臺灣博碩士論文加值系統

本篇論文主要為開發新形態高分子整體成形管柱微萃取(polymer monolith microextraction, PMME)之萃取管柱材料：結合甲基丙烯酸烷基酯單體與二乙烯苯交聯劑並以乙二醇做為擴孔劑，針對水樣中九種非類固醇抗發炎藥物(non-steroid anti-inflammatory durgs, NSAIDs)進行萃取，最後以毛細管微乳化方法檢測其萃取效果。
實驗首先以聚(甲基丙烯酸十八烷基酯-二乙烯苯) (poly(SMA-DVB))整體成形毛細管柱作為萃取管柱，並對活化溶劑的種類及流速、清洗溶劑的種類及流速、萃取與脫附溶劑的流速、萃取管柱中擴孔劑PEG之添加量、萃取管柱長度、高分子材料聚合溶液的單體比例進行最佳化；之後再以不同碳鏈長度之甲基丙烯酸烷基酯類單體合成萃取管柱，藉以不同碳鏈長度來探討不同親疏水性對萃取的影響，最後得到以聚(甲基丙烯酸八烷基酯-二乙烯苯)之整體成形萃取管柱有最佳萃取效能，其回收率達到73.8~99.6 %，以相同管柱重覆萃取之標準偏差(RSD of run-to-run)小於10.7 %，不同批次製備管柱之標準偏差(RSD of column-to-column)小於13.5 %。

In this study, we developed a new monolithic material for polymer monolith microextraction (PMME) that was prepared in the capillary and applied to extract non-steroid anti-inflammatory durgs (NSAIDs) in water solution. Herein microemulsion electrokinetic chromatography (MEEKC) was used to check the extraction efficiency.
At first, poly(stearyl methacrylate-divinylbenzene) (poly(SMA-DVB)) monolithic column was employed, and the extracted parameters were optimized that included solvent type, flow rate, column length and composition of extraction column. Then, different alkyl chain length of alkyl methacrylate monomers have been tested and different extracted efficiency was obtained due to their hydrophobic and hydrophilic interaction. Finally poly(lauryl methacrylate- divinylbenzene) (poly(LMA-DVB)) monolithic column was the best PMME material which has higher extraction efficiency (recovery from 73.8% to 99.6%) and lower RSD% (run to run: < 10.7 %, column to column: < 13.5 %).

目錄
中文摘要 I
Abstract II
目錄 III
圖目錄 VII
表目錄 IX
第一章 緒論 1
1-1 研究緣起 1
1-2 研究目標 3
第二章 文獻回顧 4
2-1 非類固醇抗發炎藥物 4
2-1-1非類固醇抗發炎藥物簡介 4
2-1-2 非類固醇抗發炎藥物之危害性 4
2-2 固相萃取 5
2-3 固相微萃取 10
2-3-1 Fiber SPME介紹 11
2-3-2 SBSE介紹 11
2-3-3 In-tube SPME介紹 12
2-3-4 Syringe SPME 12
2-3-5 PMME 介紹 13
2-4 毛細管電泳簡介 18
2-4-1 毛細管電泳原理 18
2-4-2 電滲流 19
2-4-3 微乳化電層析(microemulsion electrokinetic chromatography,MEEKC) 21
2-5 有機高分子整體成形式管柱 23
2-5-1 聚丙烯醯胺類(polyacrylamide-based polymer monoliths) 23
2-5-2 聚甲基丙酸酯類(polymethacrylate-based polymer monoliths) 24
2-5-3 聚苯乙烯類(polystyrene-based polymer monoliths) 24
2-5-4 結合聚甲基丙烯酸酯類與聚苯乙烯類 25
2-6. 實驗方法 26
第三章 實驗介紹 28
3-1 實驗儀器設備 28
3-2 藥品名稱與廠牌介紹 29
3-3 毛細管微乳化電層析分析NSAIDs實驗介紹 33
3-3-1 NSAIDs標準品結構及性質介紹： 33
3-3-2 實驗藥品配置方法 34
3-3-3 NSAIDs藥物分離之實驗條件 35
223-4 PMME高分子整體成形萃取管柱製備 36
3-4-1 毛細管壁改質前處理 36
3-4-2 PMME高分子聚合溶液配置 37
3-4-3 PMME萃取管柱製備 38
3-4-4 高分子共聚物粉末製備 39
3-5 PMME萃取裝置 40
3-6 PMME萃取過程 41
3-7 萃取效能之計算 41
第四章 結果與討論 42
4-1 PMME萃取管柱的最佳化 42
4-1-1 PMME萃取管柱材料的選擇 42
4-1-2 PEG添加量對PMME管柱萃取效果之影響 44
4-1-3 PMME管柱長度對萃取效果之影響 46
4-1-4 改變聚合溶液之單體比例對萃取效果的影響 48
4-2 PMME萃取過程的最佳化 51
4-2-1 清洗溶液的最佳化 51
4-2-2 活化溶液的最佳化 54
4-2-3 流速的初步最佳化 56
4-2-4 以多變數方法探討流速最佳化條件 59
4-3 以不同碳鏈長度之甲基丙烯酸酯類單體合成萃取管柱對NSAIDs萃取效果的影響 64
4-4. poly(LMA-DVB) PMME萃取管柱效能評估 72
4-5. 檢量曲線與偵測極限 73
第五章 結論 74
未來展望 76
參考文獻 77
附錄I. 86
附錄II. 89
 
圖目錄
圖2-1. SPME方法的分類 10
圖2-2. 毛細管電泳裝置圖 18
圖2-3. 電雙層示意圖 19
圖2-4. 高pH值時油滴移動方向 21
圖2-5. 微乳化電層析在低pH值移動方向 22
圖2-6. 逆向偵測之示意圖 22
圖3-1. 毛細管萃取管柱與針筒連接裝置示意圖 40
圖3-2. PMME萃取裝置 40
圖3-3. PMME萃取過程示意圖 41
圖4-1. poly(SMA-DVB)添加不同比例PEG之影響 45
圖4-2. 不同長度萃取管柱之回收率表示 47
圖4-3.不同單體比例之回收率 49
圖4-4. 不同單體比例之poly(SMA-DVB) (5.8%PEG) SEM圖 49
圖4-5. 清洗溶液對萃取效果之影響 53
圖4-6. 不同條件活化管柱之回收率 55
圖4-7. 不同流速之萃取、清洗和脫附過程的檢測層析圖 57
圖4-8. 多變數方法之實驗設計 60
圖4-9. Idm於多變數中各個因子的影響 62
圖4-10. (a)未最佳化與(b)最佳化流速之回收率比較 63
圖4-11. poly(LMA-DVB)不同PEG添加量之回收率比較 65
圖4-12. poly(OMA-DVB)不同PEG添加量之回收率比較 66
圖4-13. poly(BMA-DVB)添加60.4mg PEG之回收率 67
圖4-14. poly(MMA-DVB)添加75.5mg PEG之回收率 68
圖4-15. 綜合不同AMA單體最佳PEG添加量合成之萃取管柱對萃取效果比較 69
圖4-16. 各最佳條件的poly(AMA-DVB)萃取毛細管之SEM圖 71
圖II-1. 各最佳條件的poly(AMA-DVB)高分子材料接觸角測試 88
 
表目錄
表2-1. 近五年(2008~2013)以SPE前處理分析NSAIDs水樣之文獻 7
表2-1. 近五年(2008~2013)以SPE前處理分析NSAIDs水樣之文獻 (續) 8
表2-1. 近五年(2008~2013)以SPE前處理分析NSAIDs水樣之文獻 (續) 9
表2-2. 歷年(~2013年)用於PMME管柱的材料與其應用 14
表2-2. 歷年(~2013年)用於PMME管柱的材料與其應用(續) 15
表2-2. 歷年(~2013年)用於PMME管柱的材料與其應用(續) 16
表2-2. 歷年(~2013年)用於PMME管柱的材料與其應用(續) 17
表2-3 可能影響電滲流之因素 21
表3-1.儀器設備名稱及廠牌型號 28
表3-2.實驗藥品 29
表3-3. 萃取用聚合高分子靜相所使用之藥品 30
表3-4.萃取用聚合高分子靜相所使用之藥品結構式與性質 31
表3-4.萃取用聚合高分子靜相所使用之藥品結構式與性質 (續) 32
表3-5.TBC的結構式與性質 32
表3-6. NSAIDs標準品結構及性質介紹 33
表3-6. NSAIDs標準品結構及性質介紹 (續) 34
表3-7. poly(SMA-DVB)添加模板PEG之組成變化 37
表3-8. Poly(AMA-DVB)系列單體組成變化 37
表3-9. PMME萃取最佳條件 41
表4-1 三種管柱條件與背壓之比較 43
表4-2. 添加不同比例PEG之回收率 45
表4-3. 不同萃取管柱長度之回收率 47
表4-4. 不同單體比例之回收率 48
表4-5. 不同單體比例之通透度 50
表4-6. 清洗溶液實驗之萃取過程 52
表4-7.不同活化溶液之條件與過程 54
表4-8. 不同條件活化管柱之回收率 55
表4-9. 多變數因子的設計 60
表4-10. L9直交表 60
表4-11. 九種分析物於各組實驗中的回收率 61
表4-12. Idm於四個因子中三個階層之回收率 61
表4-13. 各分析物在四個過程中的最佳流速 62
表4-14. 流速最佳化與未最佳化之回收率比較 63
表4-15. 所嘗試合成之管柱 64
表4-16. poly(LMA-DVB)不同PEG添加量之回收率 65
表4-17. poly(OMA-DVB)不同PEG添加量之回收率 66
表4-18. poly(BMA-DVB)不同PEG添加量之回收率 67
表4-19. poly(MMA-DVB)不同PEG添加量之回收率 68
表4-20. poly(LMA-DVB) PMME管柱對NSAIDs萃取之回收率及再現性 72
表4-21. Poly(LMA-DVB)以PMME方法之檢量曲線和偵測極限 73
表5-1. 本實驗成果與文獻(2008~2013)比較 75
表II-1. 最佳條件製備的poly(AMA-DVB)高分子材料之接觸角 86
表III-1. 最佳條件製備的poly(AMA-DVB)高分子材料BET數據 89

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