D301阴离子交换树脂对大豆异黄酮分离特性的影响

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。     

硅胶柱层析法提纯大豆磷脂酰胆碱的研究

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%.     

超临界流体色谱法制备高纯度EPA-EE和DHA-EE

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。     

大豆皂苷分离纯化方法研究进展

大豆皂苷(soyusaponins),是从大豆及其它豆类植物种子中提取出来的,由低聚糖及齐墩果烯三萜缩合形成的一类化合物,具有广泛的生理功能.由于其组成复杂、含量低、不稳定,分离纯化难度很大.对大豆皂苷的分离纯化方法进展进行综述.     

超临界CO2从黄花蒿中提取青蒿素的研究

研究了用超临界二氧化碳从黄花蒿中萃取青蒿素的影响因素.在15.2～29.7MPa和40～60℃范围内,萃取压力和萃取温度升高,萃取率增大,萃取选择性下降.以萃取率和萃取选择性为目标,优化了超临界萃取工艺条件,得到较佳的操作条件萃取压力20MPa,萃取温度50℃,CO2流量1kg/(h·kg原料),原料粒径60～80目.在优化条件下萃取4h,萃取率达到95%以上,萃取物纯度10%以上.     

固体酸催化水解糖苷型大豆异黄酮

以固体酸为催化剂,在固定床中将糖苷型大豆异黄酮水解成大豆异黄酮苷元.研究了温度、进料配比以及接触时间对游离型异黄酮转化率的影响.结果表明,溶剂与原料比例为1:11左右为宜,甲醇与水的比例以1:2为好,温度在60～70℃.通过固定床两次水解,糖苷型异黄酮转化率可达90%.     

棕榈油中生育酚和生育三烯酚的HPLC测定

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%。     

固定床反应器中非α-生育酚转型为α-生育酚的研究

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.     

2-(4-卤代苯甲酰基)苯胺的合成研究

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%。     

Conversion of Non-a-Tocopherols to a-Tocopherol in a Fixed Bed Reactor

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.