- 學位論文
以聚苯乙烯高分子結合活性碳之整體成形管柱進行鄰苯二甲酸酯類化合物的固相微萃取
Poly(styrene-divinylbenzene)/ activated carbon composites for solid-phase microextraction of phthalate esters
摘要
摘要 本論文為探討甲基丙烯酸正丁酯及苯乙烯兩種高分子整體成形管柱，對鄰苯二甲酸酯類化合物(Phthalate esters, 簡稱PAEs)萃取效果之影響，並比較於管柱中添加活性碳之效能。為了建立PAEs之分離技術，本實驗首先以對微胞電層析(Micellar Electrokinetic Capillary Chromatography, MEKC)及超高效液相層析(Ultra Performance Liquid Chromatography, UPLC)進行PAEs分離條件之優化，接著將活性碳分別結合兩種系列高分子單體，製備整體成形微萃取管柱(AC-polymer SPME)，針對鄰苯二甲酸酯類化合物萃取回收率探討各種萃取條件與活性碳對萃取過程的影響。對兩種高分子混摻活性碳整體成形管柱進行參數最佳化，結果顯示兩種高分子混摻活性碳整體成形管柱在萃取管柱同為5公分(62.5 % AC含量)、硼酸鹽類離子濃度為55 mM、1.5 mL 及以乙腈作為脫附溶劑的條件下，以苯乙烯高分子混摻活性碳之萃取回收率較佳，並由實驗結果發現活性碳的存在有助於PAEs的脫附。接著以苯乙烯高分子混摻活性碳整體成形管柱進行(低濃度1 ppm的)八種PAEs萃取，其萃取回收率介於71.6 %-101.4 %，相對標準偏差(n=3)為1.3 %-4.7 %，可看出此萃取管柱具良好再現性與穩定性，將有效應用於實際水樣分析。
並列摘要
Abstract In this study, two types of polymeric monoliths combined with activated carbon (AC), AC-poly(butyl methacrylate-ethylene dimethacrylate) and AC-poly(styrene-divinylbenzene), were prepared via in-situ polymerization and compared their extraction efficiency for phthalate esters (PAEs). In order to establish the PAEs separation method, Micellar Electrokinetic Chromatography (MEKC) and ultra performance liquid chromatography (UPLC) were utilized for the separation and optimization in the extraction efficiency for PAEs using the fabricated AC-polymeric monoliths. Different parameters affecting the extraction efficiency of two AC-polymeric monoliths for PAEs, such as amount of AC, desorption solvent, desorption volume and ion concentration for sample loading, were investigated. The results for both AC-polymer (62.5 wt.% AC), using an extraction column of 5 cm, borates ion concentration at 55mM and 1.5 mL ACN as the desorption solvent, showed that AC-poly(styrene-DVB) has better extraction recovery for PAEs than AC-poly(BMA-EDMA). It was found that the presence of AC has significant effect in PAEs desorption. Under the optimized condition of AC-poly(styrene-DVB), eight PAEs were extracted at low concentrations (1ppm) with recovery range of 71.6% to 101.4% (<4.7% RSD), good reproducibility and stability. Finally, the fabricated column was applied in water sample.