CN103059008A - 一种同时制备高纯度葛根素和大豆苷元的方法 - Google Patents
一种同时制备高纯度葛根素和大豆苷元的方法 Download PDFInfo
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Abstract
一种同时制备高纯度葛根素和大豆苷元的方法,将粉碎的葛根与乙醇按料液比是1:6~1:10混合提取,将所得混合物过滤,滤液减压浓缩至干,得到葛根提取物浸膏,将葛根提取物浸膏用适当浓度的乙醇溶液复溶后,加入盐酸溶液和氯仿回流水解萃取一定时间,静置冷却,分出氯仿,减压浓缩,浓缩物采用乙醇溶液重结晶,得到大豆苷元结晶,酸水解液加水稀释,放置48-72h可析出葛根素粗晶,将其用乙酸-甲醇重结晶,得葛根素产品。本发明同时提取分离葛根中葛根素和大豆苷元,提高了葛根自身的利用价值,充分利用了中药材资源。水解和萃取同时完成,节省操作工序和溶剂的使用量,生产成本低,得率高。
Description
技术领域
本发明属于天然产物化学领域,特别涉及一种同时制备高纯度葛根素和大豆苷元的方法。
背景技术
葛,Pueraria lobata (willd.) Ohwi,为豆科类多年生落叶藤本植物。自然分布于温带和亚热带地区,全世界葛属品种有20余种,我国有11个葛属品种,常见的品种有野葛和粉葛(甘葛)两种。
葛的藤、叶、花、种子及块根等,均可入药。其中根和花的利用价值最高。葛的块根,即“葛根”。其中含有大量的淀粉和生物活性成分—异黄酮类化合物;此外,还富含蛋白质及人体必需的矿物质和微量元素钙、铁、锌、硒、钾等。
葛根在《神农本草经》、《本草纲目》、《中国药典》、《中药大词典》等古今医药大典中均有专述,记载其主要功能为:清热、止呕、清脾、解诸毒、开胃下食、治高血压、心绞痛、耳聋等。最新医学研究表明,葛根可改善心脑血管循环,调节血压,具有排毒、养颜、美容、丰胸等功能。国家卫生部已将葛根列入药食两用品种。
葛根的主要化学成分有:异黄酮类化合物,其中有大豆苷元、大豆苷、葛根素;还含有葛根苷类化合物,其中有葛根苷A、葛根苷B、葛根苷C,这些物质被认为是二氢查尔酮的衍生物;葛根中还含有三萜皂醇B、大豆苷醇A、大豆苷醇B、大豆苷醇C;还含有氯化胆碱、甘露醇、胡萝卜苷、胆碱和乙酰胆碱、甾醇等。
1959年日本人柴田承二对葛根化学成分的研究表明,异黄酮类化合物是葛根的主要有效成分,其中含量较多的有葛根素、大豆苷和大豆苷元。在国内,1974年方起程等成功地提取了葛根素,1993年葛根素被卫生部批准用于临床。目前葛根素在临床上已被广泛应用于心脑血管系统疾病(如心绞痛、心肌梗死、心律失常、冠心病、心力衰竭、椎-基底动脉供血不足、高黏血症、高血压、脑血栓、脑水肿等)、糖尿病、眼底疾病(如视网膜动脉栓塞、单纯性青光眼)、突发性耳聋、急性酒精中毒、拟菊酯类农药中毒及肿瘤的治疗。另外,与单用法莫替丁、羟氨苄青霉素及氧氟沙星相比,将葛根素与这3种药联用治疗十二指肠溃疡,溃疡愈合率有显著提高。1972年由我国药物工作者合成大豆苷元,已被广泛用于药品、食品补充剂和化妆品等。现代药理学研究表明,大豆苷元具有抗肿瘤、心脑血管保护、雌激素和抗雌激素样作用、抗骨质疏松、抗氧化、提高机体免疫力及影响内分泌系统等多种药理作用。因此具有多种药用活性的葛根素和大豆苷元的提取、纯化也越来越引起人们的关注。
美国专利(USP 7384657)从葛根粉末中提取出了葛根素,主要工艺流程为甲醇提取3次、过滤、浓缩、从葛根总黄酮中分离得到葛根素产品,但此方法存在溶剂消耗量大、成本高等缺点。
公开号为CN1415609A的中国专利介绍了一种葛根素的提取方法,该方法采用醇溶媒提取的方法在醇溶媒提取过程中,实施超声波穿透处理,将醇溶媒提取后的过滤提取液蒸馏回收醇溶媒,再进行层析分离,将点样后收集的洗脱液进行浓缩,再经过净化处理得葛根素产品。该技术工艺繁琐,难以形成工业化规模。
公开号为CN1163127A的专利介绍了一种葛根素及其提取方法,其提取工艺流程为:原料葛根清杂粉碎→水煎煮→水浸膏→乙醇沉淀→醇浸膏→聚酰胺柱层析→水洗脱→浓缩→放置析晶→粗品→精制→干燥→葛根素精品,此法葛根素精品含量达97-100%,收率达1%以上。该技术收率低,工艺繁琐,难以形成工业化规模。
公开号为CN1129700A的专利介绍了一种葛根素及其提取方法,其提取方法为水提醇沉后,经聚酰胺柱层析,以水洗脱、浓缩、放置析出葛根素粗品,粗品再次经聚酰胺柱层析、水洗脱、浓缩析出结晶,再经冷冻干燥或喷雾干燥或用70%-80%醇重复结晶制得精品,此法所得葛根素含量在90%以上。该技术得到的葛根素产品纯度较低。
公开号为CN1927876A的专利介绍了一种葛根素提取物的生产方法,其工艺步骤:将葛属的根部原材料粉碎后煎煮,进行离子交换型大孔树脂层析,再经过大孔树脂层析,先以2-4倍主题及的水洗,再以5-7倍柱体积的20%乙醇洗脱,收集20%乙醇洗脱液,回收乙醇得葛根素提取物,此法所得葛根素含量可达到近80%、收率约2.5%,大豆苷元收率约1%。该技术工艺繁琐,难以形成工业化规模。
公开号为CN1365976A的专利介绍了一种葛根药用成分提取工艺,其采用微波萃取技术进行提取,用弱极性大孔树脂进行总黄酮富集,采用不同浓度的乙醇溶液进行洗脱,葛根素得率为1.21%。该技术能耗高,难以形成工业化规模。
公开号为CN1629174A的专利介绍了一种制备葛根素的方法,其采用水为溶媒提取葛根素,提取液过滤后直接上层析柱分离,洗脱液采用膜分离技术进行浓缩,再经过结晶,精致得到葛根素纯品。该技术采用膜分离的方法,难以形成工业化规模。
公开号为CN1696142A的专利介绍了一种高纯度葛根素及大豆苷元联合生产的方法,该方法以葛根为原料,加入乙醇水溶液,在加热条件下回流提取,提取后进行离心分离除渣,提取液浓缩成浸膏,用酸酸解,再用乙酸乙酯萃取其中有效成分;接着浓缩萃取液,静置使之结晶,抽滤滤去酸液,再用纯净水或乙醇进行重结晶,干燥即得高纯度大豆苷元;将萃取后的酸液浓缩,静置结晶,抽滤滤去母液,再用纯净水或乙醇进行重结晶,干燥即得高纯度葛根素。该技术将水解和萃取分步进行,操作繁琐,费时,因此工业利用效果欠佳。
综上所述,现有提取葛根有效成分的方法中,大多只提取葛根素一种有效成分,而没有同时提取分离出大豆苷元,降低了葛根自身的利用的价值,造成中药材资源的浪费。目前一般是采用酸水解-有机溶剂萃取法转化和分离葛根素和大豆苷元,即直接将葛根提取物加酸水解其中所含的结合态葛根素和大豆苷元,然后用有机溶剂提取。该工艺操作繁琐,多次萃取,收率低。所以本发明考虑了以上情况开发了水解同时萃取从葛根中制备葛根素和大豆苷元的方法。同时提取分离两种有效成分,提高了葛根自身的利用价值,充分利用了中药材资源。
发明内容
本发明的目的在于提供一种同时制备高纯度葛根素和大豆苷元的方法。
为了达到上述目的,本发明采用的技术方案为:一种同时制备高纯度葛根素和大豆苷元的方法,其特征在于包括如下步骤:
1)、将葛根粉与乙醇溶液混合,加热提取2~4小时,重复提取1~3次,过滤,滤液减压浓缩至干,得葛根提取物浸膏;
2)、将步骤1)得到的葛根提取物浸膏用乙醇溶液复溶,加入盐酸溶液和氯仿,进行回流水解萃取,静置冷却,分出氯仿层和酸水解液层;
3)、将氯仿层减压浓缩,浓缩物采用乙醇溶液重结晶,得到大豆苷元结晶;
4)、将酸水解液加水稀释,放置48~72h析出葛根素粗晶,然后用乙酸-甲醇溶液重结晶,得葛根素。
步骤1)中乙醇溶液的体积分数为55%~85%,葛根粉与乙醇溶液的料液比是1:6~1:10,即1g葛根粉(绝干)与6~10mL乙醇溶液混合,提取温度为70~90℃。
步骤2)中乙醇溶液的体积分数为35~75%,提取物浸膏与乙醇溶液的固液比为1:20~1:40,即1g提取物浸膏溶于20~40mL乙醇溶液中。
步骤2)中盐酸溶液浓度为3%~8%,提取物浸膏和盐酸溶液的固液比为1:3~1:10,即1g提取物浸膏溶于3~10mL盐酸溶液中,氯仿的用量为盐酸溶液用量的1.5~2.5倍(体积倍数)。
步骤2)中水解萃取温度为60~90℃,时间1~8小时。
步骤3)中乙醇溶液的体积分数为40%~60%,重结晶次数为1~3次。
步骤4)中酸水解液加水稀释0.5~1.5倍,所述乙酸-甲醇溶液的体积比为3:7~7:3,重结晶次数为1~3次。
有益效果:
1、同时提取分离葛根中葛根素和大豆苷元,提高了葛根自身的利用价值,充分利用了中药材资源。
2、水解和萃取同时完成,节省操作工序和溶剂的使用量,生产成本低,得率高。
具体实施方式
下面结合实施例对本发明作进行进一步的说明,但是它并不限于这些实施例的任一个或类似实例。
实施例1
将500g(绝干)粉碎后的葛根用85%的乙醇溶液5000ml(葛根与乙醇溶液的料液比是1:10),于90℃回流提取4小时,重复提取3次,过滤,滤液减压浓缩至干,得葛根提取物浸膏78g,向葛根提取物浸膏中加入75%的乙醇溶液1560ml使其复溶,加入8%的盐酸水溶液780ml,再加入氯仿1950ml,回流水解萃取8小时,温度为90℃。静置冷却分出氯仿相,减压浓缩,浓缩物用50%乙醇重结晶3次,得大豆苷元结晶;酸水解液加水稀释1.5倍,放置72h析出葛根素粗晶,将其用乙酸-甲醇(1:1)重结晶3次,得葛根素产品。葛根素收率为1.12%,纯度为98.6%;大豆苷元收率为0.49%,纯度为95.8%。
实施例2
将500g(绝干)粉碎后的葛根用55%的乙醇溶液3000ml(葛根与乙醇溶液的料液比是1:6),于70℃回流提取2小时,重复提取1次,过滤,滤液减压浓缩至干,得葛根提取物浸膏37.8g,向葛根提取物浸膏中加入35%的乙醇溶液1520ml使其复溶,加入3%的盐酸水溶液114ml,再加入氯仿171ml,回流水解萃取1小时,温度为60℃。静置冷却分出氯仿相,减压浓缩,浓缩物用60%乙醇重结晶1次,得大豆苷元结晶;酸水解液加水稀释0.5倍,放置48h析出葛根素粗晶,将其用乙酸-甲醇(3:7)重结晶1次,得葛根素产品。葛根素收率为1.00%,纯度为96.4%;大豆苷元收率为0.42%,纯度为94.3%。
实施例3
将500g(绝干)粉碎后的葛根用75%的乙醇溶液4000ml(葛根与乙醇溶液的料液比是1:8),于80℃回流提取3小时,重复提取2次,过滤,滤液减压浓缩至干,得葛根提取物浸膏58.6g,向葛根提取物浸膏中加入60%的乙醇溶液1180ml使其复溶,加入6%的盐酸水溶液295ml,再加入氯仿590ml,回流水解萃取4小时,温度为80℃。静置冷却分出氯仿相,减压浓缩,浓缩物用40%乙醇重结晶3次,得大豆苷元结晶;酸水解液加水稀释1倍,放置72h析出葛根素粗晶,将其用乙酸-甲醇(7:3)重结晶2次,得葛根素产品。葛根素收率为1.07%,纯度为98.1%;大豆苷元收率为0.46%,纯度为95.2%。
Claims (7)
1.一种同时制备高纯度葛根素和大豆苷元的方法,其特征在于包括如下步骤:
1)、将葛根粉与乙醇溶液混合,加热提取2~4小时,重复提取1~3次,过滤,滤液减压浓缩至干,得葛根提取物浸膏;
2)、将步骤1)得到的葛根提取物浸膏用乙醇溶液复溶,加入盐酸溶液和氯仿,进行回流水解萃取,静置冷却,分出氯仿层和酸水解液层;
3)、将氯仿层减压浓缩,浓缩物采用乙醇溶液重结晶,得到大豆苷元结晶;
4)、将酸水解液加水稀释,放置48~72h析出葛根素粗晶,然后用乙酸-甲醇溶液重结晶,得葛根素。
2.根据权利要求1所述的同时制备高纯度葛根素和大豆苷元的方法,其特征在于:步骤1)中乙醇溶液的体积分数为55%~85%,1g葛根粉与6~10mL乙醇溶液混合,提取温度为70~90℃。
3.根据权利要求1所述的同时制备高纯度葛根素和大豆苷元的方法,其特征在于:步骤2)中乙醇溶液的体积分数为35~75%,1g葛根提取物浸膏溶于20~40mL乙醇溶液中。
4.根据权利要求1所述的同时制备高纯度葛根素和大豆苷元的方法,其特征在于:步骤2)中盐酸溶液质量浓度为3%~8%,1g葛根提取物浸膏加入盐酸溶液3~10mL,氯仿的用量为盐酸溶液体积的1.5~2.5倍。
5.根据权利要求1所述的同时制备高纯度葛根素和大豆苷元的方法,其特征在于:步骤2)中水解萃取温度为60~90℃,时间1~8小时。
6.根据权利要求1所述的同时制备高纯度葛根素和大豆苷元的方法,其特征在于:步骤3)中乙醇溶液的体积分数为40%~60%,重结晶次数为1~3次。
7.根据权利要求1所述的同时制备高纯度葛根素和大豆苷元的方法,其特征在于:步骤4)中酸水解液加水稀释0.5~1.5倍,所述乙酸-甲醇溶液的体积比为3:7~7:3,重结晶次数为1~3次。
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