- 學位論文
聚苯乙烯整體成形管柱與質譜儀偵測法在毛細管電泳技術的開發及應用
Development and Application of Polystyrene-based Monolithic Capillary Column and Mass Spectrometric Detection on Capillary Electrophoresis Technique
摘要
本研究主要為毛細管電泳的發展與開發，分為兩部分，第一部分主要發展有機共聚物作為毛細管電層析整體成形管柱，並且利用的方法分離藥妝類產品中的防腐劑。在本研究中首次使用Sodium 4-vinylbenzenesulfonate (BSA)單體作為毛細管電層析的帶電荷單體，實驗中探討聚合時間變化對聚苯乙烯共聚物之比表面積、型態及分離效率的影響。並藉由改變動相pH值、離子濃度與乙腈含量，探討分離管柱特性並且最佳化動相條件。成功應用到酸性物質的分離，使此管柱在低pH值的應用被證實其可行性。當使用有效長度為10 cm的分離管柱，防腐劑標準品可於2.5分鐘完成分離，如此超快速的分離速度，在CEC分離方法中很少見。 毛細管電泳相較於液相層析有較高的分離效率及低溶劑使用量，而質譜儀在近十年成為分子結構鑑定最關鍵的工具。因此第二部分的實驗，結合毛細管電泳與電灑質譜儀分析植物中的二級代謝物-酚酸。先以非水相毛細管電泳成功分離酚酸化合物，並且最佳化質譜儀的實驗參數(鞘流種類、鞘流流速、乾燥氣體與霧化氣體流速等…)，使得CE/MS的方法能大幅降低酚酸的偵測極限及結構定性的能力。
關鍵字
毛細管電泳並列摘要
In the study, the development and application of Capillary Electrophoresis Technology were divided into two parts. The first part of this study, polymeric monolithic capillary columns of capillary electrochromatography (CEC) were developed and used to separate preservatives in commercial products. This work demostated that the first usage of Sodium 4-vinylbenzenesulfonate (BSA) as charge-carried monomer in CEC column. Effect of polymerization time of poly(styrene-divinylbenzene-4-Vinylbenzenesulfonic acid) on the surface area, morphology and separation efficiency were examined . Buffer pH, ionic concentration and acetonitrile content in mobile phase were examined in order to evaluate properties of separation column and optimize mobile phase for separation. This work demostated that this PS-DVB based monolithic column was feasible and could be also applied to the analytes of acidic compounds. The separation time for seven tested analytes was able to be shorten to 2.5 min when the effective length of the monolithic column was reduced as 10 cm (from the inlet to the detector), this ultrafast separation speed was less found when compared to most CEC report. Compared to that of liquid chromatography, Capillary electrophoresis (CE) has higher separation efficiency and lower usage of solvent. In recent ten years, mass spectrometry (MS) has become a key tool for the characterization molecule. In this study, a CE separation coupled to an ESI-MS technology (CE/ESI-MS) was developed for determination of phenolic acid that are found as commonly secondary metabolites in plant. First, a nonaqueous capillary electrophoresis (NACE) method was used to separate seven phenolic acids, and then MS parameter (sheath liquid composition, sheath liquid flow rate, dry gas flow, nebulizing gas flow) was examined in order to achieve optimal mass sensitivity for each phenolic acids. This study demonstrated that the both detection limit and separation resolution of phenolic acids were enhanced successfully by the coupling of NACE and MS technology.