本論文主要在開發新穎奈米材料包括半導體量子點及金奈米粒子等兩種奈米材料，應用於製造白色發光元件與分析生物及環境樣品中硫醇分子。簡單區分為兩個部分，第一部份為合金量子點的合成、光學特性探討、白光的生成以及發光元件的應用，第二部分為開發具功能化金奈米材料並結合奈米濃縮技術與毛細管電泳聚合物線上濃縮技術，建立具選擇性與極高靈敏度檢測硫醇分子的分析方法。
首先，我們藉由簡單且單一步驟的水相合成反應，比例調配過氯酸鎘與過氯酸鋅濃度，再加入反應試劑NaHSe，並利用3-mercaptopropionic acid當穩定試劑包覆在奈米粒子表面，在相對低溫的條件下，經過控制的反應時間，即可合成出ZnxCd1–xSe合金量子點奈米材料。實驗發現，這類合金量子點奈米材料之光學性質與成分組成，和其反應溶液中鋅離子對鎘離子的莫耳比率有高度相關性。伴隨著合金奈米粒子組成中鋅成分的增長，吸收峰與放射峰會產生有系統地藍位移現象，此外，粉末X光繞射峰亦有系統地向較大繞射角度位移（偏向ZnSe的特性波峯），這些結果顯示了合金量子點的形成。而在不同的鋅與鎘成分比率之合金量子點奈米粒子中，我們找到可激放白光的Zn0.93Cd0.07Se合金量子點奈米粒子，其光子產率為12%，並發現調控反應時間可以平衡放射光譜中band edge emission與trap state emission之放射光相對強度，進而獲得白光。最後，我們將此白光量子點奈米材料結合polydimethylsiloxane (PDMS)，以365-nm UV lamp為激發源，製作出發白光的簡易固態發光元件。
另一部分，我們利用非離子型介面活性劑Tween 20修飾在金奈米粒子表面上，開發具功能化的Tween 20-AuNPs材料，使金奈米粒子能夠穩定分散在高鹽類溶液中，並可透過金硫鍵結選擇性地萃取濃縮硫醇分子，再藉由毛細管電泳搭配雷射誘導螢光偵測法(CE-LIF)來進行分離與定量分析。我們先應用在檢測生物樣品中胺基酸硫醇分子，將吸附在金奈米粒子表面的胺基酸硫醇分子離心濃縮後以2-thioglycolic acid取代出來，並加入衍生試劑OPA進行衍生，再引入CE-LIF分析。研究結果顯示，運用金奈米粒子萃取濃縮Hcys、GSH及GluCys等胺基酸硫醇分子可分別提升11、282與21倍的偵測靈敏度，且偵測極限分別可達4013 pM、80 pM及383 pM濃度範圍，並實際應用在人體尿液中的檢測。再者，我們應用在檢測環境樣品中含硫醇胜肽分子，實驗中使用1,4-dithiolthreitol作為取代試劑，萃取後胜肽分子再以OPA進行衍生，並使用poly(ethylene oxide)聚合物作為電泳分離及線上濃縮之添加劑，同時增加樣品注入量，藉由線上濃縮提升偵測靈敏度。分析結果GSH、GluCys及植物螯合素PC2~ PC4等5種含硫醇胜肽分子之偵測極限可達0.1-6 pM 範圍。此分析方法相較於文獻中已發表的方法，具有最低的偵測極限，且實際應用在海水樣品分析。我們所開發的方法結合了奈米材料技術與毛細管電泳技術，具有超靈敏檢測生物及環境樣品中硫醇分子之能力。

This thesis focuses on development of novel nanomaterials, including semiconductor quantum dots (QDs) and gold nanoparticles (AuNPs), for fabricating white-light emitting devices and assaying thiols in biological and environmental samples. The thesis mainly contains two divisions. One demonstrates synthesis, optical properties and white-light emissions of alloyed quantum dots and their application to light-emitting devices. The other describes to combine functionalized gold nanoparticles with capillary electrophoresis and accomplish high selectivity and ultrasensitive detection for thiols.
First, through one-step aqueous synthesis, alloyed ZnxCd1–xSe QDs have been successfully prepared at low temperatures by reacting a mixture of Cd(ClO4)2 and Zn(ClO4)2 with NaHSe using 3-mercaptopropionic acid as a surface-stabilizing agent. The optical properties and composition of the alloyed QDs were highly dependent on the molar ratio of Zn2+ to Cd2+. With the increase in Zn content, a systematic blue shift occurred in the first exciton absorption and band edge emission. Moreover, X-ray diffraction peaks of the alloyed QDs systematically shifted to larger angles simultaneously. These systematic shifts indicated the formation of the alloyed QDs. Interestingly, among these alloyed QDs, Zn0.93Cd0.07Se QDs exhibited white-light emission with quantum yields of 12%. In addition, we discovered that we could adjust the relative strength of the band edge and trap state emissions by controlling the reaction time, thereby attain white-light-emitting QDs. Finally, we blended alloyed QDs with ultraviolet-transparent polydimethylsiloxane (PDMS) to develop a white-light, solid-state lighting device by using a 365-nm UV lamp as the pump source.
In the other part of this thesis, we proposed a method for selective enrichment of thiols using Tween 20-capped gold nanoparticles (AuNPs) prior to capillary electrophoresis coupled with laser-induced fluorescence (CE-LIF). By forming Au-S bonds, Tween 20-AuNPs can selectively extract thiols from a complicated matrix. A Tween 20 capping layer not only suppresses nonspecific adsorption, but also enables NPs to disperse in a highly-salinity solution. For analyses of aminothiols, after extraction and centrifugation, thioglycollic acid was utilized to remove aminothiols that attached to the NP surfaces. The extracted aminothiols was derivatized with o-phthalaldehyde (OPA) followed by CE-LIF. The use of this nanoprobe provided approximately 11-, 282-, and 21-fold sensitivity improvements for homocysteine (HCys), glutathione (GSH), and γ-glutamylcysteine (GluCys), respectively. Furthermore, the limits of detection (LODs) at a signal-to-noise ratio of 3 for HCys, GSH, and GluCys are 4013, 80, and 383 pM, respectively. A practical analysis of aminothiols in human urine sample has been accomplished by our proposed method. For another application to determining thiol-containing peptides, we use dithiothreitol to remove thiol-containing peptides from the NP surface through ligand exchange. The released peptides are selectively derivatized with OPA to form tricyclic isoindole derivatives. After injecting a large sample volume, the sensitivity of these peptides was improved by stacking them via using polyethylene oxide (PEO) as additive for on-line concentration and separation. As a result, LODs for GSH, GluCys, and phytochelatins (PC2 ~ PC4) were down to 0.1-6 pM. The proposed method has the lowest LODs for five peptides compared to other reported methods, and it also detect dissolve thiols in seawater in practice. Our proposed method is capable of ultrasensitive detection for thiols in biological and environmental samples.

中文摘要 i
英文摘要 iii
目錄 v
圖次 ix
表次 xii
第一章 緒論 1
1.1奈米材料簡介 1
1.1.1 奈米介觀 1
1.1.2 奈米材料的物理效應與特性 2
1.1.3 奈米粒子的製備與表面修飾 5
1.2 半導體量子點 8
1.2.1 量子點定義與特性 8
1.2.2 化學合成與量子點結構 9
1.2.3 量子點的修飾與應用 15
1.3 金奈米粒子 18
1.3.1 光學特性 18
1.3.2 合成製備方法 20
1.3.3 感測方法與應用 20
1.4 毛細管電泳 26
1.4.1 分離模式 27
1.4.2 偵測方法 32
1.4.3 毛細管線上濃縮技術 35
1.5 研究動機 40
1.6參考文獻 42
第二章 單一步驟水相低溫合成可激放白光之合金量子點 61
2.1 摘要 61
2.2 前言 62
2.3 實驗 64
2.3.1 實驗藥品與材料 64
2.3.2 NaHSe溶液之製備 65
2.3.3 ZnxCd1–xSe合金量子點之合成 66
2.3.4 CdSe與ZnSe量子點之合成 66
2.3.5 量子點定性與儀器設備 67
2.3.6 簡易固態發光元件的製作 70
2.4 結果與討論 72
2.4.1 改變Zn2+�Cd2+莫耳比的影響 72
2.4.2 白光量子點的定性 82
2.4.3 成長機制 85
2.4.4 發光元件的應用 92
2.5結論 94
2.6參考文獻 95
第三章 利用非離子型界面活性劑修飾之金奈米粒子萃取濃縮並結合毛細管
電泳雷射誘導螢光偵測法分析生物樣品中胺基酸硫醇分子 101
3.1 摘要 101
3.2 前言 102
3.3 實驗 105
3.3.1 藥品與溶液製備 105
3.3.2 實驗儀器 108
3.3.3 金奈米粒子的合成與定性 110
3.3.4 萃取及衍生流程 111
3.3.5 毛細管處理與電泳分離 111
3.3.6 尿液中胺基酸硫醇分子與肌酸酐的分析 112
3.4 結果與討論 113
3.4.1 胺基酸硫醇分子衍生與電泳分離的最佳化 113
3.4.2 取代試劑的選用 117
3.4.3 金奈米粒子濃度與取代試劑濃度的變化 119
3.4.4 樣品體積的影響 121
3.4.5 定量與真實樣品之應用 125
3.5結論 131
3.6參考文獻 132
第四章 利用金奈米粒子萃取濃縮並結合毛細管電泳雷射誘導螢光偵測方式
分析海水中的含硫醇胜肽分子 137
4.1 摘要 137
4.2 前言 138
4.3 實驗 142
4.3.1 藥品與溶液製備 142
4.3.2 實驗儀器 145
4.3.3 金奈米粒子的合成與修飾 147
4.3.4 奈米粒子的萃取流程 148
4.3.5 衍生方法 148
4.3.6 毛細管電泳分離與線上濃縮 148
4.3.7 海水中硫醇分子的分析 149
4.4 結果與討論 151
4.4.1 植物螯合素的衍生 151
4.4.2 PEO扮演的角色 155
4.4.3 偵測靈敏度的改善 158
4.4.4 再現性與定量及真實樣品之應用 167
4.5結論 171
4.6參考文獻 172
第五章 總結 179
附錄 181

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