摘 要
　　將β-環糊精(β-cyclodextrin)各葡萄糖單體上C(2)、C(3)位置之二級羥基衍生化成丁醇基，並將GPTMS 與環糊精衍生物C(6)位置反應，接上silica 粒子，最後脫去保護基，完成在環糊精上衍生化長鏈羥基的目的，所有步驟皆以NMR 定性。完成反應之silica 衍生物粒子以高壓填入空的熔融矽膠毛細管，利用整體管柱技術，製備μ-HPLC的新靜相管柱；製備方法是將毛細管內壁表面活化後，填入3μm 靜相粒子，再注入TMOS 與EtMOS 混合膠體，並進行縮和反應，將3μm 矽膠粒子固定在毛細管柱中，形成整體管柱。實驗中解決過去充填3 μm 靜相粒子所遇到的瓶頸，同時改善製備整體管柱時，管柱內容易產生氣泡，造成管柱不連續的問題。

　　所製備的整體管柱利用一系列多環芳香烴(PAHs)，經由分離參數的改變，測定其滯留時間變化，以評估新型靜相的性質。研究發現以下三點結果：1.該反應路徑能以高產率進行一系列環糊精衍生化反應。2.修正充填技術後的乾式充填法，可提高充填3μm 粒子成功率。3.注入11 種濃度為100 ppm 的PAHs 分析物，以體積比為40%的氰甲烷的水溶液，偵測分析波長為240、254、280nm。測試結果顯示新靜相阻塞空腔口，對於PAHs 分離效果不理想。

Abstract
　In this study, we focus on transferring the functional groups in each glucoses-linked of β-cyclodextrin, especially on the hydroxyl groups of the C2 and C3 positions as well as the C6 terminal hydroxyl group.
First, the hydroxyl group in C2 and C3 positions have used synthesized by 1-bromo-butanol to be the primary butanol species.

　On the other hand, to combine the silica particle molecule linked the primary alcohol at C6 position by using GPTMS and continued deprotecting the functional groups. All synthesized intermediate compounds were independently and conduct spectroscopy characterization including 1H-NMR and 13C-NMR.

　The terminal silica-linked β-cyclodextrin was added into the fuse capillary by high-pressure and using monolithic column technique，to prepared newly column for μ-HPLC. In addition, the prepared method by re-actively inside surface of capillary, added stationary phase and the gel combined TMOS with EtMOS for condensation reaction for 3 μm silica
particles bonding at surface in capillary to be a monolithic column. In past experiences, the method of packing 3 μm silica particle molecules into prepared-column were difficult problems, and we have salve this problem, by the way , we have saw out the bubble problem
when we make up a column, that will cause the broken wall in the column.

　As result, this study was developed three excellent points. The first, we can synthesized the different protect groups of β-cyclodextrin in good yields. The second, we revised the technique of drying packing column in
good yields when we packing 3μm silica particle. The third, we loading the PAHs compounds to test the column, the data seems that the CD’s hole was block up, and the result was not fit in with early supposition.

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