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研究生:李沂玶
研究生(外文):Lee, Yi-Ping
論文名稱:應用非水相毛細管電泳法分離芳杯化合物
論文名稱(外文):Separation of calix[4]arenes by non-aqueous capillary electrophoresis
指導教授:謝有容謝有容引用關係
指導教授(外文):Hsieh, You-Zung
學位類別:碩士
校院名稱:國立交通大學
系所名稱:應用化學研究所
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2010
畢業學年度:98
語文別:中文
論文頁數:73
中文關鍵詞:非水相毛細管電泳芳杯
外文關鍵詞:nonaqueous capillary electrophoresiscalixarenesNACE
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在本研究中,我們選用非水相毛細管電泳法作為八種芳杯化合物的分離方法。非水相毛細管電泳法使用有機溶劑取代水溶液作為背景電解液的溶劑,可增加疏水性分析物的溶解度,因此可增加系統的選擇性。由於八種芳杯化合物分別帶有不同取代基,因此在甲酸/甲酸銨及乙酸/乙酸銨的背景電解液中,會有不同的去質子化程度。我們選用乙?咫峊珧禰秭Q胺混合溶劑作為背景電解液的溶劑組成。在此溶劑系統當中,我們將探討甲酸及乙酸的濃度、有機溶劑的比例,以及乙酸銨的濃度對其分離效果造成之影響。最後我們使用100 mM乙酸,20 mM乙酸銨,溶劑組成為乙??甲基甲醯胺 (70:30, v/v) 的背景電解液,在11分鐘內成功分離八種芳杯化合物。在最佳化條件下,線性範圍為2.5-100 ?慊/mL,線性相關係數(r2)皆大於0.9914,表示其線性關係良好。八種分析物的偵測極限在0.73-2.32 ?慊/mL之間。除此之外,每單位公尺的理論板數範圍也在3.58 - 5.21×105之間,表示分離效率良好;遷移時間之相對標準偏差(RSD)也都小於1.0%。因此非水相毛細管電泳法應用於分析八種芳杯化合物確實為一種具有高再現性以及高分離效率的分析方法。
中文摘要 i
英文摘要 ii
誌謝 iv
目錄 vii
圖目錄 xi
表目錄 xii
一、毛細管電泳 1
1.1 簡介 1
1.2 電滲流 2
1.3 分離原理 4
1.4 分離效率 6
1.5 毛細管電泳常見之分離模式 7
1.5.1 毛細管區帶電泳 7
1.5.2 微胞電動層析 7
1.5.3 毛細管凝膠電泳 8
1.5.4 毛細管等電聚焦 8
1.5.5 毛細管等速電泳 9
二、非水相毛細管電泳 10
2.1簡介 10
2.1.1 電滲流 11
2.2 非水相毛細管電泳常用之溶劑 12
2.2.1 溶劑的選用 12
2.2.2 溶劑的影響 15
2.3 非水相溶劑中的酸解離常數(pKa) 16
2.4 非水相溶劑中的pH*值 18
2.5 非水相毛細管電泳常使用之偵測方法 19
2.5.1 紫外-可見光吸收 19
2.5.2雷射誘導螢光 19
2.5.3質譜 20
2.5.4電化學 21
2.6 非水相毛細管電泳之應用 21
2.7 非水相毛細管電泳之修飾劑使用 22
2.7.1 掌性選擇試劑 22
2.7.2 離子液體 23
2.8 非水相毛細管電泳之優點 23
三、芳杯系列化合物 25
3.1 簡介 25
3.2 芳杯化合物之應用 27
3.2.1 金屬離子之萃取 27
3.2.2 電化學感測 29
3.2.3 螢光分子感測器 29
3.2.4 分離技術之選擇試劑 31
3.3 芳杯化合物之相關分析技術 32
3.3.1 高效能液相層析 32
3.3.2 毛細管電泳法 32
四、利用非水相毛細管電泳法分離芳杯化合物 34
4.1 簡介 34
4.2 儀器裝置 34
4.3 試藥 35
4.4 實驗方法 37
4.4.1 新毛細管的調態 37
4.4.2 實驗前、後毛細管的處理 37
4.4.3 Calixarene標準溶液之配製 38
4.4.4 水相毛細管電泳分離測試 38
4.4.5 非水相毛細管電泳分離之測試 38
4.4.5.1 弱酸性有機酸之甲酸不同濃度測試 38
4.4.5.2 弱酸性有機酸之乙酸不同濃度測試 39
4.4.5.3 不同種類有機溶劑之測試 39
4.4.5.4 不同比例的有機溶劑之測試 40
4.4.5.5 不同濃度的鹽類之測試 40
4.4.5.6 定量校正曲線與再現性分析 40
4.5結果與討論 41
4.5.1水相毛細管電泳分離之結果 41
4.5.2非水相毛細管電泳分離之結果 42
4.5.2.1 弱酸性有機酸之甲酸不同濃度測試 42
4.5.2.2 弱酸性有機酸之乙酸不同濃度測試 48
4.5.2.3 不同種類有機溶劑之結果 53
4.5.2.4 不同比例的有機溶劑之結果 56
4.5.2.5 不同鹽類濃度之結果 60
4.5.2.6 定量校正曲線與再現性分析之結果 62
五、結論 65
六、參考文獻 66
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