- 學位論文
利用混摻活性碳之高分子整體成形管柱微萃取酚酸化合物
Solid-Phase Microextraction of Phenolic Acid Using Activated Carbon-Polymer Monolithic Column
摘要
本論文探討利用活性碳混摻高分子整體成形管柱對酚酸化合物萃取效果的影響，研究主要分為兩大部分進行探討，一為建立九種酚酸化合物的層析方法，二為探討活性碳(Activated carbon，AC)混摻高分子整體成形管柱對酚酸化合物之萃取效果，並搭配極致效能液相層析分析儀(Ultra Performance liquid chromatography，UPLC) 進行分析。 第一部分所建立九種酚酸化合物之層析方法的分離時間為22 mins，Intra-day及Inter-day面積相對標準偏差(relative standard deviation，RSD)為0.2~1.8%和0.2~1.6% (n=6)，線性迴歸係數(R2)均為0.9998，偵測極限為0.011~ 0.082 μg/mL，定量極限為0.025~ 0.270 μg/mL。第二部分比較未混摻及混摻活性碳之高分子整體成形管柱對酚酸化合物的萃取效能，並探討活性碳高分子萃取管柱的最佳化條件。結果顯示含50 wt% AC、萃取管柱長度4公分、脫附溶劑為0.5 mL的甲醇溶劑(含1.0 % H3PO4)為最佳化條件，得酚酸化合物萃取回收率為72.82~100.97 %，RSD低於1.3 %。Intra-day及inter-day回收率分別為75.8~ 99.8 %及74.3~100.1 %，RSD分別低於1.4 %及2.7 %；Column to column回收率為72.8~100.5 %，RSD低於2.0 % (n=6)。由結果得知，AC結合高分子整體成形管柱(AC-polymer)應用於酚酸化合物有良好的萃取效果及再現性。最後，將活性碳萃取管柱應用於實際樣品中的水果酒和蔓越莓汁，從結果得知，可成功萃取實際樣品中的酚酸化合物，並添加標準品於水果酒和蔓越莓汁的回收率分別為76.4~101.0 %及73.4~100.5 %。
並列摘要
In this study, activated carbon-polymer monolithic column was examined for the extraction of phenolic acid. This dissertation is divided into two parts: (a) a separation method to determine the nine phenolic acids was established and (b) the extraction efficiencies of phenolic acid using activated carbon-polymer monolith were analyzed using ultra performance liquid chromatography (UPLC). The first part was based on the separation of nine phenolic acids, which afforded a separation time of 22 min, with intra- and inter-day area relative standard deviation (RSD) ranged of 0.2 to 1.8% and 0.2 to 1.6%, respectively. The linear regression coefficient (R2) was 0.9998. The limit of detection and quantitation were in the range of 0.011 to 0.082 μg/mL and 0.025 to 0.270 μg/mL, respectively. The second part was conducted based on the extraction efficiencies of the neat-polymer and AC-polymer of phenolic acids, in which the AC-polymer column was optimized. The optimized condition for AC-polymer monolithic column contains 50 wt% AC, 4 cm of extraction column and 0.5 mL MeOH (containing 1.0% H3PO4) as elution solvent. Based on the optimized results, the recoveries of phenolic acid were in the range of 72.82 to 100.97% with RSD less than 1.3%. The intra-day extraction recoveries were found to be in the range of 75.8-99.8% (<1.4 % RSDs) while 74.3 to 100.1% (<2.7% RSDs) for the inter-day extraction recoveries. The recoveries for column-to-column were in the range of 72.8 to 100.5 % (<2.0% RSDs). Based on the above results, the AC-polymer demonstrated a remarkable extraction efficiency with good reproducibility for phenolic acids. Finally, the AC-polymer was used to extract phenolic acids in fruit wine and cranberry juice samples. The results showed that the AC-polymer column could extract the spiked phenolic acids in fruit wine and cranberry juice samples with recovery ranged of 76.4 to 101.0% and 73.4 to 100.5%, respectively.
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