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| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 劉春櫻 | |
| dc.contributor.author | Yu-Wen Yang | en |
| dc.contributor.author | 楊裕文 | zh_TW |
| dc.date.accessioned | 2021-06-13T04:14:32Z | - |
| dc.date.issued | 2006 | |
| dc.date.submitted | 2006-07-25 | |
| dc.identifier.citation | 1. Strain, H. H. J. Am. Chem. Soc. 1939, 61, 1292.
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/32739 | - |
| dc.description.abstract | 本研究以二氧化鈦溶膠凝膠作為開管式毛細管電層析之靜相。首先，在pH 1.5 且冰浴 (4℃) 的情況下來水解titanium isopropoxide，然後將溫度升溫至50℃，溫度維持7小時，以進行縮合反應，所得的產物為穩定且透明的膠體溶液。此膠體溶液，加入0.32 mg/ml空間穩定劑 (polyethylene glycol)，經減壓濃縮成較高濃度的膠體溶液。然後將其引入內徑為 50 μm 的毛細管中，在200℃ 下反應24小時，使毛細管管壁之矽純基與溶膠之鈦醇基進行縮合反應。經由電滲透流的測定，發覺在甲酸—Tris緩衝溶液中，管壁的等電點為pH 4.7，當pH 小於此值時，電滲透流為逆向；反之，則為正向。而在磷酸緩衝溶液下，因為磷酸分子會錯合在管壁上，所以電滲透流在pH 2.0以上恆為正向。將此二氧化鈦管柱應用於植物酚之分離，由研究發現其可用於 catechin 與 epicatechin 中性幾何異構物之分析，以分析電壓為15 kV，動相為磷酸緩衝溶液 (pH 9.0, 40 mM) 為最佳條件，平均理論板數為 3600 m-1；此管柱尚可用於分離植物酚類中的一些酸性分析物，如syringic acid、caffeic acid、salicylic acid 、p-coumaric acid 和 4-hydroxybenzoic acid。本研究選用甲酸/ Tris、EDTA 與磷酸緩衝溶液，改變 pH 值與緩衝溶液濃度等測試，發現動相會與分析物競爭管壁上之二氧化鈦而將分析物從靜相中交換出來，其分析之最佳條件為電壓 -20 kV，動相為EDTA 緩衝溶液 (pH 5.0, 40 mM)，流析順序為salicylic acid > 4-hydroxybenzoic acid > syringic acid > p-coumaric acid > caffeic acid，平均理論板數為 3.2 × 104 m-1，RSD < 4%。綜合以上，本研究所製備之二氧化鈦塗佈管柱，可成功分離植物酚的幾何異構物與植物酚酸。 | zh_TW |
| dc.description.abstract | In this study, titanium dioxide nanoparticles as a stationary phase in open-tubular capillary electrochromatography (CEC) was prepared. The process has been done in the following way. First, titanium isopropoxide was hydrolyzed at the pH 1.5 (4℃), then the mixture was condensed by heating at 50℃ for 7 h. A stable, clear solution was obtained. PEG 8000 (0.32 mg/ml) was then added to the TiO2 colloidal solution and concentrated under vacuum at 50℃.The high-concentration solution was introduced into the capillary column by nitrogen, then put in the oven and reacted at 200℃ for 24 h. The step made the condensation reaction of TiO2 nanoparticles with silanol groups of fused-silica capillary. EOF property was investigated in a variety of buffer solutions : /formate/Tris, phosphate and EDTA/. With formate/Tris buffer, EOF reversal at pH below 4.7 and cathodic EOF at pH above 4.7 were indicated. With phosphate and EDTA, only cathodic EOF were indicated. This is because of phosphate and EDTA buffer arosed titanium complex and yield a negative charge layer on the surface of TiO2. The CEC performance of the column was tested with plant phenols and phenolic acids. When mobile phase in phosphate (40 mM, pH 9.0), applied voltage of 15 kV, two plant phenols which are diastereomers, (+)-(2R,3S)-catechin and (−)-(2R,3R)-epicatechin, could be baseline separated. With the same column at the mobile phase of EDTA (40mM, pH 5.0), applied voltage of 20 kV, five phenolic acids, syringic acid, caffeic acid, salicylic acid, p-coumaric acid and 4-hydroxybenzoic acid could be baseline separated, the average theorical plate is 3.2 × 104 m-1 and RSD < 4% with four measurements. | en |
| dc.description.provenance | Made available in DSpace on 2021-06-13T04:14:32Z (GMT). No. of bitstreams: 1 ntu-95-R93223054-1.pdf: 2794770 bytes, checksum: 531d52f26bb63f825fa5f4fb8cbf159e (MD5) Previous issue date: 2006 | en |
| dc.description.tableofcontents | 摘要 A
英文摘要 B 目錄 C 圖目錄 G 表目錄 J 第一章 緒論 1 第一節 毛細管電層析簡介 1 1-1 前言 1 1-2 毛細管電層析原理 2 1-3 毛細管電層析管柱種類介紹 7 1-3.1 填充式管柱 7 1-3.2 整體式管柱 8 1-3.3 開管式管柱 8 第二節 二氧化鈦 15 2-1 二氧化鈦物理與化學性質 15 2-2 二氧化鈦應用 19 2-3 二氧化鈦奈米之製備 21 2-4 二氧化鈦為層析靜相之應用 24 第三節 分析物介紹 26 3-1 分析植物酚方法 28 第四節 研究動機 30 第二章 實驗部分 32 第一節 實驗儀器 32 第二節 實驗試藥 34 2-1 管柱製備 34 2-2 緩衝溶液 34 2-3 分析樣品 35 第三節 二氧化鈦奈米粒子合成與性質鑑定 36 3-1 二氧化鈦奈米粒子合成步驟 36 3-2 二氧化鈦奈米粒子性質鑑定 36 第四節 毛細管靜相製備與性質鑑定 37 4-1 毛細管前處理 37 4-2 二氧化鈦管柱之製備 37 4-3 二氧化鈦管柱之保存 37 第五節 毛細管電層析之實驗操作 38 5-1 藥品配製 38 5-2 毛細管電層析流程 38 5-3 電滲透流測試 39 第三章 結果與討論 41 第一節 二氧化鈦膠體粒子之製備與鑑定 41 1-1 二氧化鈦膠體粒子之製備 41 1-2 二氧化鈦膠體粒子之性質鑑定 41 1-3 改變前驅物濃度 42 1-4 穿透式電子顯微鏡鑑定 46 第二節 二氧化鈦塗佈管柱之製備 47 2-1 毛細管內部前處理 47 2-2 二氧化鈦膠體粒子濃縮 47 2-3 不同濃縮液濃度對塗佈的影響 48 2-4 管柱電滲流測定與動相組成之探討 53 2-4.1 甲酸及 Tris 緩衝溶液 54 2-4.2 磷酸與 EDTA 緩衝溶液 55 第三節 毛細管電層析之應用 59 3-1 前言 59 3-1.1 磷酸緩衝溶液 pH 值之影響 60 3-1.2 動相濃度影響 62 3-2 酸性分子之分離 70 3-2.1 動相組成影響－甲酸及 Tris 緩衝溶液 73 3-2.2 緩衝溶液的修飾劑 77 3-2.3 動相組成影響－EDTA 緩衝溶液 81 3-2.4 動相濃度影響 82 第四章 結論 93 參考文獻 95 Fig. 1-1. Flow profile driven by pressure and by EOF.----------------------4 Fig. 1-2 .Sterns Model and ζ potential.-----------------------------------------5 Fig. 1-3. Development of the electroosmotic flow.---------------------------6 Fig. 1-4. Structure of polyelectrolyte multilayer.----------------------------13 Fig. 1-5. Steps in the formation of a supported phospholipid bilayer.----13 Fig. 1-6. Porphyrin binding in the surface of capillary.--------------------14 Fig. 1-7. Steps of BSA binding in the Porous-layer.-----------------------14 Fig. 1-8. Structures of TiO2 monocrystal and crystals.---------------------17 Fig. 1-9. Proposed hydroxyl groups on hydrolysate surfaces.------------18 Fig. 1-10. Phosphate adsorption onto the surface of TiO2.----------------18 Fig. 1-11. The relationship between α value and pH of TiO2.------------18 Fig. 1-12. Structures of plant phenol.----------------------------------------31 Fig. 2-1. Homemade capillary washing kit.---------------------------------40 Fig. 2-2. Capillary filling and washing kit.----------------------------------40 Fig. 3-1. The MO structure of different molecular system.----------------43 Fig. 3-2. Absorption spectrum of TiO2 NPs with 10% TIP precursor.---43 Fig. 3-3. Absorption of TiO2 NPs at different reaction time.--------------44 Fig. 3-4. Absorption of TiO2 NPs at different reaction temperature.-----44 Fig. 3-5. Absorption spectrum of TiO2 NPs with 20% TIP precursor. --45 Fig. 3-6. Absorption spectrum of TiO2 NPs with 30% TIP precursor. --45 Fig. 3-7. TEM of TiO2 NPs synthesized from the sol-gel method.-------46 Fig.3-8. TEM of concentrated TiO2 NPs. -----------------------------------52 Fig.3-9. Electroosmotic mobility of different columns.-------------------57 Fig.3-10. (a) Electroosmotic mobility of TiO2 NPs columns (formate/ Tris buffer) (b) The relationship between α value and pH.--58 Fig. 3-11. Electrochromatographic separation of plant phenols at acidic condition.-------------------------------------------------63 Fig.3-12. Electrochromatographic separation of plant phenols at basic condition.---------------------------------64 Fig. 3-13. Electropherograms of plant phenols at different pH value.-------------------------------------------------65 Fig. 3-14. Electropherograms of plant phenols at different buffer concentration.-------------------------------------66 Fig.3-15.Comparison separation of plant phenols with different columns.---------------------------------------------------67 Fig. 3-16. Separation of plant phenols under various concentration of phosphate buffer.------------------------------------------------68 Fig.3-17. Electrochromatographic separation of phenolic acids at formate buffer.----------------------------------------------------78 Fig. 3-18. Electrochromatographic separation of phenolic acids at formate /Tris buffer.-----------------------------------------------79 Fig. 3-19. Electrochromatographic separation of phenolic acids at different amount of ethanol.--------------------------------------80 Fig. 3-20. Electrochromatographic separation of phenolic acids at EDTA buffer injected from negative end.-------------------84 Fig. 3-21. Electrochromatographic separation of phenolic acids at EDTA buffer injected from positive end -------------------85 Fig. 3-22. Electrochromatographic separation of phenolic acids at phosphate buffer. -----------------------------------------------86 Fig. 3-23. Electrochromatographic separation of phenolic acids at EDTA buffer.----------------------------------------------------87 Fig. 3-24. Separation efficiencies of phenolic acids under various concentration of EDTA buffer.-----------------------------------91 表目錄 Table 3-1. Concentration of TiO2 after vacuum distillation of 1-propanol---------------------------------------------------------50 Table 3-2. Stability of TiO2 prepared with different concentration of precursor-----------------------------------------------------------50 Table 3-3. Effect of the column preparation on the EOF mobility------51 Table 3-4. Separation efficiencies of plant phenols under various pH of phosphate buffer---------------------------------------------------69 Table 3-5. Retention time repeatability in the CEC separation of plant phenols----------------------------------------------------69 Table 3-6. Effective charge of plant phenols--------------------------------71 Table 3-7. Relative mobility of phenolic acids------------------------------72 Table 3-8. Some possible reactions between the surface of TiO2 NPs and organic functional groups-----------------------------------------74 Table 3-9. Retention time(min) of phenolic acids under various pH Table 3-10. Separation efficiencies of phenolic acids under various pH of EDTA buffer-------------------------------------89 Table 3-11. Separation efficiencies of phenolic acids under various pH of EDTA buffer-------------------------------------90 Table 3-12. Retention time repeatability in the CEC separation of phenolic acids injected from negative end-----------------92 Table 3-13. Retention time repeatability in the CEC separation of phenolic acids injected from positive end------------------92 | |
| dc.language.iso | zh-TW | |
| dc.subject | 二氧化鈦 | zh_TW |
| dc.subject | CEC | en |
| dc.title | 二氧化鈦塗佈管柱之製備及其以毛細管電層析分析植物酚類之應用 | zh_TW |
| dc.title | Titanium dioxide sol-gel coated column for the capillary electrochhromatographic separation of plant phenols | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 94-2 | |
| dc.description.degree | 碩士 | |
| dc.contributor.oralexamcommittee | 魏國佐,王書蘋 | |
| dc.subject.keyword | 二氧化鈦, | zh_TW |
| dc.subject.keyword | CEC, | en |
| dc.relation.page | 99 | |
| dc.rights.note | 有償授權 | |
| dc.date.accepted | 2006-07-25 | |
| dc.contributor.author-college | 理學院 | zh_TW |
| dc.contributor.author-dept | 化學研究所 | zh_TW |
| 顯示於系所單位： | 化學系 | |
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