从雄烯二酮发酵废液中分离甾醇和油脂的工艺研究
|
摘要
以雄烯二酮发酵废液为原料,采用有机溶剂萃取法和重结晶的方法对原料进行处理,分离获得甾醇和雄烯二酮产品。通过单因素实验考察不同溶剂、不同配比、不同温度等因素对分离影响。研究结果显示:以乙酸乙酯为溶剂,按料液比(1:3)萃取温度50℃、萃取两次、结晶温度为0℃、结晶时间为6 h、结晶二次得到甾醇提取率为46%,纯度达到80%以上;按料液比1:3加入甲醇溶解浓缩物,浓缩到体积的一半后,冷却结晶18 h,经离心得到雄烯二酮粗品。上清液再次浓缩,回收溶剂和副产品大豆油。该研究结果实现了雄烯二酮发酵废液的变废为宝及资源化综合利用。
In this paper, androstenedione fermentation waste liquid was employed as a raw material. Organic solvent extraction and recrystallization were carried out on this research. Sterols and androstenedione products has have been gained. Single factor experiment was used to invest the effect of different solvents, different proportions and different temperature on the separation. The results showed that: ethyl acetate as the solvent, according to the solid-liquid ratio(1:3) extraction temperature 50 ℃, with extraction twice, the crystallization temperature is 0 ℃, crystallization time 6 h, and crystallized twice to obtain sterol extraction rate of 46% purity more than 80%; by solid-liquid ratio of 1 : 3 methanol was added to dissolve the concentrate, concentrated to half volume followed by cooling crystallization 18 h, centrifuged and the precipitate obtained androstenedione crude products. The solvent was obtained again with byproduct soybean oil by concentrating the supernatant. The results of this study have realized the comprehensive utilization of the waste liquor of androstenedione fermentation.
In this paper, androstenedione fermentation waste liquid was employed as a raw material. Organic solvent extraction and recrystallization were carried out on this research. Sterols and androstenedione products has have been gained. Single factor experiment was used to invest the effect of different solvents, different proportions and different temperature on the separation. The results showed that: ethyl acetate as the solvent, according to the solid-liquid ratio(1:3) extraction temperature 50 ℃, with extraction twice, the crystallization temperature is 0 ℃, crystallization time 6 h, and crystallized twice to obtain sterol extraction rate of 46% purity more than 80%; by solid-liquid ratio of 1 : 3 methanol was added to dissolve the concentrate, concentrated to half volume followed by cooling crystallization 18 h, centrifuged and the precipitate obtained androstenedione crude products. The solvent was obtained again with byproduct soybean oil by concentrating the supernatant. The results of this study have realized the comprehensive utilization of the waste liquor of androstenedione fermentation.
引文
[1]林彦良.甾体化合物微生物转化的研究[D].济南:山东大学,2009, 18-24.LIN Yanliang. Microbial transformation of phytosterol[D].Jinan:Shandong University, 2009, 18-24
[2]姜绍通,赵俊平,杨英,等.两相系统发酵转化植物甾醇为雄烯二酮的研究[J].食品与发酵工业,2008, 34(6):46-48JIANG Shaotong, ZHAO Junping, Yang Ying, et al. Study on transformation of phytosterol into androst-4-ene-3,17-dione in two-phase systems[J]. Food and Fermentation Industries. 2008, 34(6):46-48
[3]汤海峰,易杨华,姚新生.海洋甾体化合物的研究进展[J].中国海洋药物,2002, 22(2):42-43TANG Haifeng,YI Yanghua,YAO Xinsheng. Progress in the study of marine steroids[J]. Chinese Journal of Marine Drugs, 2002, 22(2):42-43
[4]万建春.大豆脱臭馏出物中生育酚及甾醇单体的分离纯化[D].武汉:武汉工业学院,2008:9-17WAN Jianchun. Separation and purification of tocopherol and sterol monomers from soybean deodorant distillate[D]. Wuhan:Wuhan University of Technology, 2008:9-17
[5]李晓丽.大豆油脚提取甾醇及废水处理方法优化研究[D].长春:吉林农业大学,2005:1-8LI Xiaoli. Optimization of sterol extraction from soybean oil and wastewater treatment methods[D]. Changchun:Jilin Agricultural University, 2005:1-8
[6]李奇.大豆油脱臭馏出物中生育酚、甾醇和脂肪酸的提取工艺研究[D].天津:天津大学,2008:2-27LI Qi. Study on extraction technology of tocopherol sterol and fatty acid from deodorant distillate of soybean oil[D]. Tianjin:Tianjin University, 2008:2-27
[7]傅小峰.络合法提取植物甾醇的工艺研究及甾醇的溶解度测定[D].杭州:浙江大学,2004:17-25FU Xiaofeng. Study on the extraction process of phytosterol by complexation method and determination of its solubility[D]. Hangzhou:Zhejiang University, 2004:17-25
[8]HIROTA Y, NAGAO T, WATANABE Y, et al. Purification of steryl esters from soybean oil deodorizer distillate[J].Journal of the American Oil C.hemists Society, 2003, 80(4):341-346
[9]SHIMADA Y, NAKAI S, SUENAGA M, et al. Facile purification of tocopherols from soybean oil deodorizer distillate in high yield using lipase[J]. Journal of the American Oil C.hemists Society, 2000, 77(10):1009-1013
[10]孙德智,段晓东,徐衍岭,等.乳化液膜的润湿聚结破乳研究[J].哈尔滨工业大学学报,1996, 28(4):68-71SUN Dezhi, DU AN Xiaodong, XU Yanling, et al. A study of wetting coalescence demulsificafion of liquid emulsion membrane[J]. Journal of Harbin institute of technology,1996, 28(4):68-71
[11]管军军,裘爱泳,周瑞宝.糖对大豆分离蛋白及其改性物乳化性的影响[J].无锡轻工大学学报,2004, 23(1):84-89GUAN Jun, QIU Aiyong, ZHOU Ruibao. Effects of saccharides on the emulsifying characteristics of soybean protein and its modified products[J]. Journal of Wuxi University of Light Industry, 2004, 23(1):84-89
[12]黎金旭,陈小明,孟庆雄,王洪钟.酶法生产脂肪酸甲酯并提取植物甾醇[J].粮油加工,2007(5):73-75LI Jinxu, CHEN Xiaoming, MENG Qingxiong, et al. Enzymatic production of fatty acid methyl ester and extraction of phytosterol[J]. Grain and Oil Processing, 2007(5):73-75.
[2]姜绍通,赵俊平,杨英,等.两相系统发酵转化植物甾醇为雄烯二酮的研究[J].食品与发酵工业,2008, 34(6):46-48JIANG Shaotong, ZHAO Junping, Yang Ying, et al. Study on transformation of phytosterol into androst-4-ene-3,17-dione in two-phase systems[J]. Food and Fermentation Industries. 2008, 34(6):46-48
[3]汤海峰,易杨华,姚新生.海洋甾体化合物的研究进展[J].中国海洋药物,2002, 22(2):42-43TANG Haifeng,YI Yanghua,YAO Xinsheng. Progress in the study of marine steroids[J]. Chinese Journal of Marine Drugs, 2002, 22(2):42-43
[4]万建春.大豆脱臭馏出物中生育酚及甾醇单体的分离纯化[D].武汉:武汉工业学院,2008:9-17WAN Jianchun. Separation and purification of tocopherol and sterol monomers from soybean deodorant distillate[D]. Wuhan:Wuhan University of Technology, 2008:9-17
[5]李晓丽.大豆油脚提取甾醇及废水处理方法优化研究[D].长春:吉林农业大学,2005:1-8LI Xiaoli. Optimization of sterol extraction from soybean oil and wastewater treatment methods[D]. Changchun:Jilin Agricultural University, 2005:1-8
[6]李奇.大豆油脱臭馏出物中生育酚、甾醇和脂肪酸的提取工艺研究[D].天津:天津大学,2008:2-27LI Qi. Study on extraction technology of tocopherol sterol and fatty acid from deodorant distillate of soybean oil[D]. Tianjin:Tianjin University, 2008:2-27
[7]傅小峰.络合法提取植物甾醇的工艺研究及甾醇的溶解度测定[D].杭州:浙江大学,2004:17-25FU Xiaofeng. Study on the extraction process of phytosterol by complexation method and determination of its solubility[D]. Hangzhou:Zhejiang University, 2004:17-25
[8]HIROTA Y, NAGAO T, WATANABE Y, et al. Purification of steryl esters from soybean oil deodorizer distillate[J].Journal of the American Oil C.hemists Society, 2003, 80(4):341-346
[9]SHIMADA Y, NAKAI S, SUENAGA M, et al. Facile purification of tocopherols from soybean oil deodorizer distillate in high yield using lipase[J]. Journal of the American Oil C.hemists Society, 2000, 77(10):1009-1013
[10]孙德智,段晓东,徐衍岭,等.乳化液膜的润湿聚结破乳研究[J].哈尔滨工业大学学报,1996, 28(4):68-71SUN Dezhi, DU AN Xiaodong, XU Yanling, et al. A study of wetting coalescence demulsificafion of liquid emulsion membrane[J]. Journal of Harbin institute of technology,1996, 28(4):68-71
[11]管军军,裘爱泳,周瑞宝.糖对大豆分离蛋白及其改性物乳化性的影响[J].无锡轻工大学学报,2004, 23(1):84-89GUAN Jun, QIU Aiyong, ZHOU Ruibao. Effects of saccharides on the emulsifying characteristics of soybean protein and its modified products[J]. Journal of Wuxi University of Light Industry, 2004, 23(1):84-89
[12]黎金旭,陈小明,孟庆雄,王洪钟.酶法生产脂肪酸甲酯并提取植物甾醇[J].粮油加工,2007(5):73-75LI Jinxu, CHEN Xiaoming, MENG Qingxiong, et al. Enzymatic production of fatty acid methyl ester and extraction of phytosterol[J]. Grain and Oil Processing, 2007(5):73-75.