The invention discloses a method for purifying sodium taurocholate, in which crude sodium taurocholate is dissolved in alcoholic solvents, ester solvents are added while hot, filtered after cooling, and high purity sodium taurocholate is obtained by vacuum drying. Compared with the prior art, the invention has the following advantages: the refining method is simple in operation, uses ester solvents with relatively higher boiling point, can reduce solvent volatilization, avoids using acetone with irritating odor and low boiling point ether, is safer in operation, and is convenient for industrial production; the method has high yield, good product purity, yield (>91%) and purity of sodium taurocholate after refining. The purity of HPLC was more than 99.00% by ELSD and 100% by area normalization. Among them, the highest purity of HPLC was 99.91%, the content of single impurity A was less than 0.30%, and the content of impurity B was less than 0.8%. The types of impurities were obviously reduced. The final product after refining did not contain impurity C and D.
【技术实现步骤摘要】
一种牛磺胆酸钠的精制方法
本专利技术属于药物化学领域,具体涉及牛磺胆酸钠的一种精制方法。
技术介绍
牛磺胆酸(taurocholicacid,TCA)是牛胆汁中的主要胆汁酸,也是其有效成分之一。它是由胆酸和牛磺酸结合形成的一种结合型胆汁酸。TCA广泛存在于牛、羊、蛇、兔等动物的胆汁中,是重要的有效成分。对其药效学研究表明,该物质具有利胆、镇咳、祛痰、平喘的作用,同时具有杀菌抗炎等作用。对心血管系统亦有影响,可以降血压、降低心脏收缩幅度及频率,有报道称其对癌症也有一定的治疗作用。可见牛磺胆酸是具有开发应用前景的药物。牛磺胆酸的化学名称为3α,7α,12α-三羟基-5β-胆甾烷-24-羧酸-24-牛磺酸酰胺,分子式为C26H45NO7S,分子量为515.6,为淡黄色粉末,无臭味,可溶于水,易溶于氯仿、甲醇、乙醇、异丙醇等有机溶剂中。牛磺胆酸钠的结构如下所示:目前,国内外经过精制后的牛磺胆酸或牛磺胆酸钠盐(胆酸偶联物),收率低,纯度低。已有文献CN101307088B、CN101503454A、CN103755764B公开胆酸偶联物的精制方法。这些精制方法可以分为以下几种:方法一:CN101503454A胆酸偶联物的乙酸乙酯浓缩液用浓盐酸调至pH1~2加入少量晶种,于0~5℃搅拌2h,抽滤,滤饼用少量丙酮洗涤,再用丙酮-水单相体系进行溶解,重结晶得到牛磺胆酸白色粉末,收率仅78.7%。方法二:CN101307088B牛磺胆酸溶解于含有碳酸氢钠的甲醇水溶液,然后加入乙醚,冷却析晶得到牛磺胆酸的钠盐。方法三:CN103755764B胆酸偶联物加入甲醇升温溶解,加入丙 ...
【技术保护点】
1.一种牛磺胆酸钠的精制方法,其特征在于:将牛磺胆酸钠粗品加入醇类溶剂中,升温至40‑60℃,搅拌溶解,然后加入酯类溶剂,降温至0‑40℃析晶,过滤,干燥得到精制的牛磺胆酸钠,其结构如下所示:
【技术特征摘要】
1.一种牛磺胆酸钠的精制方法,其特征在于:将牛磺胆酸钠粗品加入醇类溶剂中,升温至40-60℃,搅拌溶解,然后加入酯类溶剂,降温至0-40℃析晶,过滤,干燥得到精制的牛磺胆酸钠,其结构如下所示:2.根据权利要求1所述的精制方法,其特征在于:所述醇类溶剂包括甲醇、乙醇、丙醇或丁醇;所述酯类溶剂包括乙酸甲酯、乙酸乙酯、乙酸丙酯、乙酸丁酯、丙酸乙酯、丁酸乙脂或戊酸乙酯。3.根据权利要求2所述的精制方法,其特征在于:所述醇类溶剂包括甲醇或乙醇;所述酯类溶剂包括乙酸甲酯或乙酸乙酯。4.根据权利要求1所述的精制方法,其特征在于:所述醇类溶剂与牛磺胆酸钠粗品的体积质量比为2:1~10:1,酯类溶剂与牛磺胆酸钠粗品的体积质量比为2:1~20:1。5.根据权利要求4所述的精制方法,其特征在于:所述醇类溶剂与牛磺胆酸钠粗品的体积质量比为3:1~6:1,酯类溶剂与牛磺胆酸钠粗品的体积质量比为4:1~8:1。6.根据权利要求1所述的精制方法,其特征在于:所述牛磺胆酸钠粗品的溶解温度为50-55℃。7.根据权利要求1所述的精制方法...
【专利技术属性】
技术研发人员:徐奎,刘鹏飞,徐勇刚,陈松,张昊宁,
申请(专利权)人:美药星南京制药有限公司,南京汉欣医药科技有限公司,
类型:发明
国别省市:江苏,32
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