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In this study, supercritical carbon dioxide purified Molecular distillated Soybean Oil Deodorized Distillates (MDSOD) semi-batchly and continuously, respectively, in order to concentrate tocopherols. Initial experimental data showed that when 31.0MPa 60(Bottom)~80(Top)oC, and 1000L CO2 extracted a feed containing 11.58% tocopherol, total yield is 65.48﹪, and the recovery of tocopherols is 65.48%, the concentration factor is 1.28. When 150L CO2 at 31.0Mpa and 60(Bottom)~80(Top)oC extracted MDSOD which contains 44.02﹪tocopherols continuously, the recovery of tocopherols is 10.57% and the concentration factor is 1.20 in the extracted oil . The result above is similar to the result of simulation research (Pessoa et al.,2000).
Our results further indicated that when 600L CO2 at 12.4Mpa and 40 oC (Bottom)~60 oC (Top) extracted semi-batchly a esterified and sterolsfree MDSOD, which contains 47.94﹪tocopherols, total yield, and concentration factor of tocopherols is 45.47﹪, 70.38﹪and 1.55
,respectively. When semi-batchly extracted another esterified MDSOD without sterols removing which contains 44.02﹪tocopherols at 12.4 MPa
,50~70oC and 900L CO2, total yield is 56.92﹪, the recovery and concentration factor of tocopherols is 85.58% and 1.57, respectively. In the same raffinate the recovery and concentration factor of sterols is 89.41% and 1.5, respectively; the recovery and concentration factor of squalene is 92.17﹪and 1.63. Finally when continuously extracted the latter esterified feed at 12.4 MPa ,50~70oC, the recovery and concentration factor of tocopherols is 52.90% and 1.35 respectly, after 200L CO2 usage. Both semi-batchly and continuously supercritical carbon dioxide extraction of esterified MDSOD feeds revealed that tocopherols, sterols and squalene could be concentrated in the raffinate. Our investigations concluded that supercritical carbon dioxide extraction not only could increase the concentration factor of tocopherols, but also separate fatty acids methyl ester effectively in the countercurrently continuous operation.
本研究以超臨界二氧化碳，分別進行半批式與連續式萃取分子蒸餾濃縮之黃豆油脫臭液(或將其甲酯化後之脫臭液)，期能製備高純度維生素E油。實驗數據顯示，半批式萃取[31.0MPa,70(塔底)~90(塔頂)℃,1000L]含11.58﹪維生素E原脫臭液，可得65.48﹪總產率及83.55﹪維生素E回收率與1.28濃縮倍數的萃出油。再以31.0MPa,60(塔底)~80(塔頂)℃,150LCO2連續萃取含44.02﹪維生素E油的分子蒸餾濃縮之脫臭液，僅得10.57﹪回收率和1.20倍的維生素E萃出油。上述不理想的實驗結果與Pessoa et al.(2000)模擬研究來分離維生素E與脂肪酸的結論相似。
本研究再以甲酯化之兩種脫臭液作為進料。當半批式萃取(12.4MPa,40~60℃,600L) 含47.94﹪維生素E的去固醇甲酯化進料，可得70.38﹪回收率及1.55濃縮倍數的維生素E萃餘油，但僅得45.47﹪產率。當半批式萃取(12.4MPa,50~70℃,900L) 含42.48﹪維生素E的未去固醇甲酯化進料，可得56.92﹪產率及維生素E85.58﹪回收率及1.5濃縮倍數的萃餘油，而固醇類有89.41﹪回收率及濃縮倍數亦達1.57，同時在塔底角鯊烯亦有92.17﹪回收率及濃縮倍數可達1.63。若以12.4MPa及50~70℃連續式逆向萃取未去固醇之甲酯化進料，在200升CO2用量時，可平均得52.90﹪維生素E回收率及1.35濃縮倍數。本研究總結超臨界二氧化碳不但可提高甲酯化脫臭液中維生素E的濃縮倍數，亦可有效分離出游離脂肪酸甲酯物。
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