) as a chromophore wih 3 mM SDS provided the best detectability for all homologues. The reproducibility of the migration time and quantitative analysis can be improved by using tetraoctylammonium bromide ( TOA+B- ) as an internal standard, giving the relative standard deviation ( RSD ) less than 0.8% for the relative migration times, and 2.5 to 5.5% for the relative peak areas. A good linearity of CE analysis was obtained in the range of 1.0 to 2.0 μg/mL with r2 values of above 0.999. The analysis of cationic surfactants in commercial products of hair conditioners and fabric softeners was also performed. Electrospray mass spectrometric method ( ESI-MS ) was applied to evaluate the CE method , and the compatible results were obtained.

    目錄 中文摘要 -------------------------------------------------------------------------- Ⅰ 英文摘要 -------------------------------------------------------------------------- Ⅱ 目錄 -------------------------------------------------------------------------------- Ⅳ 表目錄 ----------------------------------------------------------------------------- Ⅷ 圖目錄 ----------------------------------------------------------------------------- Ⅸ 第一章 前言 ---------------------------------------------------------------------- 1 1-1 研究的緣起 --------------------------------------------------------------- 1 1-2 研究目標 ------------------------------------------------------------------ 4 第二章 文獻回顧 ---------------------------------------------------------------- 5 2-1 陽離子型界面活性劑的分類和命名 ---------------------------- 6 2-2 國內外之相關研究 ------------------------------------------------- 14 2-3 電泳歷史背景和發展 ---------------------------------------------- 21 2-3-1 基本原理 ------------------------------------------------------- 23 2-3-2 毛細管電泳儀之裝置 ---------------------------------------- 24 2-3-3 分離模式 ------------------------------------------------------- 25 2-3-4 間接偵測法 ---------------------------------------------------- 31 2-3-5 影響毛細管電泳現象的因素 ------------------------------- 35 2-3-6 樣品的注入 ---------------------------------------------------- 37 2-3-7 偵測器 ---------------------------------------------------------- 38 第三章 實驗方法 -------------------------------------------------------------- 40 3-1 實驗藥品與儀器設備 ------------------------------------------------ 40 3-1-1 實驗藥品 ------------------------------------------------------- 40 3-1-2 儀器設備 ------------------------------------------------------- 42 3-2 實驗步驟 ---------------------------------------------------------------- 43 3-2-1 標準品的製備 ------------------------------------------------- 43 3-2-2 毛細管的處理 ------------------------------------------------- 45 3-2-3 緩衝溶液的製備 ---------------------------------------------- 46 3-2-4 實驗操作條件 ------------------------------------------------- 46 3-2-5 實驗最佳化操作條件 ---------------------------------------- 47 3-2-6 ESI-MS實驗操作條件 ------------------------------------- 48 第四章 結果與討論 ----------------------------------------------------------- 49 4-1 樣品基質比例的影響 ------------------------------------------------- 49 4-2 緩衝溶液的影響 ------------------------------------------------------- 50 4-2-1 發色團的選擇 ------------------------------------------------- 50 4-2-2 pH值的影響 --------------------------------------------------- 51 4-2-3 內標準品的選擇與有機修飾劑比例的問題 -------------- 51 4-2-4 最佳化條件 ----------------------------------------------------- 53 4-3 再線性 ------------------------------------------------------------------- 59 4-4 潤髮乳與衣物柔軟精之檢測 ---------------------------------------- 60 4-4-1 檢量線的製作 ------------------------------------------------- 60 4-4-2 測定真實樣品中之ATMABs與DADMABs之含量 -- 64 4-4-3 ESI-MS的定性 ------------------------------------------------ 64 第五章 結果與建議 ----------------------------------------------------------- 69 5-1 結論 ---------------------------------------------------------------------- 69 5-2 建議 ---------------------------------------------------------------------- 70 第六章 參考文獻 -------------------------------------------------------------- 71 第七章 附錄 -------------------------------------------------------------------- 79 7-1 微胞電動毛細管層析法 ---------------------------------------------- 79 7-2 毛細管等電聚焦電泳法 ---------------------------------------------- 80 7-3 毛細管凝膠電泳法 ---------------------------------------------------- 82 7-4 毛細管等速電泳法 ---------------------------------------------------- 83 7-5 毛細管電動層析法 ---------------------------------------------------- 84 7-6 樣品檢測之電泳圖與ESI-MS質譜圖 ----------------------------- 85

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