奈米粒子應用於毛細管電層分析鏡像異構物

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题名:	奈米粒子應用於毛細管電層分析鏡像異構物 Application of nanoparticles in capillary electrochromatographic analysis of enantiomers
作者:	許宏杰
贡献者:	藥學系碩士班
关键词:	毛細管電層析法;奈米殼聚糖;奈米碳管;氯化銅;多孔層開管式毛細管電層析管柱;開管式管柱;掌性化合物;兒茶素;色胺酸;苯苷胺酸;纈胺酸;類黃酮;含氮鹼基;核苷 Capillary electrochromatography;carbon nanotubes;open-tubular capillary;nano-chitosans;catechin;phenylglycine;valine
日期:	2011-06-23
上传时间:	2011-10-17 17:03:59 (UTC+8)
出版者:	中國醫藥大學
摘要:	毛細管電層析 (capillary electrochromatography; CEC) 乃是結合高效液相層析法 (high performance liquid chromatography, HPLC) 與毛細管電泳法 (capillary electrophoresis, CE) 的操作特性之新分離系統。本研究擬結合奈米粒子，合成一新型開管式毛細管電層析固定相管柱，結合奈米聚殼醣 (chitosan, CS)、GTPMS(γ(3)-Glycidoxypropyl -trimethoxysilan)與TEOS(Tetra-ethoxysilane)，形成管柱之固定相，並依合成順序不同分為三管柱，以討論合成步驟的不同對於分析結果的差異性，以及最佳化條件。除調整最佳毛細管電層析分析條件，分析物結構同樣影響分析速度因子 (velocity factors) 與遷移因子 (retention factors)，本實驗中選用兒茶素、丙胺酸、苯苷胺酸及色胺酸等具有掌性異構物的有機分子做為分析樣品，並藉觀察樣品在不同管柱的最佳分析條件，希望未來分析其他掌性物質能夠藉此結果合成合適管柱以及尋找最佳條件。第二篇的研究為利用 bare fused silica 毛細管，利用 3-(trimethoxysilyl)- propylmethacrylate (γ-MAPS)試劑進行烷矽化反應，使得丙烯酸 (acrylate) 能夠在接下來的聚合反應中連接在毛細管內壁上。接著以butyl methacrylate (BMA) 為單體、ethylene dimethacrylate (EDMA) 為聯接劑，再加入奈米碳管 (carbon nanotubes, CNTs)和氯化銅做為功能性單體，利用化學鍵結在經 γ-MAPS 處理過的毛細管壁上製備一種多孔層開管式(porous-layered open-tubular, PLOT)毛細管電層析管柱 (BMA-CNT-Cu-N)。將上述的混合溶液中的加入還原劑borane morpholine complex(C4H12BNO)成製備成 BMA-CNT-Cu-R 毛細管電層析管柱。利用這兩種管柱運用在類黃酮、含氮鹼基、核苷和掌性異構物(如：兒茶素、苯苷胺酸及纈胺酸)樣品的分析及探討電層析參數的影響。探討添加氯化銅是否有幫助以及將BMA-CNT-Cu-N與BMA-CNT-Cu-R管柱對類黃酮、含氮鹼基、核苷及掌性異構物(如：兒茶素、苯苷胺酸及纈胺酸)樣品的最佳分析條件進行比較。根據以上的研究結果，未來可以運用在生藥樣品及掌性異構物的分析。 Capillary electrochromatography (CEC) is a new and exciting hybrid separation technique that seeks to exploit the combined advantages of both capillary electrophoresis and high performance liquid chromatography. The subject of this study is to prepare three new types of open-tubular capillary electrochromatographic (CEC) stationary phases, where nano-chitosans were covalently immobilized in the column with γ(3)-glycidoxypropyl-trimethoxysilan and tetraethoxysilane. By three column synthesis processes, the corresponding separations of alanine, catechin, tryptophan, and phenylglycine will be discussed. Besides the optimizing CEC conditions, chiral compounds were analyzed with respect to velocity and retention factors to respectively evaluate electrophoretic and chromatographic contributions to the CEC mechanism for each analyte. These columns and optimal CEC conditions will be aided to analyze other enantiomers in the future. In the second study, the bridging agent, 3-(trimethoxysilyl) propylmethachylate, was treated on the inner wall of a bare capillary prior to the polymerization of acrylate monomers. The polymerization solution, consisting of butyl methacrylate (BMA) as bulk monomer, ethylene dimethacrylate as crosslinker, carbon nanotubes (CNTs) and copper chloride as functional monomer, was coated on the treated capillary to form a porous-layered open-tubular phases in the electrochromatography capillary (BMA-CNT-Cu-N). Another mixture of BMA-CNT-Cu was added with reducing agent, borane morpholine complex (C4H12BNO), to complete the electrochromatographic capillary (BMA-CNT-Cu-R) in a similar manner. The two capillaries were tried to separate nitrogenous bases, nucleosides, flavonoids and enantiomers, such as catechin, phenylglycine, and valine. The CEC mechanism of these separations was also studied. In order to understand whether the copper chloride in polymerization mixture is helpful or not, the difference of the optimal CEC conditions between BMA-CNT-Cu-N and BMA-CNT-Cu-R columns was compared. The results showed that they will be suitable to analyze the Chinese herbs and enantiomers.
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