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  • 學位論文

有序中孔碳材 CMK-3 結合高分子製備整體成形材料對磺胺類藥物與防腐劑進行固相微萃取

Fabrication of orderd mesoprous carbon CMK-3-polymer monolith for solid-phase microextraction of sulfonamide antibiotics and parabens

指導教授 : 黃悉雅

摘要


本論文率先運用中孔有序碳材(orderd mesoporous carbon, OMC)CMK-3之大表面積、大孔洞體積與均一孔徑分佈等優勢,結合高分子製備CMK-3-高分子(CMK-3-polymeric monolith, CMK-3-polymer)整體成形材料,以其做為SPME的吸附材,針對磺胺類藥物(sulfonamides)及防腐劑(paraben)進行固相微萃取(solid-phase microextraction, SPME)。實驗過程使用石墨烯(graphene)、活性碳(activated carbon, AC)、CMK-3及CMK-8四種孔洞碳材做為吸附劑萃取磺胺類藥物及防腐劑,個別進行萃取條件最佳化,並以毛細管電泳(capillary electrophoresis, CE)進行回收率之檢測,最後比較不同結構及孔洞性質的孔洞性碳材對於分析物萃取效果差異。 實驗結果顯示,以32 wt% CMK-3所製備之CMK-3-polymer,對磺胺類藥物萃取擁最好萃取回收率,原因為中孔有序碳材除了本身碳結構芳香環具豐富π電子結構外,更具有均一且有序的2D中孔結構,使分析物與CMK-3-polymer有大的接觸面積,增強兩者間π-π作用力,其不僅有好的吸附能力亦有好的脫附性能,因此可得79.7 - 100.8%之回收率,column to column回收率76.8 - 99.1%且相對標準偏差(relative standard deviation, RSD%)(n=3)小於3.6%,可知CMK-3-polymer具有良好再現性與穩定性。 CMK-3-polymer對於防腐劑亦具有優異的萃取效果,以26 wt% CMK-3、pH 2樣品基質、MeOH做為脫附溶劑為最佳化條件下,對parabens進行固相微萃取,可得回收率為88.9 - 96.6%,RSD小於2.1%,顯示其對於疏水性質之分析物parabens也具有好的萃取效果。

並列摘要


In this dissertation, an ordered mesoporous carbon (OMC), CMK-3, with advantages such as high surface area, pore volume and uniform pore size distribution, was combined with polymer to fabricate a CMK-3-polymeric monolith (CMK-3-polymer) and applied for the first time in solid-phase microextraction (SPME) of sulfonamide antibiotics and parabens. In this experiment, four kinds of porous carbons, graphene, activated carbon (AC), CMK-3 and CMK-8 were used as adsorbent for the extraction of sulfonamide antibiotics and parabens, and individually optimized each extraction conditions, then determined the extraction recoveries by capillary electrophoresis (CE). Finally, the extraction efficiencies of each analytes, which was extracted by different structure and pore characteristics of porous carbon, were compared. The results showed that CMK-3-polymer (32 wt% CMK-3) demonstrated the best extraction efficiency than the other adsorbents for sulfonamide antibiotic extractions. Due to the aromatic structure of OMC, which is rich in π electrons, the existence of homogeneous and ordered 2D mesopore structure is likely possible. The high surface area favored the enhanced the π-π interactions between the analytes and CMK-3-polymer to afford not only a good adsorption but as well as good desorption. The recovery of CMK-3-polymer was in the range of 79.7 to 100.8%, and column-to-column ranged was 76.8 to 99.1% with relative standard deviations (RSDs %) (n=3) of less than 3.6%, indicating its good reproducibility and stability. CMK-3-polymer also afforded excellent extraction efficiency for parabens. Under a optimized conditions in which pH 2 sample matrix, MeOH as eluent for parabens, the recovery ranged were 88.9 to 96.6% with < 2.1% RSDs suggesting that CMK-3-polymer also had an excellent extraction efficiency for parabens, which are hydrophobic analytes.

參考文獻


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