隨科技發達，人們之生活與飲食習慣使全球之糖尿病患者人數逐年攀升，因此，自我檢測血糖的需求增加，然而並非所有人皆能克服扎針採血之恐懼。因此，本研究希望透過非侵入式之唾液葡萄糖感測概念，提升病友對於檢測之意願，其唾液葡萄糖之感測電極主要由網版印刷電極作為工作電極，並利用奈米碳管、全氟磺酸基聚合物與葡萄糖氧化酶進行修飾，製備出一款輕便、高靈敏度、寬檢測範圍與專一性佳之葡萄糖感測電極。
本研究利用超聲波震盪製備奈米複合材料(Nf-CNT)，並利用滴鑄法以一滴之形式(One drop)將其修飾於經電漿清洗之網版印刷電極(Nf-CNT/SPE)，而後分別利用改變濃度與電漿轟擊之手段調整電極狀態再將葡萄糖氧化酶修飾於上(GOx/Nf-CNT/SPE)，並利用多種材料分析儀器搭配電化學之循環伏安法與阻抗頻譜法探究不同參數與各階段之電極其結構與性質之改變，進行葡萄糖感測，並藉由該電極之特性對其感測表現進行分析與比較。依據本研究之結果，經奈米複合材料之修飾，電子傳輸效率與反應表面積提升，此外，適當之電漿轟擊使最上層之奈米碳管露出，同時亦保有固定電極之全氟磺酸基聚合物，並且使材料親水化，使葡萄糖氧化酶之修飾更為均勻與貼合，感測結果顯示，經電漿處理之1分鐘之Nf-CNT/SPE製備而成之電極具有最佳之感測表現，其靈敏度高達99.13 μA/mMcm2，線性範圍為 20 – 700 μM，於涵蓋健康個體與糖尿病患者之唾液葡萄糖濃度中，表現其高靈敏度、高專一性之表現，顯示其應用於實際唾液葡萄糖感測之潛力。

The population of subjects with diabetes increases due to unhealthy lifestyle. Therefore, the needs for self monitoring of blood glucose (SMBG) increases. However, not all the people could tolerate and overcome the fear of jabbing of needle. Thus, we aim to take a noninvasive measurement that measures of the glucose concentration in saliva to raise up the willingness of the patients. The combination of glucose sensing electrode includes a screen-printed electrode (SPE) that serves as working electrode, conductive and biocompatible Nafion-carbon nanotubes nano-composite (Nf-CNT), and the glucose oxidase (GOx).
In this work, we prepare Nf-CNT by ultrasonication and drop cast it onto the SPE. After that, we adjust the parameters by using different addition of CNT and various time of plasma treatment to Nf-CNT/SPE. Finally, GOx is drop casted the on it. To further investigate the properties and electrochemical performance, various kinds of material analysis instruments and cyclic voltammetry are used. Meanwhile, glucose sensing is taken and we will get the calibration curve. Based on the results, electron transfer efficiency and active area increase due to the coating of the nano-composite. Besides, proper plasma treatment to the Nf-CNT/SPE not only makes the electrode hydrophilic, but it also let the CNT on the surface of the Nf-CNT layer exposed. In this way, GOx could get more closed to the CNT and coat on the Nf-CNT/SPE more uniformly. According to the sensing results, GOx/1 min-Nf-CNT/SPE shows the best performance which the sensitivity is 99.13 μA/mMcm2 and linear range is 20 – 700 μM. The result indicates high potential of the electrode applied to the diabetes diagnosis.

摘要 I
Abstract II
誌謝 III
目次 IV
表目次 VIII
圖目錄 IX
第一章 緒論 1
1.1 前言 1
1.2 研究動機 2
第二章 文獻回顧 3
2.1 糖尿病 3
2.1.1 糖尿病症狀與分類 4
2.1.2 糖尿病之檢測方式 5
2.2 唾液葡萄糖感測方法與機制 7
2.3 葡萄糖感測之種類與發展 10
2.3.1 以光學方式感測葡萄糖 10
2.3.2 以電化學方法感測葡萄糖 12
2.3.2.1 電化學感測葡萄糖之機制 12
2.3.2.2 第一世代葡萄糖感測器 13
2.3.2.3 第二世代葡萄糖感測器 15
2.3.2.4 第三世代葡萄糖感測器 16
2.3.2.5 第四世代葡萄糖感測器 17


2.3.3 葡萄糖感測電極基材選擇 18
2.3.3.1 玻璃碳電極基材 18
2.3.3.2 貴金屬電極基材 20
2.3.3.3 導電玻璃基材 22
2.3.3.4 網版印刷電極基材 24
2.4 修飾葡萄糖感測電極之材料 26
2.4.1 碳材料應用於電極修飾 26
2.4.2 高分子應用於電極修飾 27
2.5 本實驗室於葡萄糖感測之回顧27
第三章 實驗方法 29
3.1 實驗藥品 30
3.2 實驗製程設備 32
3.3 電極製備流程 33
3.3.1 單極網版印刷電極之前處理 34
3.3.2 奈米碳管之酸處理 34
3.3.3 稀釋全氟磺酸基聚合物 35
3.3.4 利用滴鑄法修飾電極 35
3.3.5 利用電漿轟擊已修飾之電極 36
3.3.6 利用滴鑄法將酵素修飾於電極36
3.4 材料分析儀器與電化學感測 37
3.4.1 感測電極之材料分析儀器 37
3.4.1.1 傅立葉轉換紅外線光譜 37
3.4.1.2 冷場發射掃描式電子顯微鏡 37
3.4.1.3 能量色散X射線能譜儀 38
3.4.1.4 拉曼能譜儀 39
3.4.1.5 微阻邏輯錶 39
3.4.1.6 影像式接觸角量測儀 39
3.4.1.7 原子力顯微鏡 40
3.4.1.8 X射線光電子能譜儀40
3.4.2 感測電極之電化學與葡萄糖感測效能分析41
3.4.2.1 循環伏安法測試與阻抗測試頻譜分析 42
3.4.2.2 實驗之電解液與葡萄糖待測液配置 43
3.4.2.3 電極反應表現定義 44
第四章 結果與討論 45
4.1 酸處理奈米碳管之結果分析 45
4.2 網印電極經電漿處理後之水接觸角 46
4.3 全氟磺酸基聚合物-奈米碳管/網版印刷複合電極之分析 47
4.3.1 不同修飾體積之影響分析 47
4.3.1.1 冷場發射掃描式電子顯微鏡 48
4.3.1.2 循環伏安圖分析 49
4.3.2 不同濃度之奈米碳管分散於全氟磺酸基聚合物之影響 52
4.3.2.1 循環伏安圖分析 52
4.3.3 不同電漿處理時間對複合電極之影響 54
4.3.3.1 冷場發射掃描式電子顯微鏡 54
4.3.3.2 影像式接觸角量測儀 56
4.3.3.3 原子力顯微鏡 57
4.3.3.4 能量色散X射線光譜 59
4.3.3.5 X射線光電子能譜儀 62
4.3.3.6 拉曼能譜儀 66
4.3.3.7 電阻變化 67


4.4 葡萄糖氧化酶/全氟磺酸基聚合物-奈米碳管/網印電極之電化學特性 68
4.4.1 不同濃度之葡萄糖氧化酶於全氟磺酸基聚合物-奈米碳管複合電極 68
4.5 複合電極之物理與化學特性 69
4.5.1 循環伏安圖分析 70
4.5.2 電化學阻抗頻譜分析 71
4.5.3 原子力顯微鏡與冷場發射顯微鏡 73
4.5.4 葡萄糖氧化酶之氧化還原峰於磷酸鹽緩衝溶液 74
4.5.5 掃速探討 76
4.6 葡萄糖氧化酶/全氟磺酸基聚合物-奈米碳管/網印電極之電極感測效能 78
4.6.1 全氟磺酸基聚合物含不同濃度的奈米碳管之葡萄糖感測 79
4.6.2 不同電漿處理時間電極之葡萄糖感測 86
4.6.3 干擾物分析 94
4.6.4 人工唾液分析 96
第五章 結論 99
參考文獻 100

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