單層硫醇修飾的奈米金應用於辨識金屬離子之研究：探討奈米金之分散與聚集的實驗設計

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研究生：	吳松勳 Sung-Hsun Wu
論文名稱：	單層硫醇修飾的奈米金應用於辨識金屬離子之研究：探討奈米金之分散與聚集的實驗設計 Development of the Dispersion-Aggregation Transitions of Monolayer-Functionalized Gold Nanoparticles for Metal-Ion Sensing
指導教授：	陳俊顯 Chun-hsien Chen 何佳安 Ja-an Annie Ho
口試委員:
學位類別：	博士 Doctor
系所名稱：	理學院 - 化學系 Department of Chemistry
論文出版年：	2008
畢業學年度：	96
語文別：	中文
論文頁數：	100
中文關鍵詞：	金奈米粒子、金屬離子、感測器、皇冠醚、半胱胺酸、鉀、鉛、銅
外文關鍵詞：	gold nanoparticles, metal ion, sensor, crown ether, cysteine, K, Pb, Cu
相關次數：	點閱：2 下載：0
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本論文主要針對以金奈米粒子所設計的金屬離子感測器，提出改善偵測效能的方法，並且設計新的辨識機制和觀測現象，以擴展金奈米粒子感測器的應用性，內容包括：(1)對於以顆粒聚集變分散作為辨識過程的金奈米粒子感測器，提出降低顆粒間的排斥力的方法改善其偵測極限：以15c5-C4-/TA-GNPs偵測鉀離子為例，藉由調整溶液的pH值和離子強度可降低靜電斥力，獲得最佳化的偵測效能；(2)設計以聚集變分散作為辨識過程的金奈米粒子感測器偵測金屬離子：主要的概念是以顆粒間製造氫鍵形成聚集，再以辨識作用力使氫鍵斷裂或顆粒間斥力的增加使聚集的顆粒變成分散，達到辨識的效果。利用此概念，我們設計以15c5-C4-/TA-GNPs在甲醇中所形成的聚集偵測鉛離子，藉由TA的羧酸根在甲醇中形成顆粒間氫鍵製造顆粒聚集，再利用羧酸根和鄰近的15-crown-5共同對鉛離子的辨識錯合作用，在辨識鉛離子的過程中，導致顆粒間的氫鍵斷裂，並造成靜電斥力的增加，使顆粒形成分散；(3)發展以目視觀察相變化的方法偵測金屬離子的濃度範圍：利用銅離子和cysteine反應產生如棉絮狀物的不均相，設計出以觀察不均相的出現與否判斷銅離子濃度範圍的方法，過程中利用金奈米粒子吸附於棉絮狀物凸顯相變化，使之容易觀察。我們對銅離子和cysteine反應產生棉絮狀物的現象加以推論和驗證，並探討影響偵測範圍的因素，進而控制實驗條件降低可偵測範圍。

Development of gold nanoparticles (GNPs) for metal-ion sensing is an active research because of their high extinction coefficients and distance-dependent optical absorbance. The aims of this study are to improve the the analytical performance and to design new sensing strategies for GNP-based sensors. To improve the sensitivity of the GNP sensors with the dispersive-to-aggregated transformation, the minimization of electrostatic repulsion is suggested as well as the increase of the sensing moieties on the GNPs. For the model system, the recognition of K+ by 15c5-C4-/TA-GNPs, the adjustments of pH and ionic strength were carried out to reduce electrostatic repulsion and the optimizd sensing performance was achieved. Different from the dispersion-to-aggregation transformation, a novel sensing strategy that the aggregated GNPs recognize analytes followed by forming dispersion is also reported. The interparticle hydrogen bonds are introduced to trigger GNP aggregation. The recognition events break the hydrogen bonds and make the GNPs dispersive. The proof-of-concept study is the recognition of Pb2+ by using 15c5-C4-/TA-GNPs in the methanol solution. A visual sensing phenomenon with phase segregation is provided for the circumstances without instrumental assistance. An example demonstrated here is the detection of Cu2+ via the cysteine-copper chemistry. The fluffy flocculates resulting from the reaction of Cu2+ with cysteine are applied to recognize Cu2+ concentration range.

第一章、緒論    1
1-1金屬離子感測器的簡介    1
1-2金奈米粒子的簡介    3
1-3金奈米粒子感測器    5
1-4金奈米粒子在金屬離子偵測上的應用    6
第二章、實驗部分    10
2-1藥品與器材    10
2-1-1化學藥品    10
2-1-2實驗器材    12
2-2實驗儀器與設備    13
2-3金奈米粒子的製備    14
2-3-1 citrate-GNPs的合成    14
2-3-2金奈米粒子的表面修飾    15
2-3-2-1 15-croown-5 ether修飾的金奈米粒子的製備    15
2-3-2-2 cysteine修飾的金奈米粒子之製備    16
2-4儀器的量測    17
2-4-1金膜的製作    17
2-4-2 XPS的量測    17
2-4-3 TEM的量測    18
2-4-4 zeta電位的量測    18
2-4-5 UV/Vis的量測    18
2-4-6 IR的量測    19
第三章、降低顆粒間的排斥力改善GNPS的偵測靈敏度    20
3-1前言    20
3-1-1顆粒之間的作用力與偵測靈敏度的關係    20
3-1-2改善金奈米粒子偵測能力的方法    21
3-1-3鉀離子在生理上的重要性    23
3-1-4研究目的    24
3-2實驗部分    25
3-2-1金奈米粒子的修飾    25
3-2-2溶液的配製    25
3-2-3偵測流程    25
3-2-4儀器的量測    26
3-3結果與討論    27
3-3-1 15c5-C4-/TA-GNPs表面組成的定性分析    27
3-3-2溶液pH值對偵測極限的影響    30
3-3-3溶液離子強度對金奈米粒子偵測極限的影響    34
3-3-4 金奈米粒子表面組成對偵測極限的影響    37
3-3-5 金奈米粒子對真實樣品的分析    40
3-4結論    43
第四章、以金奈米粒子聚集偵測金屬離子的實驗設計    44
4-1前言    44
4-1-1以分散變聚集的金奈米粒子感測器    44
4-1-2以金奈米粒子從聚集變分散進行偵測的感測器設計    45
4-1-3鉛的危害與偵測鉛的重要性    47
4-1-4偵測鉛離子的方法    49
4-1-5研究目的    50
4-2實驗部分    51
4-2-1溶液配製    51
4-2-3儀器的量測    51
4-3結果與討論    52
4-3-1以15c5-C4-/TA-GNPs(MeOH)偵測鉛離子    52
4-3-2 15c5-C4-/TA-GNPs(MeOH)偵測鉛離子的機制    54
4-3-3溶液組成對15c5-C4-/TA-GNPs(MeOH)的影響    59
4-3-4 15c5-C4-/TA-GNPs(MeOH)對鉛離子的偵測靈敏度    63
4-3-5 15c5-C4-/TA-GNPs(MeOH)偵測鉛離子的選擇性    65
4-4 結論    66
第五章、以目視的方法測定金屬離子的濃度範圍    68
5-1前言    68
5-1-1金奈米粒子感測器的形式    68
5-1-2測量銅離子的重要性    69
5-1-3測量銅離子的方法    70
5-1-4研究目的    72
5-2實驗部分    72
5-2-1 Cys-GNPs的製備    72
5-2-2溶液的配製    72
5-2-3以相變化偵測銅離子    73
5-2-4儀器的量測    73
5-3結果與討論    73
5-3-1利用cysteine和銅離子產生相變化辨識銅離子    73
5-3-2 cysteine和銅離子反應產生相變化的機制    76
5-3-3 Cys-GNPs扮演的角色    84
5-3-4降低相變化可偵測的銅離子濃度範圍    85
5-4結論    89
第六章、總結    90
第七章、參考文獻    92

                                

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