謝學真臺灣大學：化學工程學研究所洪偉翔Hung, Wei-HsiangWei-HsiangHung2007-11-262018-06-282007-11-262018-06-282007http://ntur.lib.ntu.edu.tw//handle/246246/52257Abstract In this research, porous chitosan microparticles were prepared by using a emulsification/freeze-gelation method. The effects of various processes parameters were investigated. The BSA-loading capability of the porous chitosan microparticles and that of a commercial powder were compared. First, the optimum HLB value of the surfactant utilized in this method was found to be in the range of 8.6-11.0. The size of the porous chitosan microparticles became smaller as the HLB values of the different surfactants approached the optimum HLB value. These microparticles prepared by using different surfactants had different structures；some were dense porous and some were loose porous. Second, Span 20/Tween 21 was found to be the optimum combination of surfactants with the HLB value of 10. The microparticles had homogeneous and loose porous structure, and the particle size was 153.4 μm and C.V. was 33.9%. Third, in the emulsification system when the proportion of petroleumbenzin (mL) / 1 wt% chitosan solution (mL) / surfactants (g) was adjusted to 100/20/1.5, the particle yield was increased by 3.2 folds with size of 163.3 μm (C.V. = 37.3%). Fourth, this research also investigated the influence of freezing temperature. The water uptake capability of microparticles increased obviously when the freezing temperature decreased. The water uptake capability was about 2300% when the freezing temperature was -25℃, which was 5.5 folds of that of commercial powder. Finally, the application of the porous chitosan microparticles in BSA loading indicated that BSA loading was complete at low BSA concentration (＜0.8 mg/mL) and was 190 mg BSA/g chitosan at high BSA concentration (＞2.0 mg/mL). The loading capacity of these microparticles was 4 folds of that of commercial powder. This research demonstrated that the properties of the porous chitosan microparticles could be modulated by varying the process parameters for application in various fields.目錄 誌謝.........................................................................................................................I 中文摘要..............................................................................................................III Abstract..................................................................................................................V 目錄.................................................................................................................... VII 圖目錄..................................................................................................................XI 表目錄............................................................................................................. XVII 縮寫與符號說明...............................................................................................XIX 中英名詞對照...................................................................................................XXI 1. 緒論.................................................................................................................1 1.1. 研究背景..........................................................................................1 1.2. 研究構想..........................................................................................2 2. 文獻回顧.........................................................................................................5 2.1. 幾丁聚醣..........................................................................................5 2.1.1. 幾丁聚醣的結構與性質..........................................................5 2.1.2. 幾丁聚醣的應用.......................................................................6 2.1.2.1. 生醫方面之應用........................................................6 2.1.2.2. 工業廢棄物方面之應用............................................6 2.1.2.3. 其他方面之應用........................................................7 2.2. 微粒製備法與應用..........................................................................7 2.2.1. 乳化法及其衍生之改良製備方法..........................................7 2.2.1.1. 乳化之介紹................................................................7 2.2.1.2. 乳化液的穩定性........................................................8 2.2.1.3. 界面活性劑的分類..................................................10 2.2.1.4. 選擇界面活性劑的方法..........................................11 2.2.1.5. 乳化法及其衍生之改良製備方法介紹..................13 2.2.2. 其他製備微粒之方法............................................................18 2.2.2.1. 噴霧法(spray method) .............................................18 2.2.2.2. 凝聚法(coacervation method)..................................19 2.2.2.3. 超音波霧化法(ultrasonic atomization) ...................19 2.2.2.4. 滴入法(orifice method)............................................20 2.2.2.5. 其他方法..................................................................21 2.2.3. 微粒之應用.............................................................................21 2.2.3.1. 藥物控制釋放之應用..............................................21 2.2.3.2. 微載體(microcarrier)之應用...................................23 目錄 VIII 2.2.3.3. 等溫吸附模式簡介..................................................23 2.3. 多孔性幾丁聚醣基材之製備........................................................25 2.3.1. 非溶劑相分離法.....................................................................25 2.3.2. 溫度誘導相分離.....................................................................25 2.3.3. 冷凍凝膠法.............................................................................27 2.4. 影響多孔性幾丁聚醣微粒型態的因素........................................29 2.4.1. 界面活性劑的種類.................................................................29 2.4.2. 界面活性劑的用量及兩相間比例的影響............................29 2.4.3. 冷凍溫度的影響.....................................................................30 2.4.4. 攪拌轉速的影響.....................................................................30 2.4.5. 其他因素的影響.....................................................................30 2.5. 先前研究對乳化/冷凍凝膠法之探討...........................................36 2.5.1. 不同流場對乳化效果的影響................................................36 2.5.2. 冷凍步驟.................................................................................36 2.5.3. 冷凍時間.................................................................................36 2.5.4. 界面活性劑種類及添加量....................................................37 2.5.5. 攪拌轉速.................................................................................37 3. 實驗藥品、儀器及方法...............................................................................39 3.1. 實驗藥品........................................................................................39 3.1.1. 多孔性幾丁聚醣微粒製備所需藥品....................................39 3.1.2. 多孔性幾丁聚醣微粒吸附應用測試所需藥品....................40 3.2. 實驗儀器........................................................................................40 3.2.1. 一般儀器.................................................................................40 3.2.2. 多孔性幾丁聚醣微粒製備儀器............................................40 3.2.3. 多孔性幾丁聚醣微粒性質測定............................................41 3.2.4. 多孔性幾丁聚醣微粒之BSA負載量測定.............................41 3.3. 實驗方法........................................................................................42 3.3.1. 多孔性幾丁聚醣微粒製備裝置............................................42 3.3.2. 多孔性幾丁聚醣微粒製備分析............................................43 3.3.2.1. 不同HLB值的影響..................................................43 3.3.2.2. 不同混合型界面活性劑之影響..............................44 3.3.2.3. 連續相、分散相、界面活性劑比例之影響..........45 3.3.2.4. 不同冷凍溫度之影響..............................................46 3.3.3. 多孔性幾丁聚醣微粒之性質測定........................................47 3.3.3.1. 多孔性幾丁聚醣微粒粒徑大小及分布..................47 3.3.3.2. 多孔性幾丁聚醣微粒產量......................................48 3.3.3.3. 多孔性幾丁聚醣微粒之SEM結構觀察.................48 3.3.3.4. 多孔性幾丁聚醣微粒之吸水能力..........................48 目錄 IX 3.3.3.5. 傅立葉轉換紅外線光譜(FTIR)測定......................49 3.3.4. 多孔性幾丁聚醣微粒之BSA負載量測定.............................49 4. 結果與討論...................................................................................................51 4.1. HLB值對微粒的影響....................................................................51 4.2. 混合型界面活性劑對微粒的影響................................................58 4.3. 兩相及界面活性劑間之比例對微粒的影響................................66 4.4. 冷凍溫度對微粒之影響................................................................81 4.5. 多孔性幾丁聚醣微粒之吸水能力................................................90 4.6. 多孔性幾丁聚醣微粒之BSA負載量............................................93 5. 結論與未來方向...........................................................................................99 5.1. 結論................................................................................................99 5.2. 未來研究方向..............................................................................101 參考文獻............................................................................................................1037544282 bytesapplication/pdfen-US幾丁聚醣多孔性ChitosanPorousthesishttp://ntur.lib.ntu.edu.tw/bitstream/246246/52257/1/ntu-96-R94524033-1.pdf