整體成形管柱之毛細管電層析方法檢測酸性化合物：1、帶電荷單體對線上濃縮效果之影響2、新型態聚三烯丙基異三聚氰酸酯類型管柱之開發

Monoliths on the CEC Determination of Acidic Compounds:1.Charged Monomer Effect on Sample Stacking in On-line Concentration Step 2.Development of Novel Poly(triallyl isocyanurate) Monoliths

吳靜宜(Ching-Yi Wu)

指導教授 ： 黃悉雅

中原大學/理學院/化學研究所/碩士(2011年)

https://doi.org/10.6840/cycu201100696

摘要

摘要
本篇論文進行毛細管電層析技術的研究，分為兩部份探討。第一部分討論以甲基丙烯酸十八烷基酯與二乙烯苯(stearyl methacryate-divinylbenzene, SMA-DVB)整體成形式管柱，結合不同帶電荷單體(charge monomer)進行毛細管電層析(capillary electrochromatography, CEC)，探討兩種線上樣品濃縮(on-line sample concentration)模式，場增強樣品堆積注射(field-enhanced stacking injection, FESI)與階段式梯度沖提(step-gradient elution)，對非類固醇抗發炎藥物(non-steroidal anti-inflammatory drugs, NSAIDs)之偵測感度的影響，結果顯示使用正電荷單體(vinylbenzyl trimethylammounium, VBTA)較負電荷單體(sodium 4-vinylbenzenesulfonate, VBSA)有較高的線上濃縮倍率(約1-3倍)。
當以此最佳化靜相條件(poly(SMA-DVB-VBTA)管柱)並結合線上樣品濃縮方法應用於另一酸性化合物，盤尼西林(penicillin)時，顯示在動相為40% acetonitrile 及60 % phosphate buffer (pH 2)的條件下，能在14分鐘內成功分離六種盤尼西林藥物，偵測極限可達十幾ppb左右，相較傳統進樣模式放大倍率約200倍左右。
本研究第二部份討論新型態聚三烯丙基異三聚氰酸酯(triallyl isocyanurate)類型管柱之開發，選擇三烯丙基異三聚氰酸酯、乙二醇二甲基丙烯酸(ethylene dimethacrylate)與甲基丙烯酸十八烷基酯單體聚合成整體成形管柱應用於CEC上，分離八種酚酸化合物，其中藉由改變靜相組成中之單體組成比例、孔洞溶劑組成比例、單體含量與帶電荷單體含量。並與本實驗室之前開發之其他三種管柱比較，結果顯示此新型態管柱對親水性的酚酸化合物具有較佳分離效果。

關鍵字

毛細管電層析 ； 酸性化合物

並列摘要

Abstract
In this study, two types of monolithic columns were developed for the capillary electrochromatographic (CEC) separation of acidic compounds. In the first part, the separation performance of poly(stearyl methacryate-divinylbenzene) monolithic columns carrying two different charged monomers namely, vinylbenzyl trimethylammounium (VBTA) and sodium 4-vinylbenzenesulfonate (VBSA) were tested for the sensitivity enhancement of non-steroidal anti-inflammatory drugs (NSAIDs) by two on-line concentration methods, field-enhanced stacking injection (FESI) and step-gradient elution. Results showed that NSAIDs sensitivities were enhanced with VBTA charged monomer for about 1-3 times than with VBSA. These on-line concentration methods were also examined using 6 penicillin compounds on poly(SMA-DVB-VBTA) monolithic columns and results indicated that reproducible baseline separations within 14 min at phosphate buffer (pH 2) and acetonitrile in the volume ratio of 6:4 were achieved. The detection limit was about 10ng/mL which was about 200 times better compared with normal injection mode.
In the second part of the study, a novel poly(triallyl isocyanurate) based monolithic columns were developed. The synthesized monolithic stationary phase composed of triallyl isocyanurate (TAIC), ethylene dimethacrylate (EDMA) and stearyl methacrylate (SMA) monomers was used for the CEC separation of phenolic acids. The effect of polymerization conditions of the stationary phase (ratio of monomer composition, composition of porogenic solvent and charge-bearing monomer) were examined. This monolithic column was compared with another three types of monolithic columns and results indicated that novel poly(TAIC-EDMA-SMA) had better separation for hydrophilic phenolic acids.

並列關鍵字

acdic compounds ； capillary electrochromatography

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