利用單變數與多變數方法進行毛細管電層析分析非類固醇抗發炎藥物之最佳化

Optimization of Non-steroidal Anti-inflammatory Drugs Analyses by Capillary Electrochromatography Using Univariate and Multivariate Approaches

許朝祥(Chao-Hsiang Hsu)

指導教授 ： 黃悉雅

中原大學/理學院/化學研究所/碩士(2010年)

https://doi.org/10.6840/cycu201000487

摘要

摘要
本篇論文進行毛細管電層析技術的研究，分成兩部分討論。第一部分討論有機高分子整體成形管柱之開發，以甲基丙烯酸十八烷基酯與二乙烯苯單體，製備整體式毛細管柱，並應用在毛細管電層析分離九種非類固醇抗發炎藥物。以單變數與多變數方法兩種方式對管柱效能進行最佳化。單變數方法每次只改變組成中(單體含量、單體組成比例、反應時間及孔洞溶劑)之其中某一變數，同時藉由多變數方法，利用四個變數條件，每個變數有三個階層，同時改變兩個變數以上去製備9支管柱，在考慮分析物解析度的情況下，可找出每個變數中最佳化條件，再與單變數方法之最佳化條件加以比較。最後將最佳化管柱結合線上樣品濃縮步驟的階段式梯度沖提方法，探討非類固醇抗發炎藥物分析之效能。研究顯示在十分鐘內完成九種非類固醇抗發炎藥物分離。而結合線上樣品濃縮技術，使分析物之偵測極限降低約150倍，偵測極限範圍為3.4-10.3 ng/mL。將此方法應用在水樣品檢測上，可成功檢測水樣品中50 ng/mL含量的非類固醇抗發炎藥物。
本研究第二部分討論離子液體(ionic liquids, ILs)做為溶劑製備整體成形管柱，選擇甲基丙烯酸丁酯，乙二醇二甲基丙烯酸為單體。將製備的整體成形管柱應用在CEC上，分離六種烷基苯類。藉由改變ILs中陽離子碳鏈數、陰離子種類、聚合時間及聚合溫度。結果顯示ILs可成功取代傳統溶劑製備整體成形管柱，以減少環境上的汙染，並且成功分離六種烷基苯類。

關鍵字

毛細管電層析

並列摘要

Abstract
In the thesis, capillary electrochromatography (CEC) technique was studied and divided into two parts. In the first-part of the study, development of organic polymer-based monolithic column was investigated. Stearyl methacrylate and divinylbenzene were monomers, which were used to prepare monolithic column. The monolithic column was applied to nine non-steroidal anti-inflammatory drugs (NSAIDs) separation by CEC. Optimization efficiency of the column using univariate and multivariate approaches. In the univariate approach, discussion about optimization of the column (ratio of monomer level, component ratio of monomers, reaction time, and composition of porogenic solvent) changed a level in each parameters. Subsequently, the polymerization procedure was optimized by varying the four parameters likely to have the most significant effect on the resolution of IND and DIC. The polymerization was performed at three levels of each parameter, then compared with optimization of the column in the univariate approach. Finally, optimization of the column coupled step-gradient elution of on-line sample concentration which was examined for the separation efficiency of NSAIDs.
This study indicated that the nine NSAIDs have achieved a reproducible baseline separation within 10 min. For detection limit of nine NSAIDs, optimization of the column with on-line sample concentration could improve to about 150 times. The detection limit was in the range of 3.4 to 10.3 ng/mL. This method has been applied to water analyses with 50 ng/mL NSAIDs detected successfully.
In the second-part of this study, preparation of monolithic column with ionic liquids as solvent was studied. Both butyl methacrylate (BMA) and ethylene dimethacrylate (EDMA) were used as monomers for synthesis of stationary phase. The monolithic column was applied to six alkylbenzenes separation by CEC. The effect of the polymerization condition of the stationary phase (the different carbon chains of cation and types of anion of ionic liquids, reaction time, and reaction temperature) which were examined for separation efficiency of alkylbenzenes. The result showed that monolithic column was prepared successfully, and reduce environmental pollution. The poly(BMA-EDMA) monolithic column was applied to six alkylbenzenes separation successfully.

並列關鍵字

capillary electrochromatography

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