臺灣博碩士論文加值系統

對許多牙科執業醫師而言，牙本質過敏症是很常見的主訴，卻也是很棘手的難題。目前市面上有許多號稱能有效緩解牙齒敏感症狀的商品，但卻沒有任何產品能立即而持久的療效。本團隊所研發之第一代含氧化鈣中孔洞二氧化矽材料，已被證實能有效進入牙本質小管內，產生深達100μm的結晶，且使用液體流動模組測試牙本質通透性，發現其可將牙本質滲透性降低至19.1%。但在綠色化學觀念抬頭的二十一世紀，以更環保的方法製造有效材料，是本團隊努力的方向。除此之外，本團隊更進一步探討以中孔洞鈣矽材料治療牙本質過敏症的優勢，並評估其在活體的效用性與生物相容性。本實驗主要分成三個部分，首先，本團隊先合成以明膠為模版之中孔洞鈣矽材料，將其與不同體積之30%磷酸混和，探討在不同pH值下的製劑對牙本質小管的封閉情形，發現當製劑pH值在5.0~5.5時，能在不酸蝕牙本質結構的情形下，在牙本質小管內產生深達30μm以上的結晶。第二部分，則以鈣離子釋放量以及碳酸鈣與中孔洞二氧化矽混和方式，探討以中孔洞鈣矽材料治療牙本質過敏症的優勢。實驗結果發現，將碳酸鈣含浸於二氧化矽顆粒的孔洞內，與磷酸溶液混和後才能產生過飽和的鈣離子與磷酸根離子溶液，且中孔洞二氧化矽顆粒能扮演反應槽的角色吸附酸液，並扮演結晶的起始點，使得此製劑相較於碳酸鈣/30%磷酸製劑與碳酸鈣/中孔洞二氧化矽/30%磷酸製劑，能更有效且不破壞牙本質結構的情形下，封閉牙本質小管。第三部分，則進行動物實驗以評估此製劑在活體的效用性與對牙髓組織的刺激性。在電子顯微鏡觀察下，發現本製劑在活體內有牙髓腔靜水壓存在下，仍可在牙本質小管內產生超過30μm的結晶。而比較中孔洞鈣矽材料/30%磷酸製劑與市售產品Seal and Protect與負對照組IRM對牙髓組織的刺激性，發現三者並無統計上顯著差異。
結論：(1) 中孔洞鈣矽材料/30%磷酸製劑在pH 5.0~5.5時，能在不酸蝕牙本質的情形下有效封閉牙本質小管。(2) 將碳酸鈣含浸於二氧化矽顆粒的孔洞內，與磷酸溶液混和後才能產生過飽和的鈣離子與磷酸根離子溶液，在不破壞牙本質的情形下有效封閉牙本質小管。(3)在動物實驗中證實，本製劑在活體內仍內有效封閉牙本質小管，且對牙髓組織無顯著刺激性。

Dentin hypersensitivity is a common encountered chief complaint for dental general practitioner, but it is also a troublesome issue. There are various kinds of commercial products which claim to be able to relieve the symptoms of dentin hypersensitivity, but none of the products have immediate and long-lasting effects. The first generation of CaO@mesoporous silica developed by our group was proved to be effective in occlusion of the dentinal tubules with recrystallized precipitants penetrating into the tubules as deep as 100 μm. Also, after application of Cao@mesoporous silica paste mixing with 30% phosphoric acid, the permeability of dentin disc decreased to 19.1% when evaluated by fluid flow model.
With the advocation of green chemistry in the 21st century, it is our goal to develop efficient materials in a more environmentally friendly way. In addition, we also tried to investigate the advantages using mesoporous calcium silicate materials for the treatment of dentin hypersensitivity, and evaluate its in vivo efficacy and biocompatibility. This research comprised of three parts. First, we developed the gelatin-templated calcium silicate material, and mixing it with different volumes of 30% phosphoric acid, and evaluate the efficacy of occlusion of dentinal tubules by using pastes with different pH value. The results showed that by using pastes with the pH value between 5.0~5.5, the dentinal tubules could be occluded by precipitates as deep as 30μm without eroding the dentin. The second part investigated the advantages of mesoporous calcium silicate material by measuring calcium ion concentration and evaluation the efficacy by mixing calcium carbonate and mesoporous silica in different ways. The results revealed that only by impregnating calcium carbonate in the nano pores of mesoporous silica could the paste be hypersaturated with calcium ions and phosphate ions. Also, the mesoporous silica played the role of acid adsorption and the starting point of nucleation, which enabled the paste occlude the dentinal tubules efficiently without eroding the dentin. In the third part, we evaluated the in vivo efficacy and biocompatibility of the desensitizing paste. Under SEM observation, we found precipitates penetrated more than 30μm despite the presence of pulpal hydrostatic pressure. As to the pulp irritation, we found that there were no significant differences among our desensitizing paste, commercial products Seal & Protect, and the negative control IRM.
In conclusion：(1) Mesoporous calcium silicate material mixing with 30% phosphoric acid could effectively occlude the dentinal tubules without eroding the dentin. (2) Only by impregnating calcium carbonate in the nano pores of mesoporous silica could the paste be hypersaturated with calcium ions and phosphate ions, which enabled the dentinal tubules be occluded without being eroded. (3) Animal study demonstrated that the paste could effectively occlude the dentinal tubules in vivo without irritating the pulp.

中文摘要 i
Abstract iii
目 錄 v
圖 次 ix
表 次 xii
第一章 前言 1
第二章 文獻回顧 4
2.1 牙本質過敏症的定義 4
2.2 牙本質過敏症盛行率 4
2.3 牙本質過敏症致病因子 5
2.3.1 牙本質曝露 5
2.3.2 牙本質小管開口通暢 6
2.4 牙本質過敏症的機制 8
2.4.1 造牙本質細胞感覺接受器理論 8
2.4.2 神經支配理論 8
2.4.3 流體力學理論 9
2.5 牙本質滲透性 10
2.6 牙本質過敏症治療材料與方法 12
2.6.1 化學性減敏方法 12
2.6.2 物理性減敏方法 17
2.7 生醫玻璃的應用 20
2.8 孔洞材料原理 21
2.8.1 中孔洞分子篩 21
2.8.2 中孔洞分子篩的性質與應用 22
2.9 奈米孔洞材料 23
2.9.1 中孔洞二氧化矽模板 23
2.9.2 結合金屬氧化物與中孔洞二氧化矽 24
2.10動物實驗 25
第三章 動機與目的 28
第四章 材料與方法 30
4.1 製備去敏感材料 30
4.1.1 以明膠為模版之中孔洞鈣矽材料之製作－Ca：Si= 1：1 30
4.1.2 含氧化鈣中孔洞二氧化矽製劑之準備 31
4.2 觀察及比較不同含中孔洞鈣矽材料/30%磷酸製劑對牙本質小管封閉效果 31
4.2.1 牙本質試片之製備 31
4.2.2 評估不同中孔洞鈣矽材料/30%磷酸製劑對牙本質試片的影響 32
4.2.3 掃描式電子顯微鏡之觀察： 32
4.3中孔洞鈣矽材料粉末與中孔洞鈣矽材料/30%磷酸製劑之性質分析 32
4.3.1 測量中孔洞鈣矽材料粉末與不同中孔洞鈣矽材料/30%磷酸製劑之酸鹼值 33
4.3.2 以明膠為模版之中孔洞二氧化矽粉末與中孔洞鈣矽材料之電子顯微鏡觀察 33
4.3.3中孔洞鈣矽材料/30%磷酸製劑之電子顯微鏡觀察 33
4.3.4 X光繞射分析(XRD) 33
4.4碳酸鈣粉末以及碳酸鈣/30%磷酸製劑之性質分析以及對於牙本質小管封閉效果之評估： 34
4.4.1碳酸鈣粉末之電子顯微鏡觀察 34
4.4.2 測量碳酸鈣粉末以及碳酸鈣/30%磷酸製劑之酸鹼值 34
4.4.3 評估碳酸鈣/30%磷酸製劑對於牙本質小管之封閉效果 34
4.5 物理混和之碳酸鈣/中孔洞二氧化矽粉末以及碳酸鈣/中孔洞二氧化矽/30%磷酸製劑之性質分析以及對於牙本質小管封閉效果之評估： 35
4.5.1測量物理混和之碳酸鈣/中孔洞二氧化矽粉末以及碳酸鈣/中孔洞二氧化矽/30%磷酸製劑之酸鹼值 35
4.5.2評估碳酸鈣/中孔洞二氧化矽/30%磷酸製劑對牙本質小管之封閉效果 36
4.6 鈣離子釋放量 36
4.6.1 待測溶液之配製 36
4.6.2 鈣離子濃度之測量 37
4.7 動物實驗 37
4.7.1 實驗動物之選擇與照顧 37
4.7.2實驗動物之麻醉 37
4.7.3實驗步驟 38
第五章 結果 42
5.1觀察及比較不同含中孔洞鈣矽材料/30%磷酸製劑的酸鹼值，並評估其對牙本質小管封閉效果 42
5.1.1中孔洞鈣矽材料粉末及不同含中孔洞鈣矽材料/30%磷酸製劑之酸鹼值 42
5.1.2 掃描式電子顯微鏡之觀察評估製劑對牙本質小管的封閉效果 43
5.2中孔洞鈣矽材料粉末與中孔洞鈣矽材料/30%磷酸製劑之性質分析 44
5.2.1以明膠為模版之中孔洞二氧化矽粉末與中孔洞鈣矽材料之電子顯微鏡觀察 44
5.2.2 X光繞射分析(XRD) 44
5.2.3 以掃描式電子顯微鏡觀察中孔洞鈣矽材料/30%磷酸製劑結晶過程 45
5.3 碳酸鈣粉末與碳酸鈣/30%磷酸製劑的性質分析，並評估其對牙本質小管封閉效果 45
5.3.1 碳酸鈣粉末的電子顯微鏡觀察 45
5.3.2與碳酸鈣/30%磷酸製劑的酸鹼值測量(圖5-16) 45
5.3.3掃描式電子顯微鏡之觀察評估碳酸鈣/30%磷酸製劑對牙本質小管的封閉效果 46
5.4 碳酸鈣/中孔洞二氧化矽粉末與碳酸鈣/中孔洞二氧化矽/30%磷酸製劑的性質分析，並評估其對牙本質小管封閉效果 47
5.4.1 碳酸鈣/中孔洞二氧化矽粉末與碳酸鈣/中孔洞二氧化矽/30%磷酸製劑的酸鹼值測量(圖5-17) 47
5.4.2 掃描式電子顯微鏡之觀察評估碳酸鈣/中孔洞二氧化矽/30%磷酸製劑對牙本質小管的封閉效果 47
5.5 鈣離子釋放量 48
5.5.1 比較同一時間點，不同材料的鈣離子釋放量 48
5.5.2 比較同一材料，在不同時間點的鈣離子釋放量 49
5.6 動物實驗 50
5.6.1 活體有效性測試 50
5.6.2牙髓刺激性測試 50
第六章 討論 52
第七章 結論 63
第八章 未來研究方向 65
參考文獻 67



圖 次
圖4-1 慢速鋸片機 75
圖4-2場發射式電子顯微鏡 75
圖4-3桌上型電子顯微鏡 76
圖4-4桌上型酸鹼度測定儀 76
圖4-5 液態凍凝(Nitrogen slush)真空槽 77
圖4-6 X光繞射分析儀 77
圖4-7離子層析儀(Ion chromatography, Metrohm, Switzerland) 78
圖5-1中孔洞鈣矽材料粉末及不同含中孔洞鈣矽材料/30%磷酸製劑之酸鹼值 78
圖5-2 pH值6.5~7.0之中孔洞鈣矽材料/30%磷酸製劑塗抹於牙本質試片表面，作用10分鐘後，牙本質小管封閉情形 (a)1500x, (b) 5000x 79
圖5-3 pH值5.0~5.5之中孔洞鈣矽材料/30%磷酸製劑塗抹於牙本質試片表面，作用10分鐘後，牙本質小管封閉情形 (a) 3000x,(b) 5000x 80
圖5-3 pH值5.0~5.5之中孔洞鈣矽材料/30%磷酸製劑塗抹於牙本質試片表面，作用10分鐘後，牙本質小管封閉情形(c) 20000x 81
圖 5-4 pH值4.5~5.0之中孔洞鈣矽材料/30%磷酸製劑塗抹於牙本質試片表面，作用10分鐘後，牙本質小管封閉情形 (a) 1500x 81
圖 5-4 pH值4.5~5.0之中孔洞鈣矽材料/30%磷酸製劑塗抹於牙本質試片表面，作用10分鐘後，牙本質小管封閉情形 (b) 5000x, (c) 5000x 82
圖5-5 pH值約2.5~3.0之中孔洞鈣矽材料/30%磷酸製劑塗抹於牙本質試片表面，作用10分鐘後，牙本質小管封閉情形(a) 1500x,(b) 15000x 83
圖5-6 以掃描式電子顯微鏡觀察以明膠為模版之中孔洞二氧化矽粉末(15000x) 84
圖5-7 以穿透式電子顯微鏡觀察以明膠為模版之中孔洞二氧化矽粉末 84
圖5-8 以掃描式電子顯微鏡觀察以明膠為模版合成之中孔洞鈣矽材料(15000x) 85
圖5-9 以以明膠為模版合成之中孔洞鈣矽材料X光繞射圖 85
圖5-10中孔洞鈣矽材料/30%磷酸製劑(粉液比=1：2)X光繞射圖 86
圖5-11 中孔洞鈣矽材料/30%磷酸製劑剛混和時結晶型態(a) 5000x 86
圖5-11 中孔洞鈣矽材料/30%磷酸製劑剛混和時結晶型態(b) 15000x 87
圖5-12中孔洞鈣矽材料/30%磷酸製劑混和後5分鐘的結晶型態(a) 5000x 87
圖5-12中孔洞鈣矽材料/30%磷酸製劑混和後5分鐘的結晶型態(b) 15000x 88
圖5-13中孔洞鈣矽材料/30%磷酸製劑混和後15分鐘的結晶型態(a) 5000x 88
圖5-13中孔洞鈣矽材料/30%磷酸製劑混和後15分鐘的結晶型態(b) 15000x 89
圖5-14中孔洞鈣矽材料/30%磷酸製劑混和後20分鐘的結晶型態(a) 1500x 89
圖5-14中孔洞鈣矽材料/30%磷酸製劑混和後20分鐘的結晶型態(b) 5000x 90
圖5-15碳酸鈣粉末的結晶型態(4000x) 90
圖5-16碳酸鈣粉末及不同碳酸鈣/30%磷酸製劑之酸鹼值 91
圖5-17 pH值約5.0~5.5之碳酸鈣/30%磷酸製劑塗抹於牙本質試片表面，作用10分鐘後，牙本質小管封閉情形(a) 1500x 91
圖5-17 pH值約5.0~5.5之碳酸鈣/30%磷酸製劑塗抹於牙本質試片表面，作用10分鐘後，牙本質小管封閉情形(b) 10000x 92
圖5-18碳酸鈣/中孔洞二氧化矽粉末與碳酸鈣/中孔洞二氧化矽/30%磷酸製劑的酸鹼值測量 92
圖5-19 pH值約5.0~5.5之碳酸鈣/中孔洞二氧化矽/30%磷酸製劑塗抹於牙本質試片表面，作用10分鐘後，牙本質小管封閉情形(a) 1500x,(b) 5000x 93
圖5-20 鈣離子釋放量 94
圖5-21 中孔洞鈣矽材料/30%磷酸製劑於活體封閉牙本質小管(a)1500x 94
圖5-21 中孔洞鈣矽材料/30%磷酸製劑於活體封閉牙本質小管(b)10000x, (c) 30000x 95
圖5-22 Seal & Protect®於活體封閉牙本質小管(a)1500x, (b) 3000x 96
圖5-23 玻璃離子體於活體封閉牙本質小管(a)3000x, (b) 10000x 97
圖5-24 電子顯微鏡觀察玻璃離子體型態(30000x) 98
圖5-25 中孔洞鈣矽材料/30%磷酸製劑塗抹於活體牙本質七天後，牙髓組織型態觀察(a) 400x 98
圖5-25 中孔洞鈣矽材料/30%磷酸製劑塗抹於活體牙本質七天後，牙髓組織型態觀察(b) 400x 99
圖5-26圖5-25 Seal & Protect®塗抹於活體牙本質七天後，牙髓組織型態觀察
(400x) 99
圖5-27 負對照組IRM覆蓋於活體牙本質七天後，牙髓組織型態觀察(a) 400x,
(b) 400x 100
圖5-28 Seal & Protect®塗抹於活體牙本質70天後，牙髓組織型態觀察(400x) 101





表 次
表4-1 本研究所使用之相關儀器 102
表4-2 本實驗所使用之化學藥品 103
表4-2 本實驗所使用之化學藥品 103
表4-3 牙髓刺激性實驗分組 103
表4-5 本研究所使用去敏感劑之成分及使用方式 104
表4-6 牙髓刺激性實驗牙髓組織發炎程度分級標準 105
表5-1 粉末的鈣離子釋放量統計分析結果 106
表5-2 與磷酸混和後鈣離子釋放量統計分析結果 107
表5-3 與磷酸混和後1分鐘鈣離子釋放量統計分析結果 108
表5-4 與磷酸混和後5分鐘鈣離子釋放量統計分析結果 109
表5-5 與磷酸混和後10分鐘鈣離子釋放量統計分析結果 110
表5-6 與磷酸混和後15分鐘鈣離子釋放量統計分析結果 111
表5-7 以明膠為模版之中孔洞鈣矽材料/30%磷酸製劑不同時間點的鈣離子釋放量 112
表5-8 以MCF為模版之中孔洞鈣矽材料/30%磷酸製劑不同時間點的鈣離子釋放量 113
表5-9 以碳酸鈣為模版之中孔洞鈣矽材料/30%磷酸製劑不同時間點的鈣離子釋放量 114
表5-10以生醫玻璃Novamin為模版之中孔洞鈣矽材料/30%磷酸製劑不同時間點的鈣離子釋放量 115
表5-11 牙髓刺激性實驗結果：發炎反應分數 116
表5-12牙髓刺激性實驗：塗抹中孔洞鈣矽材料/30%磷酸製劑、Seal & Protect和IRM七天後牙髓組織發炎評分之統計分析結果 116
表5-13牙髓刺激性實驗：塗抹中孔洞鈣矽材料/30%磷酸製劑、Seal & Protect和IRM 28天後牙髓組織發炎評分之統計分析結果 117
表5-14牙髓刺激性實驗：塗抹中孔洞鈣矽材料/30%磷酸製劑、Seal & Protect和IRM 70天後牙髓組織發炎評分之統計分析結果 117
表5-15牙髓刺激性實驗：塗抹中孔洞鈣矽材料/30%磷酸製劑後7天、28天及70天後牙髓組織發炎評分之統計分析結果 118
表5-16牙髓刺激性實驗：塗抹Seal & Protect後7天、28天及70天後牙髓組織發炎評分之統計分析結果 118
表5-17牙髓刺激性實驗：以IRM覆蓋牙本質後7天、28天及70天後牙髓組織發炎評分之統計分析結果 119

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