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以超臨界反溶劑沉澱法進行兒茶素微粒化之研究

Micronization of Catechins Using the Supercritical Anti-Solvent Precipitation Process

摘要


本研究建立連續式超臨界反溶劑(supercritical antisolvent,SAS)沉澱操作系統,以二氧化碳為反溶劑,對兒茶素(catechins)進行微粒化研究。經過初步的溶劑篩選結果發現,使用乙醇或異丙醇為溶劑時,可得到分散之球形微粒;使用丙酮或乙酸乙酯為溶劑時,可得到不規則形狀且輕微聚集之微粒。就顆粒大小與回收率而言,丙酮為最適溶劑,因而選擇丙酮為溶劑,探討壓力、溫度、溶液濃度及溶液進料流速等四種操作參數對粒徑大小之影響。結果發現在120bar壓力、35℃溫度、1.00mL/min溶液流速與45mg/mL溶液濃度下操作可獲得平均粒徑為0.76μm之兒茶素微粒,相較於原始粒徑57.5μm之噴霧乾燥所得樣品,有明顯微粒化效果。此外由總多元酚含量分析結果發現,兒茶素經過SAS微粒化處理後,純度並未顯著改變,顯示SAS沉澱法應用於兒茶素微粒化具可行性。。

關鍵字

超臨界 微粒化 兒茶素 參數效應

並列摘要


The continuous supercritical anti-solvent (SAS) precipitation process was established in this study to micronize catechins using carbon dioxide as anti-solvent. The solvent effect was first studied to explore the suitable solvent used in the SAS process. Spherical non-agglomerated particles were obtained in the experiments using ethanol or isopropanol as solvent, whereas slightly sintered particles with irregular shape were observed using acetone or ethyl acetate. With the consideration of particle size and recovery, acetone was selected as solvent for the further study on the effects of the SAS process parameters including the concentration of the catechin solution, the flow rate of solution, pressure and temperature on particle size distribution. At a higher pressure of 120 bar, a lower temperature of 35℃, a higher solution flow rate of 1.00mL/min and a higher concentration of 45mg/mL, the size of catechins particles was reduced to 0.76μm which showed a significant micronization from the spray-dried particles with particle size up to 57.5μm. No significant change in purity after the SAS process was confirmed by total polyphenolic analysis of catechins.

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