| Summary: | 碩士 === 國立成功大學 === 化學系碩博士班 === 92 === Abstract
In recent years, the development and research of the monolithic column is prosperously. This technique is packing stationary phase particles into a column followed by injecting the sol-gel into the column to carry out cross-linking reaction, which bonding the particles in the column and making the inner wall of column, support and stationary phase into one unity. This kind of column is called monolithic column or sol-gel column. The column could be reached higher efficiency by changing the composition of the sol-gel, controlling the size of the inner diameter and porosity of the monolithic column. It also could separate enantiomeric drugs by using some specific stationary phase particles.
Cyclodextrins, which utilizing it’s cavity to complex with a variety of enatiomers, have used extensively to separate enantiomeric drugs by the diffferents stability of the enantiomeric inclusion complex formation. Acetylated β- CD to form 2,3-di-O-acetyl-6-O-β-CD, which directly react with (3-Glycidoxypropyl)trimethoxysilane then bonded to silica particles . To prepare the monolithic column is packing the particles into the capillary column, then using Sol-Gel to fix it in the column.
Using Naphthalene、Acenaphthene、Phenanthracene、Fluoranthene and Pyrene to test the size of Acetyl-β- CD’s cavity and the efficiency of the column. Changing the sort of the solvent, using methanol will get more resolution then Acetonitrile. Changing the percentage of solvent and water, using Acetonitrile and raising the percentage of water will increase the resolution of those. But using methanol and changing the percentage of water, won’t increase the resolution of Fluoranthene and Pyrene.
Using diamethyl-2-(2-(p-toluidino)-4-methylpent-1-en-3ylamino)- 2-(4-hydroxyphenyl)acetate and methyl-2-(2-(p-toluidino)-4-methyl- pent-1-en-3-ylamino)-3-phenylpropanoate to test the character of the molecules entering the Acetyl-β- CD’s cavity. The result is that the phenyl group is the position to enter the Acetyl-β- CD’s cavity. And the phenyl group’s para-position has hydrophilic group, it can’t be resoluted. (D,L)-1-phenyl-ethylamine is to confirm the mechanism of the chiral separation. This column can separate (D,L)-1-phenyl-ethylamine.
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