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为更好地将离子交换树脂应用于大豆异黄酮的分离纯化,研究了乙醇含量、pH、温度、初始浓度等条件对D301阴离子交换树脂吸附分离大豆异黄酮的影响。静态吸附实验结果表明,该树脂在以水为溶剂、pH 8左右、40℃时对大豆异黄酮有最好的吸附效果。穿透曲线实验表明,动态饱和吸附量受温度影响较大,当柱温为50℃、初始浓度C07.03 mg/mL时,饱和吸附量为105.0 mg/g干树脂。洗脱曲线实验表明,采用体积分数75%乙醇洗脱,异黄酮回收率为89.3%,产品中大豆异黄酮含量高达56.0%,含量比原料提高了十几倍。表明D301阴离子交换树脂对大豆异黄酮的分离纯化具有较好的选择性和应用前景。 相似文献
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硅胶柱层析法提纯大豆磷脂酰胆碱的研究 总被引:2,自引:0,他引:2
探讨了以大豆浓缩磷脂为原料,应用柱层析法提纯大豆磷脂酰胆碱(PC)的工艺过程.用TLC法考察了水、异丙醇与正己烷的体积配比,确定流动相适宜配比为正己烷:异丙醇:水(1:1:0.175,v/v/v).通过对固定相、流动相和上载量的考察,得到了柱层析最佳工艺条件:在空塔流速为0.382 cm·min-1,进样浓度为0.25 g浓缩磷脂·(mL流动相)-1的室温条件下,固定相选用100~200目粗孔2号硅胶,流动相为正己烷:异丙醇:水(1:1:0.16,v/v/v),最适上载量为0.086gPC·(g硅胶)-1.经高效液相色谱法定量分析,产品中磷脂酰胆碱纯度高达85%. 相似文献
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超临界流体色谱法制备高纯度EPA-EE和DHA-EE 总被引:6,自引:2,他引:4
以二氧化碳作流动相,分别以极性相反的C18柱和硅胶柱为固定相,用超临界流体色谱法分离二十碳五烯酸乙酯(EPA-EE)和二十二碳六烯酸乙酯(DHA-EE)。比较C18柱和硅胶柱分离EPA-EE和DHA-EE的机理和分离效果,提出结合C18柱和硅胶柱的超临界流体色谱制备高纯度EPA-EE和DHA-EE的方法。 相似文献
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棕榈油中生育酚和生育三烯酚的HPLC测定 总被引:3,自引:0,他引:3
建立了棕榈油中生育酚和生育三烯酚的准确、快速的HPLC分析方法。选用Nucleosil硅胶柱正相分离,以正己烷-异丙醇为流动相,梯度洗脱,在紫外波长292nm下进行检测,获得较理想的分离效果。该方法线性范围为0.2275~1.3031mg/mL,平均加样回收率为100.17%,RSD=0.5905%。 相似文献
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Since α-tocopherol has special biological and nutritional activities, it is important to convert non-α-tocopherols to α-tocopherol. This paper focuses on the effects of residence time, pressure, temperature and the mass ratio of formaldehyde to tocopherols on the content of α-tocopherol, the conversion of non-α-tocopherols,the selectivity and yield of α-tocopherol in a fixed-bed reactor. The reactor is made from 12 (I.D.)×360mm stainless steel pipe. It is packed with a mixture of 5% Pd/C and cation exchange resin catalysts. Preliminary results indicated the suitable operation conditions are pressure 5.0 MPa, temperature 180°C, and mass ratio of formaldehyde to tocopherols 2.0. A product of more than 50% α-tocopherol content has been obtained by using88.85% mixed tocopherols as raw material. 相似文献
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2-(4-卤代苯甲酰基)苯胺的合成研究 总被引:2,自引:0,他引:2
研究了重要的有机中间体2-(4-卤代苯甲酰基)苯胺的通用合成路线,是以邻苯二甲酸酐为原料,与卤代苯(分别为氟苯、氯苯和溴苯)进行付-克反应得到羧酸;羧酸经酰氯化、酰胺化,制得邻苯甲酰基苯甲酰胺衍生物,然后再经过霍夫曼降解合成了标题化合物。对主要步骤反应条件进行了优化,得出比较合理的条件为:付-克反应,催化剂:AlCl3,配料比:1:2.2:6.4(苯酐:AlCl3:卤代苯);同时使用卤代苯既作反应试剂,又作溶剂,未反应的卤代苯回收套用,使收率基本定量;酰胺化反应氨气流量:10mLmin-1,使反应得以室温进行,无需制冷;四步反应总收率可达70%。 相似文献
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Since a-tocopherol has special biological and nutritional activities, it is important to convert non-a-tocopherols to a-tocopherol. This paper focuses on the effects of residence time, pressure, temperature and the mass ratio of formaldehyde to tocopherols on the content of a-tocopherol, the conversion of non-a-tocopherols, the selectivity and yield of a-tocopherol in a fixed-bed reactor. The reactor is made from φ12 (I.D.)×360mm stainless steel pipe. It is packed with a mixture of 5% Pd/C and cation exchange resin catalysts. Preliminary results indicated the suitable operation conditions are pressure 5.0 MPa, temperature 180℃, and mass ratio of formaldehyde to tocopherols 2.0. A product of more than 50% a-tocopherol content has been obtained by using 88.85% mixed tocopherols as raw material. 相似文献