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研究生：	丁冠中 Ding, Guan-Jhong
論文名稱：	水分散性聚氨酯/聚麩胺酸/三鈣磷酸鹽複合支架之製備與特性分析 Preparation and characterization of waterbased poly(urethane) / poly(γ-glutamate) / tricalcium phosphate composite scaffolds
指導教授：	林睿哲 Lin, Jui-Che
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2010
畢業學年度：	98
語文別：	中文
論文頁數：	124
中文關鍵詞：	支架、水分散性聚氨酯、三鈣磷酸鹽、聚麩胺酸
外文關鍵詞：	scaffolds, water-based polyurethane, tricalcium phosphate, poly(γ-glutamate)
相關次數：	點閱：86 下載：1
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本實驗主要目的為研製出新型具組織可吸收性的骨替代材料，以水分散性聚氨酯為基材，並摻混β型三鈣磷酸鹽與聚麩胺酸製備成孔洞複合支架。
實驗結果顯示經聚麩胺酸改質後的聚氨酯具有較小的接觸角及較高的吸水量，體外血小板貼附實驗結果得知，將聚麩胺酸摻混至聚氨酯中，會降低血小板在聚氨基甲酸酯表面上的貼附數目及活化程度。實驗結果亦指出以NCO/OH=1.8及DMPA=6wt%之比例所合成出的水分散性聚氨酯具有較大的拉伸強度，以及較適當的粒徑大小、吸水率與降解率。
本實驗利用掃描式電子顯微鏡觀察、X光繞射分析、傅利葉紅外線光譜儀、接觸角測試、孔隙度分析、吸水率測試、壓縮強度測試、降解率測試來觀察複合支架的表面型態與整體性質。結果顯示複合支架具有相互連通之孔洞，聚麩胺酸添加量提高會使得複合支架的壓縮強度降低，但親水性、吸水率、降解率、孔隙度與孔徑大小皆隨著聚麩胺酸添加量的提高而增加。並利用X光繞射分析與傅利葉紅外線光譜儀來判定三鈣磷酸鹽的晶相與複合支架的組成。

Novel porous composite scaffolds for bone tissue engineering were prepared from water-based polyurethane (WPU), tricalcium phosphate (TCP) and poly(γ-glutamate) (γ-PGA).
γ-PGA modified commercially available pellethane exhibit a smaller contact angle, and higher water absorption value than the pellethane without γ-PGA. In vitro platelet adhesion studies indicated that the addition of γ-PGA into pellethane leads to a reduction in platelet adhesion and activation. Results indicated that NCO/OH=1.8 and DMPA=6wt% of water-based polyurethane(WPU) had superior tensile strength, adequate particle size, swelling ratio, degradation ratio.
The morphology and properties of the scaffolds were characterized by scanning electron microscope, X-ray diffraction, infrared absorption spectra, static contact angle analysis, porosity analysis, swelling ratio, compressive strength testing, and in vitro degradation measurement. The results indicated that the porous composite scaffolds had an interconnected porous structure. The compressive strength of the porous composite scaffolds showed lower enhancement with increasing γ-PGA content. The hydrophilic, swelling ratio, degradation raio, porosity and pore size of the porous composite scaffolds showed higher value with increasing γ-PGA content. X-ray diffraction and Fourier transform infrared spectroscopy were used to determine the crystal structure and chemical composition of scaffolds.

目錄………………….………………………………………………….Ⅰ
圖目錄…………………………………………………………………..Ⅵ
表目錄…………………………………..………………………………Ⅷ
 
第一章	  緒論............................................................................................1
1-1  前言......................................................................................1
1-2  硬骨組織工程......................................................................2
1-3  凝血機制..............................................................................4
1-4  生醫支架材料應具備的條件..............................................7
1-5  聚氨脂..................................................................................8
     1-5-1  聚氨脂發展.............................................................8
     1-5-2  聚氨酯簡介.............................................................9
1-6  水分散性聚氨酯組成....................................................11
     1-6-1  二異氰酸酯...........................................................11
     1-6-2  軟鏈段……….......................................................14
     1-6-3  非離子型鏈延長劑...............................................15
     1-6-4  離子型鏈延長劑...................................................17
     1-6-5  催化劑...................................................................18
1-7  研究動機............................................................................19
第二章   文獻回顧................................................................................21
       2-1  骨骼...................................................................................21
       2-2  生醫骨骼材料的分類.......................................................24
         2-2-1  天然骨骼材料.....................................................24
         2-2-2  人工合成骨骼材料.............................................26
       2-3  生醫孔洞支架...................................................................29
         2-3-1  生醫孔洞支架發展.............................................29
         2-3-2  生醫孔洞支架製備方法.....................................31
2-3-3  生醫孔洞支架之特性.........................................33
       2-4  影響血液相容性的因素...................................................34
            2-4-1　親水性表面.........................................................34
            2-4-2  負電荷的表面.....................................................35
2-5  聚麩胺酸...........................................................................36
2-6  三鈣磷酸鹽.......................................................................39
2-7　聚己內酯...........................................................................43
2-8  戊二醛...............................................................................44
2-9  水分散性聚氨酯...............................................................46
2-9-1  DMPA添加量的影響.......................................46
            2-9-2  軟鏈段的影響………………………………….47
2-9-3  分散機制...........................................................48
2-9-4  水分散性聚氨酯製備方法...............................48

第三章   實驗材料與方法....................................................................56
       3-1  藥品...................................................................................56
3-2  實驗儀器...........................................................................59
3-3  實驗流程......................................... .................................60
3-3-1  Pellethane摻混聚麩胺酸....................................60
3-3-2  水分散性聚氨酯之合成.....................................60
3-3-3  部分離子化聚麩胺酸.........................................62
3-3-4  三鈣磷酸鹽粉末處理.........................................62
3-3-5  複合支架製備......................................................62
            3-3-6  複合支架交聯與清洗......................... ...............64
       3-4  材料特性分析...................................................................65
            3-4-1  傅立葉轉換紅外線光譜儀.................................65
            3-4-2  X-ray繞射分析儀...............................................65
            3-4-3  粒徑分析儀.........................................................65
            3-4-4  孔隙度測試.........................................................66
            3-4-5  機械強度測試.....................................................67
            3-4-6  接觸角測試.........................................................68
            3-4-7  吸水率測試.........................................................69
            3-4-8  降解率測試.........................................................70
            3-4-9  血小板貼附性分析.............................................71
            3-4-10 表面型態觀察.....................................................74
            3-4-11 統計分析方法......................................................74

第四章   結果與討論............................................................................75
      4-1  探討聚麩胺酸對聚氨酯血液相容性的影響....................75
           4-1-1  薄膜液面下接觸角..............................................77
           4-1-2  薄膜吸水率測試..................................................79
           4-1-3  血小板貼附性分析...............................................82
      4-2  水分散性聚氨酯之合成.....................................................82
           4-2-1  粒徑測試...............................................................85
           4-2-2  水分散性聚氨酯機械性質測試...........................87
           4-2-3  水分散性聚氨酯液面上接觸角測試...................88
           4-2-4  水分散性聚氨酯吸水率測試..........................89
           4-2-5  水分散性聚氨酯降解率測試............................90
      4-3  複合支架之製備與特性分析.............................................90
4-3-1  複合支架摻混比例測試.......................................90
           4-3-2  傅利葉紅外線光譜...............................................92
           4-3-3  三鈣磷酸鹽XRD分析..........................................97
           4-3-4  薄膜液面上接觸角測試.......................................99
           4-3-5  複合支架孔隙度測試........................................100
           4-3-6  複合支架吸水率測試........................................102
           4-3-7  複合支架降解率測試........................................103
           4-3-8  複合支架機械性質測試....................................104
           4-3-9  複合支架孔洞型態觀察.................................106

第五章   總結……………..................................................................112
參考文獻................................................................................................114

圖目錄
圖1-1 組織工程關係圖............................................................................3
圖1-2 血小板結構....................................................................................4
圖1-3 二異氰酸酯的反應形式.................... .........................................13
圖1-4 合成聚氨酯常用之觸媒..............................................................18
圖2-1 生醫孔洞支架的階段發展..........................................................30
圖2-2  γ-PGA結構 (a) ionic γ-PGA, and (b) H-form γ-PGA…….…..38
圖2-3  Hoerstrupum於可降解之動脈基材的研究流程.......................38
圖2-4  HA/TCP於1150℃~1300℃煅燒之XRD繞射圖......................39
圖2-5 磷酸鈣陶瓷做為骨骼替代材料所具有的骨鍵結能力..............42
圖2-6 磷酸鈣陶瓷與骨細胞在骨組織修復所產生微環境的變化…..42
圖2-7 聚氨酯粒子中和前後示意圖......................................................50
圖2-8 預聚物混合法..............................................................................51
圖2-9 丙酮法..........................................................................................54
圖3-1 水分散性聚氨酯合成步驟..........................................................61
圖3-2 生醫孔洞複合支架製備流程圖..................................................63
圖3-3 生醫孔洞複合支架交聯與清洗流程圖......................................64
圖4-1 血小板貼附情形..........................................................................80
圖4-2 水分散性聚氨酯吸水率..............................................................88
圖4-3 水分散性聚氨酯WPU-1.8-6 FTIR圖譜.....................................94
圖4-5 聚麩胺酸離子化前後疊圖..........................................................95
圖4-6 不同比例之複合支架交聯前疊圖...............................................96
圖4-9 (a) β-TCP繞射圖譜; (b) β-TCP標準繞射圖譜.........................98
圖4-10複合支架之吸水率....................................................................102
圖4-11複合支架之降降解....................................................................103
圖4-12複合支架壓縮性質....................................................................105
圖4-13 複合支架交聯前孔洞型態......................................................107
圖4-14 複合支架交聯後之表面型態..................................................109
圖4-15 複合支架交聯後之截面型態...................................................111
表目錄
表1-1 血小板之五個階段型態變化........................................................6
表1-2 合成聚氨酯生醫材料常用的二異氰酸酯. ................................12
表1-3 合成聚氨酯生醫材料常用的軟鏈段..........................................14
表1-4 合成聚氨酯生醫材料常用的非離子型鏈延長劑......................16
表3-1  Hepes-Tyrodes緩衝溶液之組成................................................73
表4-1  Pellethane摻混不同量γ-PGA後之液面下接觸角...................76
表4-2  Pellethane摻混不同量γ-PGA後之吸水率...............................78
表4-3 薄膜上血小板貼附數目………………………………………..80
表4-4 水分散性聚氨酯合成條件..........................................................82
表4-5 水分散性聚氨酯粒徑大小..........................................................84
表4-6 水分散性聚氨酯拉申強度與伸長率..........................................86
表4-7 水分散性聚氨酯液面上接觸角..................................................87
表4-8 水分散性聚氨酯降解率..............................................................89
表4-9複合支架浸泡於37℃之PBS中兩天的降解率……………..….91
表4-10薄膜液面上接觸角......................................................................99
表4-11複合支架交聯前後之孔隙度....................................................101
表4-12複合支架之壓縮強度................................................................104
                                    

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