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|標題:||Extraction and Purification of Isoflavones and Saponins from Defatted Soybean Flakes using Hot Pressurized Fluids
Hsun, Chang Li
|關鍵字:||熱壓流體;Hot pressurized fluids;實驗設計;脫脂大豆粉;異黃酮;皂素;萃取及純化;experimental design;defatted soybean flakes;isoflavones;soyasaponins;extraction and purification||出版社:||化學工程學系||摘要:||
本研究首先探討，批式熱壓流體萃提脫油大豆粉中五種異黃酮素及總皂素的可行性，並以陡升實驗設計法求得萃提之適當條件。並應用於半連續式之程序。隨後，探討壓力（60~735 psig），溫度（60~120 C），溶劑流速（10~25 ml/min），及固溶比對大豆異黃酮素之回收率的影響。再以田口實驗設計法檢驗，何種萃提條件是影響回收率的主要因子。由陡升實驗設計結果顯示，批式熱壓水自180g DSF粉中萃取異黃酮之適當條件為110 C，641 psig及2.3 hours，並得到99.72 %的總異黃酮回收率。另外，在批式及半連續式的萃提製程中，溫度是主要的影響因素，且壓力在100 psig 至640 psig，對回收率沒有影響。接續的半連續式實驗又發現，當增加溶劑流速，減少固體進料，及高乙醇含量之水溶液時，可提高大豆中異黃酮與皂素的回收率。田口實驗設計結果得到，高乙醇含量（95 % EtOH）與高溶劑流速（25ml/min）是影響回收率的兩大因子。以Amberlite XAD16-HP樹脂對熱壓水萃出液進行分離和純化，得到9.40 %產率，36.98 %純度 及48.95 %的異黃酮素回收率。當以DIAION HP21樹脂純化時，可得到9.37 %產率，38.40 %純度 及66.16 %的異黃酮素回收率。最後，以Amberlite XAD16-HP樹脂對熱壓乙醇萃出液進行分離和純化，可得到7.34 %產率，58.00 %純度 及40.90 %的異黃酮素回收率。諸純化實驗結果，五種異黃酮素的回收率接近99 %。
This study preliminarily inspected the batch hot pressurized water extractions of five isoflavones and saponins from defatted soybean flakes (DSF) using the simulation optimization approach known as “steepest ascent”. A suitable condition of batch hot pressurized water extraction was applied to carry out the semi-continuous process testing. Then, the effects of process pressure (60~735 psig), process temperature (60~120 C), flow rate (10~25 ml/min) of solvent, and the solid to solvent ratio were investigated in terms of solubility, total yield, and the recovery of five isoflavones. Finally, Taguchi experimental design was used to examine the influence of each independent variable on the recovery of total isoflavones (TIF) and total soyasaponins (TSP) extracted using semi-continuous process. The steepest ascent design of batch hot pressurized water process revealed that extraction at 110 C, 641 psig and 2.3 hours did recovery 99.72 % TIF from 180g DSF. Furthermore, the temperature effect is predominant for batch as well as semi-continuous hot pressurized fluid extractions, and no pressure effect between 100 and 640 psig. It also revealed increasing the flow rate of fluids or decreasing the loading of DSF, and high content of ethanol should enhance the recovery. Taguchi method definitely disclosed that the content of ethanol (95 % EtOH) and flow rate (25 ml/min) of solvent are two major operating parameters affecting the recovery of TIF and TSP for the semi-continuous process. Purifying the extracts from batch hot pressurized water obtained a solid with 9.40 % yield, 36.98 % purity, 48.95 % TIF recovery and a solid with 9.37 % yield, 38.40 % purity, 66.16 % TIF recovery, by individually using Amberlite XAD16-HP and DIAION HP21 resins. Finally, Amberlite XAD16-HP resin purified the extract from hot pressurized ethanol could obtain a solid with 7.34 % yield, 58.00 % purity, and TIF 40.90 % recovery. The overall recoveries of TIF from all purifications are closed to 99 %.
|Appears in Collections:||化學工程學系所|
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