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研究生:張詠雅
研究生(外文):Yung-Ya Chang
論文名稱:綠色溶劑離子液體微萃取結合高效能液相層析分析水溶液中
論文名稱(外文):Green Solvent Ionic Liquid Microextraction Combined with HPLC for Analysis of Aquatic Animal Medicine
指導教授:喻家駿
口試委員:喻家駿魏玉麟瞿港華
口試日期:2013-07-22
學位類別:碩士
校院名稱:逢甲大學
系所名稱:環境工程與科學學系
學門:工程學門
學類:環境工程學類
論文種類:學術論文
論文出版年:2013
畢業學年度:101
語文別:中文
論文頁數:102
中文關鍵詞:室溫離子液體離子液體分散式液-液微萃取方法孔雀石綠亞甲藍綠色化學
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近年來分析技術強調快速與較低成本之綠色化學萃取技術,是許多檢測方法開發的重點,並選擇較安全、無毒性與對環境友善之化學溶劑,來取代具毒性化學溶劑。分析微量污染物之檢測技術日趨重要,使用綠色化學萃取技術幫助分析微量污染物,為現今許多分析化學研究追求之目標。傳統液相-液相萃取法使用之溶劑多為揮發性有機化合物(Volatile organic compounds, VOCs ),然而VOCs具有高毒性、易燃性與易揮發性等,對於人類及環境有較大之影響。因此發展出室溫離子液體(Room temperature ionic liquids, RTILs)之綠色化學溶劑,具有不易燃性、不易揮發性、可回收再利用及對環境友善等特性,可用來取代高毒性之揮發性有機溶劑。
本研究使用離子液體分散式液-液微萃取方法(ionic liquids distributed liquid - liquid microextraction,IL-DLLME),搭配室溫離子液體[BMPy][Tf2N]萃取含有亞甲藍(MB)及孔雀石綠(MG)之樣品,搭配高效能液相層析儀分析,經實驗得到最佳沖提液比例氰甲烷/水(20/80)梯度沖提,搭配MB及MG最佳之吸收波長為664nm及617nm;計算出方法偵測極限為0.0369 mg/L及0.0519 mg/L;使用離子液體[BMPy][Tf2N]萃取兩種藥品,萃取效率皆達97%以上;與其他萃取溶劑[Bmin][PF6]、二氯甲烷及正己烷比較,得到[BMPy][Tf2N]為最適合使用之萃取溶劑,有良好分離效果且波峰面積明顯增加;應用於實際樣品上之結果萃取率皆達97%以上,對於實際樣品之應用結果良好。綜合本研究結果得知,以離子液體分散液相微萃取法搭配萃取溶劑離子液體[BMPy][Tf2N]萃取MB及MG,低濃度萃取濃縮後波峰面積明顯增加,使用少量萃取溶劑及樣品,步驟簡單快速及萃取率佳,為分析前處理可行之萃取濃縮方法。
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 研究緣起與目的 1
1.2 研究內容概要 3
第二章 文獻回顧 5
2.1萃取方法發展及演變 5
2.1.1 固相萃取法 5
2.1.2固相微萃取 6
2.1.3液相-液相萃取法 7
2.1.4液相-液相微萃取 7
2.1.4.1單滴微萃取 8
2.1.4.2中空纖維液相微萃取 10
2.1.4.3分散液液微萃取 12
2.1.5分散液相微萃取之應用 13
2.1.6離子液體分散液相微萃取 14
2.2 離子液體 16
2.2.1常見離子液體之種類 18
2.2.2 離子液體之物性與化性 20
2.2.2.1 熔點 20
2.2.2.2黏度 22
2.2.2.3密度 23
2.2.2.4 表面張力 24
2.2.2.5 親水性 25
2.2.2.6 毒性 26
2.2.3 離子液體之合成方法 28
2.2.3.1 直接合成法 28
2.2.3.2 兩步合成法 29
2.2.3.3 離子液體[BMPy][Tf2N]之製備合成30
2.2.3.4 離子液體[BMPy][Tf2N]之選用 31
2.3 分析藥品 33
2.3.1 孔雀石綠 36
2.3.2 亞甲藍 40
第三章 實驗方法 44
3.1 實驗藥品與試劑 44
3.1.1 實驗萃取溶劑 44
3.1.2 萃取分析之樣品 45
3.1.3 液體相層析使用之試劑 45
3.2 實驗儀器與設備 46
3.3 實驗流程與分析方法 46
3.3.1 實驗研究設計 46
3.3.2 實驗分析方法 48
3.3.2.1建立樣品檢量線 48
3.3.2.2方法偵測極限 48
3.3.3 萃取操作步驟 51
3.3.3.1 離子液體萃取步驟 51
3.3.3.2 有機溶劑二氯甲烷萃取步驟 52
3.3.3.3 有機溶劑正己烷萃取步驟 53
3.3.3.4 萃取效率之計算 55
第四章 結果與討論 56
4.1藥品之偵測波長 56
4.2液相層析條件之確立 58
4.2.1最佳高效能液相層析條件 58
4.3高效能液相層析分析樣品 60
4.3.1背景值空白試驗 60
4.3.2單一樣品之高效能液相層析分析 61
4.3.3混合樣品之高效能液相層析分析 63
4.4檢量線與方法偵測極限 64
4.4.1檢量線建立 64
4.4.2方法偵測極限 68
4.5離子液體萃取樣品 70
4.5.1高效能液相層析儀進行萃取分析 70
4.5.2不同萃取溶劑萃取比較 76
4.6環境樣品萃取分析 83
4.7萃取效率計算 87
第五章 結論 91
第六章 參考文獻 93
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