毛細管電層析之聚苯乙烯整體成形管柱的製備與應用

Preparation and Application of Polystyrene Monolithic Column for Capillary Electrochromatography

林衡毅(Heng-Yi Lin)

指導教授 ： 黃悉雅

中原大學/理學院/化學研究所/碩士(2005年)

https://doi.org/10.6840/cycu200500616

摘要

摘要
　　本研究主要為發展有機高分子聚苯乙烯整體成型管柱，並將其應用於毛細管電層析之靜相上。文中對於聚合高分子反應設計了一系列的變因，包含了改變單體比例、孔洞溶劑比例、聚合反應時間與帶電荷源等，並藉由這些條件對高分子的型態與分離效能做討論。於動相的組成部分，對於緩衝溶液的pH值，乙腈含量與緩衝溶液之離子濃度做有系統的研究，尋找聚苯乙烯管柱的最佳化分離條件。
　　本研究的實驗區分為兩部分，第一部分之管柱最佳化製備條件為25%的單體，50%的甲苯，所需聚合反應時間為12小時與25%的甲基丙烯酸。於第二部分，使用乙烯磺酸取代先前所使用的甲基丙烯酸，目的在於使聚苯乙烯管柱可應用的pH值更廣，而此部分的最佳製備條件為50μl的乙烯磺酸配以46.6%的環己醇、50%的二甲基乙醯胺和5%的水。本實驗成功地將甲基丙烯酸置換成乙烯磺酸，最後在低pH值下能有效的檢驗實際樣品中所含的分析物。

關鍵字

毛細電層析

並列摘要

Abstract
In this study, a series of polystyrene monolithic column was for the developed usage of stationary phase in capillary electrochromatography (CEC). In order to optimize the separation performance, the effects of the polymerization conditions of the polymeric stationary phase, the pH and composition of the mobile phase on separation were examined. It was found that an increase in monomer content or toluene content caused a reduction in retention time. However, separation performances were greatly improved in monolithic columns with larger monomer or toluene content. In addition, the composition of mobile phase including buffer pH, acetonitrile concentration and ionic concentration was determined significantly the resolution and efficiency for parabens separation.
The experiment is divided into two sections. In section one, an optimal paraben separation was achieved when polystyrene monolithic column prepared by 25% monomer, 50% toluene, and 25% methacrylic acid under 12hr reaction. In section two, methacrylic acid was charged-bearing monomer polymerization replaced by vinylsulfonic acid for the preparation of PS monolithic column. The optimal column was obtained when the porogenic solvent was composed by 46.6% cyclohexanol, 50% N,N-dimethylacetamide (DMAc), 5% H2O, and 50μl vinylsulfonic acid was used as charge-bearing monomer. Finaly, several preservatives in real sample were successfully determined by the poly(styrene-co-divinylbenzene-co-vinylsulfonic acid) monolithic column under pH3.0.

並列關鍵字

Monolithic Column ； Capillary Electrochromatography

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