TWI639426B - 一種含有配位子鍵結的金奈米團簇的溶液之製備方法 - Google Patents
一種含有配位子鍵結的金奈米團簇的溶液之製備方法 Download PDFInfo
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- 239000010931 gold Substances 0.000 title claims abstract description 80
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 78
- 239000003446 ligand Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 26
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 12
- 239000012045 crude solution Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000000746 purification Methods 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- 238000006722 reduction reaction Methods 0.000 claims abstract description 6
- 239000002585 base Substances 0.000 claims abstract description 5
- 230000009471 action Effects 0.000 claims abstract description 4
- 238000000502 dialysis Methods 0.000 claims abstract description 4
- 239000012528 membrane Substances 0.000 claims abstract description 3
- AGBQKNBQESQNJD-UHFFFAOYSA-M lipoate Chemical compound [O-]C(=O)CCCCC1CCSS1 AGBQKNBQESQNJD-UHFFFAOYSA-M 0.000 claims description 30
- 235000019136 lipoic acid Nutrition 0.000 claims description 30
- 229960002663 thioctic acid Drugs 0.000 claims description 30
- 238000002360 preparation method Methods 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 238000002441 X-ray diffraction Methods 0.000 claims description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- 239000002537 cosmetic Substances 0.000 claims description 4
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 4
- 238000002329 infrared spectrum Methods 0.000 claims description 4
- IZFHEQBZOYJLPK-SSDOTTSWSA-N (R)-dihydrolipoic acid Chemical compound OC(=O)CCCC[C@@H](S)CCS IZFHEQBZOYJLPK-SSDOTTSWSA-N 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- LLNAMUJRIZIXHF-CLFYSBASSA-N (z)-2-methyl-3-phenylprop-2-en-1-ol Chemical compound OCC(/C)=C\C1=CC=CC=C1 LLNAMUJRIZIXHF-CLFYSBASSA-N 0.000 claims description 2
- 108010024636 Glutathione Proteins 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- VHJLVAABSRFDPM-QWWZWVQMSA-N dithiothreitol Chemical compound SC[C@@H](O)[C@H](O)CS VHJLVAABSRFDPM-QWWZWVQMSA-N 0.000 claims description 2
- 235000013305 food Nutrition 0.000 claims description 2
- 229960003180 glutathione Drugs 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 239000008194 pharmaceutical composition Substances 0.000 claims description 2
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 claims description 2
- 239000001472 potassium tartrate Substances 0.000 claims description 2
- 229940111695 potassium tartrate Drugs 0.000 claims description 2
- 235000011005 potassium tartrates Nutrition 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- SBZQSKGVWLMJEH-UHFFFAOYSA-N C(=O)(O)CCP(CCC(=O)O)CCC(=O)O.C(=O)(O)CCP(CCC(=O)O)CCC(=O)O Chemical compound C(=O)(O)CCP(CCC(=O)O)CCC(=O)O.C(=O)(O)CCP(CCC(=O)O)CCC(=O)O SBZQSKGVWLMJEH-UHFFFAOYSA-N 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- 230000008569 process Effects 0.000 description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000002096 quantum dot Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 238000002296 dynamic light scattering Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002343 gold Chemical class 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- PZBFGYYEXUXCOF-UHFFFAOYSA-N TCEP Chemical compound OC(=O)CCP(CCC(O)=O)CCC(O)=O PZBFGYYEXUXCOF-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000000412 dendrimer Substances 0.000 description 1
- 229920000736 dendritic polymer Polymers 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- ZFGJFDFUALJZFF-UHFFFAOYSA-K gold(3+);trichloride;trihydrate Chemical compound O.O.O.Cl[Au](Cl)Cl ZFGJFDFUALJZFF-UHFFFAOYSA-K 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001420 photoelectron spectroscopy Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
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- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- A61K47/24—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing atoms other than carbon, hydrogen, oxygen, halogen, nitrogen or sulfur, e.g. cyclomethicone or phospholipids
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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Abstract
本發明提供一種含有配位子鍵結的金奈米團簇的溶液之製備方法，該方法包含以下步驟：提供一含有金的前驅物、鹼和配位子的水溶液；進行一還原反應使上述之水溶液在一還原劑作用下形成一含有配位子鍵結的金奈米團簇的液體；濃縮該液體至一固體；溶解該固體至水中形成一粗溶液；和進行一純化程序，使該粗溶液通過一薄膜或一透析管而得到該含有配位子鍵結的金奈米團簇的溶液。
Description
本發明係關於一種含有配位子鍵結的金奈米團簇的溶液之製備方法。特別是該配位子包含硫辛酸和二氫硫辛酸。
傳統的有機染料分子的性質在高解析的生物影像應用上受到了限制，但是量子點相較於傳統的有機染料分子具有螢光亮度強、光穩定性佳、以及用單一波長的雷射便可以激發出多種不同波長的發射波之特性。發射波是一狹窄且對稱的波形，且可重複激發，因此螢光時效可以持久。這些特性吸引科學家的重視，奈米量子點的應用也越來越多樣性，深具取代傳統染劑的潛力，因此，在生醫工程應用方面，更有令人期待的發展性。
近年來量子點以其優異的光學特性，已成功地克服過去生物及醫學光學探針所面臨之瓶頸，成為新一代螢光探針設計之重要奈米材料。從細胞立體影像、活細胞監控、單分子胞內追蹤、長效型光學感測器研製、癌症診斷與治療皆有突破性進展，
加上量子點快速產業化及其上億商機，已成奈米生物技術極為成功應用之典範。然而傳統市售以鎘或鉛等有毒重金屬材料為主之水溶性量子點，其延伸對環境及人體健康可能帶來的衝擊逐漸受到重視，是目前全面開拓其生醫應用所面臨之窘境。
金係為研究較早之一種奈米材料，在生物學研究中被稱為膠體金，粒子尺寸在1-100nm之間。金量子點具有很高的電子密度，在電子顯微鏡下有很好的襯度，並且具有相當高之生物相容性，其已被證實經由改變其原子團簇之大小即可發出不同顏色之螢光，能夠應用在多元之生醫標定或光學元件的製作上，但由於製程相當不易，合成時需要利用昂貴的樹狀聚合物(dendrimer)作為金量子點之包覆材料，耗時且不易大量生產，故限制其廣大生醫應用之開發。因此，開發出簡易並可大量生產製造之金量子點形成技術係產業界亟欲發展之重點。
鑒於上述發明背景中，為了符合產業上之要求，本發明提供一種含有配位子鍵結的金奈米團簇的溶液之製備方法。
鑒於上述之發明背景，為了符合產業上之要求，本發明之目的在於提供一種含有配位子鍵結的金奈米團簇的溶液之製備方法。
本發明之一目的在於提供一種含有配位子鍵結的金奈米團簇的溶液之製備方法，該方法包含以下步驟：提供一含有
金的前驅物、鹼和配位子的水溶液；進行一還原反應使上述之水溶液在一還原劑作用下形成一含有配位子鍵結的金奈米團簇的液體；在30-60℃濃縮該液體至一固體；溶解該固體至水中形成一粗溶液；和進行一純化程序，使該粗溶液通過一薄膜或一透析管而得到該含有配位子鍵結的金奈米團簇的溶液。
綜上所述，本發明所揭露之製備方法是一步法(one-batch process)。本發明之一關鍵技術特徵是本發明所提供的製備方法是在水相中製備合成含有配位子鍵結的金奈米團簇的水溶液。再者，由於製備過程中是使用水作為溶劑，因此本發明所述之製程是一綠色環保製程，根據本發明所製備得到的含有配位子鍵結的金奈米團簇的水溶液不會含有有害性物質或溶劑，如甲苯和二甲基甲醯胺，因此，根據本發明之方法所製備得到的含有配位子鍵結的金奈米團簇的水溶液特別適合應用在化妝品和生醫產業。
有關本發明之前述及其他技術內容、特點與功效，在以下配合參考圖式之一較佳實施例的詳細說明中，將可清楚的呈現。為了能徹底地瞭解本發明，將在下列的描述中提出詳盡的步驟及其組成。顯然地，本發明的施行並未限定於該領域之技藝者所熟習的特殊細節。另一方面，眾所周知的組成或步驟並未描述於細節中，以避免造成本發明不必要之限制。本發明的較佳實
施例會詳細描述如下，然而除了這些詳細描述之外，本發明還可以廣泛地施行在其他的實施例中，且本發明的範圍不受限定，其以之後的專利範圍為準。
根據本發明的一代表實施例，本發明提供一種含有配位子鍵結的金奈米團簇的溶液之製備方法，該方法包含以下步驟：提供一含有金的前驅物、鹼和配位子的水溶液；進行一還原反應使上述之水溶液在一還原劑作用下形成一含有配位子鍵結的金奈米團簇的液體；在30-60℃濃縮該液體至一固體；溶解該固體至水中形成一粗溶液；和進行一純化程序，使該粗溶液通過一薄膜或一透析管而得到該含有配位子鍵結的金奈米團簇的溶液。
於一較佳具體範例，其中上述之含有配位子鍵結的金奈米團簇的溶液之製備方法還包含一加熱程序和/或一UV處理程序以增加該含有配位子鍵結的金奈米團簇的溶液的螢光強度。
於一具體範例，該加熱程序是在30-150℃之間執行。
於一具體範例，該UV處理程序是在波長300-400nm之間執行。
於一較佳具體範例，該金的前驅物包含三價金Au(III)離子。
於一較佳具體範例，其中上述之金的前驅物對於配位子的莫耳比例是小於10，且該配位子包含硫辛酸(lipoic acid)和二氫硫辛酸(dihydrolipoic acid)。
於一具體範例，該鹼包含氫氧化鈉和氫氧化鉀。
於一具體範例，該還原劑包含硼氫化鈉、檸檬酸鈉、酒石酸鉀、二硫蘇糖醇(Dithiothreitol)、三(2-羧乙基)膦(Tris(2-carboxyethyl)phosphine)、四丁基硝酸銨、抗壞血酸和穀胱甘肽。
於一具體範例，該還原反應是在5-40℃之間執行。
於一具體範例，該純化程序是維持該含有配位子鍵結的金奈米團簇的分子量在10-100kDa之間。
於一較佳具體範例，該含有配位子鍵結的金奈米團簇的傅立葉紅外光譜包含以下波峰：3261,2920,2852,1560和1401cm-1。
於一較佳具體範例，該含有配位子鍵結的金奈米團簇的X-ray繞射圖譜包含以下波峰：8.5°(111),44.6°(200),64.8°(220),and 77.8°(311)2-theta degree。
於一較佳具體範例，該含有配位子鍵結的金奈米團簇的水力平均直徑是1-4nm。
於一較佳具體範例，該含有配位子鍵結的金奈米團簇的金對於該配位子的重量比例是0.5-10。
於一具體範例，該含有配位子鍵結的金奈米團簇是一組成物的一部份，該組成物包含化妝品組成物、食品組成物和醫藥組成物。
根據上述，本發明所揭露之含有配位子鍵結的金奈
米團簇的溶液之製備方法是一步法(one-batch process)。本發明之一關鍵技術特徵是本發明所提供的製備方法是在水相中製備合成含有配位子鍵結的金奈米團簇的水溶液。再者，由於製備過程中是使用水作為溶劑，因此本發明所述之製程是一綠色環保製程，根據本發明所製備得到的含有配位子鍵結的金奈米團簇的水溶液不會含有任何有害性物質或溶劑，如甲苯和二甲基甲醯胺，因此，根據本發明之方法所製備得到的含有配位子鍵結的金奈米團簇的水溶液特別適合應用在化妝品和生醫產業。
以下以具體實驗例說明本發明之內容和技術特徵，但並不因此限定本發明之範圍。
實驗例：製備合成含有硫辛酸配位子鍵結的金奈米團簇的水溶液
30μmol的硫辛酸溶於含有氫氧化鈉的去離子水中，加入10μmol的gold(III)chloride trihydrate。.室溫下持續攪拌並且加入硼氫化納(Sodium borohydride)再攪拌反應15分鐘後，直接在55℃濃縮上述之反應混合物至固體，然後再加入去離子水溶解該固體形成一粗溶液(crude solution)，最後以10kDa的薄膜進行純化程序得到本發明所述之含有硫辛酸配位子鍵結的金奈米團簇的水溶液。
上述實驗例所製備得到的含有硫辛酸配位子鍵結的金奈米團簇的水溶液以下述儀器進行各項分析鑑定：穿透式電子顯微鏡(Transmission electron microscopy(TEM))、動態光散射儀(dynamic
light scattering(DLS))、光電子掃描儀(X-ray photoelectron spectroscopy(XPS))、熱失重分析儀(thermogravimetric analysis(TGA))、傅立葉紅外光譜儀(Fourier transform infrared spectrometer(FTIR))和X光熱射儀(X-ray diffraction(XRD))。
本發明實驗例所述之含有硫辛酸配位子鍵結的金奈米團簇的水溶液的特性分析和鑑定如表一所示。
如第1圖和第2圖所示，TEM分析顯示本發明的含有硫辛酸配位子鍵結的金奈米團簇的尺寸小於10nm，且該硫辛酸配位子鍵結的金奈米團簇是均勻分散在水溶液之中；根據第3圖所示，本發明的含有硫辛酸配位子鍵結的金奈米團簇的平均核心直徑(average core diameter)是1.45±0.34nm。
如第4圖所示，DLS分析顯示根據本發明之方法所製備的3批次的硫辛酸配位子鍵結的金奈米團簇的數量尺寸分布分別是1.82nm(標準差是0.56nm)、2.28nm(標準差是0.60nm)和2.71nm(標準差是0.89nm)。
如第5圖所示，DLS分析顯示根據本發明之方法所製備的3批次的硫辛酸配位子鍵結的金奈米團簇的體積尺寸分布分別是2.56nm(標準差是1.44nm)、2.80nm(標準差是0.96nm)和4.00nm(標準差是2.16nm)。
如第6圖所示，X光電子圖譜顯示C,O,S,Na,N和Au的原子百分比分別是73.9%,17.0%,4.4%,2.7%,1.3%和0.6%。
如第7圖所示，熱重量分析顯示金和配位子的重量百分比分別是67.39%和32.61%。
如第8圖所示，傅立葉紅外光譜顯示以下位置之波峰：3261,2920,2852,1560和1401cm-1。
如第9圖所示，X光繞射圖譜顯示4個特徵波峰位置如下：38.5°(111),44.6°(200),64.8°(220)，和77.8°(311)。
製程參數和含有硫辛酸配位子鍵結的金奈米團簇的液體的螢光強度之關係
如第10圖所示，WG代表省略濃縮步驟的本發明之製程，IWG-55C、IWG-80C和IWG-90C分別代表同時執行濃縮步驟和加熱步驟(55℃、80℃和90℃)之製程，根據第10圖，同時
以濃縮步驟和加熱步驟(55℃、80℃和90℃)之製程所製備得到的含有硫辛酸配位子鍵結的金奈米團簇的液體的螢光強度(波長700nm)顯著的增加。
如第11圖所示，WG代表省略濃縮步驟的本發明之製程，IWG-UV代表執行濃縮步驟和以UV光(波長365nm)處理之製程，根據第11圖，同時以濃縮步驟和UV光(波長365nm)處理之製程所製備得到的有硫辛酸配位子鍵結的金奈米團簇的液體的螢光強度(波長700nm)大幅度的增加。
如第12圖所示，WG代表省略濃縮步驟的本發明之製程，IWG-50X、IWG-100X、IWG-200X、IWG-250X和IWG-300X分別代表執行濃縮步驟至含有硫辛酸配位子鍵結的金奈米團簇的濃度為原始濃度的50倍、100倍、200倍、250倍和300倍。根據第12圖，當含有硫辛酸配位子鍵結的金奈米團簇的濃度增加時，螢光強度亦增加，為了達到含有硫辛酸配位子鍵結的金奈米團簇具有最大的螢光強度的目的，本發明之方法中的濃縮步驟的關鍵是濃縮含有硫辛酸配位子鍵結的金奈米團簇的液體至固體狀態，然後再回溶該固體至水中進行純化程序後得到本發明所述的含有硫辛酸配位子鍵結的金奈米團簇的溶液。
以上雖以特定範例說明本發明，但並不因此限定本發明之範圍，熟悉本技藝者瞭解在不脫離本發明的意圖及範圍下可進行各種變形或變更。此外，摘要部分和標題僅是用來輔助專利文件搜尋之用，並非用來限制本發明之權利範圍。
第1圖是本發明實驗例所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液之TEM影像圖；第2圖是本發明實驗例所述之含有硫辛酸配位子鍵結的金奈米團簇的單顆團簇之TEM影像圖；第3圖是本發明實驗例所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液之核心尺寸分布圖；該第3圖是根據第2圖的軟體計算結果所繪製；第4圖是本發明實驗所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液之動態光散射數目尺寸分布圖；第5圖是本發明實驗所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液之動態光散射體積尺寸分布圖；第6圖是本發明實驗例所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液之光電子圖譜；第7圖是本發明實驗例所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液之熱失重分析圖；第8圖是本發明實驗例所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液之傅立葉紅外光譜圖；第9圖是本發明實驗例所述之含有硫辛酸配位子鍵結的金奈米
團簇的溶液之X光繞射圖；第10圖是本發明所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液的螢光強度和熱處理溫度之關係圖；第11圖是本發明所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液的螢光強度和UV處理程序之關係圖；和第12圖是本發明所述之含有硫辛酸配位子鍵結的金奈米團簇的溶液的螢光強度和其濃度之關係圖。
Claims (12)
- 一種含有配位子鍵結的金奈米團簇的溶液之製備方法，該方法包含以下步驟：提供一含有金的前驅物，該金的前驅物包含三價金Au(III)離子、鹼，該鹼包含氫氧化鈉和氫氧化鉀，和配位子的水溶液，其中上述之金的前驅物對於該配位子的莫耳比例是小於10，且該配位子包含硫辛酸(lipoic acid)和二氫硫辛酸(dihydrolipoic acid)；進行一還原反應使上述之水溶液在一還原劑作用下形成一含有配位子鍵結的金奈米團簇的液體；在30-60℃濃縮該液體至一固體；溶解該固體至水中形成一粗溶液；和進行一純化程序，使該粗溶液通過一薄膜或一透析管而得到該含有配位子鍵結的金奈米團簇的溶液。
- 如申請專利範圍1所述之製備方法還包含一加熱程序和/或一UV處理程序以增加該含有配位子鍵結的金奈米團簇的溶液的螢光強度。
- 如申請專利範圍2所述之製備方法，該加熱程序是在30-150℃之間執行。
- 如申請專利範圍2所述之製備方法，該UV處理程序是在波長300-400nm之間執行。
- 如申請專利範圍1所述之製備方法，該還原劑包含硼氫化鈉、檸檬酸鈉、酒石酸鉀、二硫蘇糖醇(Dithiothreitol)、三(2-羧乙基)膦(Tris(2-carboxyethyl)phosphine)、四丁基硝酸銨、抗壞血酸和穀胱甘肽。
- 如申請專利範圍1所述之製備方法，該還原反應是在5-40℃之間執行。
- 如申請專利範圍1所述之製備方法，該純化程序是維持該含有配位子鍵結的金奈米團簇的分子量在10-100kDa之間。
- 如申請專利範圍1所述之製備方法，該含有配位子鍵結的金奈米團簇的傅立葉紅外光譜包含以下波峰：3261,2920,2852,1560和1401cm-1。
- 如申請專利範圍1所述之製備方法，該含有配位子鍵結的金奈米團簇的X-ray繞射圖譜包含以下波峰：8.5°(111),44.6°(200),64.8°(220),and 77.8°(311)2-theta degree。
- 如申請專利範圍1所述之製備方法，該含有配位子鍵結的金奈米團簇的水力平均直徑是1-4nm。
- 如申請專利範圍1所述之製備方法，該含有配位子鍵結的金奈米團簇的金對於該配位子的重量比例是0.5-10。
- 如申請專利範圍1所述之製備方法，該含有配位子鍵結的金奈米團簇是一組成物的一部份，該組成物包含化妝品組成物、食品組成物和醫藥組成物。
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| CN113061261A (zh) * | 2021-03-30 | 2021-07-02 | 深圳第三代半导体研究院 | 一种铜纳米簇荧光粉及其制备方法 |
| CN113333772B (zh) * | 2021-06-18 | 2023-01-03 | 南昌大学 | 金纳米簇的制备方法及其在2,4,6-三硝基苯酚检测的应用 |
| KR102636435B1 (ko) | 2021-09-14 | 2024-02-14 | 건국대학교 산학협력단 | 칼슘 나노클러스터의 제조방법, 및 이에 따라 제조된 칼슘 나노클러스터를 유효성분으로 포함하는 화장료용 형광 소재 |
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| CN102614535A (zh) * | 2011-02-01 | 2012-08-01 | 中原大学 | 医用对比剂及含有荧光金纳米团簇的微胞的制造方法 |
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| US4243604A (en) * | 1979-03-07 | 1981-01-06 | Borg-Warner Corporation | Aliphatic metal cluster compounds |
| US7404928B2 (en) * | 2002-07-29 | 2008-07-29 | The United States Of America As Represented By The Secretary Of The Navy | Thiol terminated monodisperse ethylene oxide oligomer capped gold nanoclusters |
| US20050147963A1 (en) * | 2003-12-29 | 2005-07-07 | Intel Corporation | Composite organic-inorganic nanoparticles and methods for use thereof |
| TWI361081B (en) * | 2008-08-29 | 2012-04-01 | Univ Chung Yuan Christian | Fluorescent gold nanocluster and method for forming the same |
| CN102127428B (zh) * | 2010-12-14 | 2013-06-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | 荧光银团簇、其制备方法及应用 |
| WO2012140675A1 (en) * | 2011-04-11 | 2012-10-18 | Council Of Scientific & Industrial Research | Stable oxide encapsulated metal clusters and nano particles |
| TWI413524B (zh) * | 2011-08-26 | 2013-11-01 | 財團法人台灣基督長老教會馬偕紀念社會事業基金會馬偕紀念醫院 | 以金奈米團簇來減緩氧化壓力和／或老化的方法、組合物及用途 |
| CN103007303A (zh) * | 2012-12-19 | 2013-04-03 | 深圳先进技术研究院 | 核-壳型三模态纳米造影剂、其制备方法及应用 |
| CN103599070B (zh) * | 2013-11-26 | 2015-05-20 | 上海交通大学 | 负载金纳米簇和抗癌药物的脂质体温度荧光探针的制备方法 |
| CN105860959B (zh) * | 2016-04-16 | 2018-05-18 | 福建医科大学 | 精氨酸/6-氮杂-2-硫代胸腺嘧啶-金纳米团簇及其制备方法 |
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| JP6810268B2 (ja) | 2021-01-06 |
| JP2019528381A (ja) | 2019-10-10 |
| WO2018036078A1 (zh) | 2018-03-01 |
| KR20190042668A (ko) | 2019-04-24 |
| TW201806591A (zh) | 2018-03-01 |
| US20180055083A1 (en) | 2018-03-01 |
| CN109689256A (zh) | 2019-04-26 |
| EP3508291A4 (en) | 2020-03-11 |
| EP3508291A1 (en) | 2019-07-10 |
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