CN107353282A - 从葛根中萃取高纯度葛根素及多种珍稀医药成分的工艺 - Google Patents

从葛根中萃取高纯度葛根素及多种珍稀医药成分的工艺 Download PDF

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CN107353282A
CN107353282A CN201710504780.7A CN201710504780A CN107353282A CN 107353282 A CN107353282 A CN 107353282A CN 201710504780 A CN201710504780 A CN 201710504780A CN 107353282 A CN107353282 A CN 107353282A
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卓宇哲
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Abstract

本发明属于中药提取技术领域，具体地说是从野葛根中萃取高纯度葛根素及多种珍稀医药成分的工艺，包括酒精超声波浸提、药液回收、蒸发浓缩成膏状、对浸膏溶解萃取、以及分别采取三步萃取分离有效组分大豆苷元、尿囊素、葛根素。本发明对葛根中大部分有效成分都分离提纯加以利用，大大提高了葛根的综合利用价值。特别值得一提的是，本发明从葛根素中分离了不可利用的剧毒成分3＇氰基葛根素，其收率3.22％(含量98.1％)，同时还提供了葛根复方制剂。

Description

从葛根中萃取高纯度葛根素及多种珍稀医药成分的工艺
技术领域
本发明属于中药有效成分生物提取技术领域，具体的说涉及从野葛根中提取有效成分葛根素技术。
技术背景
葛根素是近十年来年世界各国广泛研究和发展的专供医药工业用于攻克心脑血管、各种癌症、眼科杂顽症的生物原料药。该产品具有所有化学药品不可替代的多种优点：1、生物药理有效成份多样化，主要成份具有防止血管通透性异常升高。迅速抑制病灶细胞和血小板凝集，增加血中氧含量和氧饱和度，改善微循环和促进血管生成使裂壁得到修复等作用。对闭塞性心脑血管病，中心性视网膜炎、动脉硬化、冠心病、梗塞前综合症、血栓性静脉炎等可以达到多重效果。2、对动物性神经行为很安全。葛根素针剂、片剂作用方式主要是通络、活血化瘀、降低梗塞动物的血浆内皮素含量，提高血清SOD含量，增强肌体的免疫功能，无负作用。3、肌体不易产生抗药性。中草药往往含有数种成份，且作用机理与一般化学药品截然不同。如：日本从黄豆中提取葛根素针剂治疗心脑血管病，经过数年的临床实践，康复率达98％以上，同时，未发现任何不良反应及副作用。4、对环境安全，没有毒废物残留。中草药制剂含有的化学成份是自然畀中具有的天然生理结构，在自然生态中必然存在降解它的物质基因。因此，在生产过程中无任何累废积物链和残毒之虑。
日本从黄豆中提取葛根素系列产品，但成本较高，主要因素是原料较贵。国内报道的葛根素提取工艺较复杂，手段落后，收率较低，并对副产品无利用，经过实践证明不成功。
本申请人在先申请(专利200910022619.1)虽然克服了现有葛根有效成分提取中一些问题，但是对于葛根中有些成分提取不够充分。由于葛根中提取的葛根黄酮类化合物具有抗氧化、抗肿瘤、防治心脑血管病等药理作用，近几年对葛根医药利用更得到重视，因此，葛根黄酮的分离成为最为紧迫的需要。
另外，葛根制剂在肠道吸收和透皮制剂中存在吸收率太低，药效难以发挥的缺陷。
发明内容
本发明目的是提供一种从葛根中萃取高纯度葛根素及多种珍稀医药成分的工艺，以提高葛根的综合利用价值。
从葛根中萃取高纯度葛根素及多种珍稀医药成分的工艺，其特征是按照以下步骤实施：
(1)葛根黄酮提取：称取野葛根加适量水润透，加80％乙醇超声提取2次，乙醇质量分数不低于60.0％、提取时间不低于138.0min、液固比至少11.3mL/g、提取温度70.0℃以下，过滤，合并滤液，70'C以下减压干燥，得黄褐色粉末；
(2)葛根素和大豆苷元分离：将黄色粉末加入适量湖景成水提取液，将提取液流过H103大孔树脂床，进行吸附操作；用4倍柱床体积水清洗树脂床，然后用4倍柱床体积的75％乙醇进行洗脱操作，收集洗脱液，浓缩回收乙醇；往浓缩液中加HCl至HCl浓度为2mRl/L，并在90℃水浴条件下酸解60min；酸解液趁热过滤，往滤液中加5倍体积水稀释后流过H103大孔树脂床，进行吸附操作；用4倍柱床体积水清洗树脂床，然后用4倍柱床体积的50％乙醇进行洗脱操作，收集洗脱液，并浓缩回收乙醇；浓缩液在4℃条件下贮存24h，收集沉淀得到葛根素；用4倍柱床体积的95％乙醇对树脂柱进行洗脱操作，收集洗脱液，并浓缩回收乙醇；往浓缩液中加入等体积的水，在4℃条件下贮存24h，收集沉淀得到大豆苷元；
(3)染料木素分离：a)以染料木素分子印迹聚合物微粒为填料制成固相萃取柱；b)对步骤a制备的固相萃取柱进行活化、上样，然后依次用体积比49-51％水的步骤(2)提取液加入乙腈的溶液、体积比4.9-5.1％水的乙腈溶液对萃取柱进行淋洗，最后用体积比0.18-0.22％TEA的甲醇溶液洗脱；洗脱液蒸干得染料木素。
步骤(1)所得葛根黄酮与黄芩、黄连、甘草四味药物按10-12∶1-2∶1-2∶0.5-1的重量比混合,提取物加入辅料,用于制备治疗腹泻的口服制剂。
步骤(2)中葛根素与牛磺酸制成复方口服制剂用于降低血糖，并且加入占总组分0.5-1％的壳聚糖做肠道吸收促进剂。
步骤(2)中葛根素与与银杏叶提取物配伍用于制备抗衰老外用制剂，并且加入肉桂油和丁香油做作为透皮吸收促进剂。
步骤(1)所得粉末混入山药、茯苓、淡竹叶、薏苡仁、桑椹、百合中的一种或多种后与山药、枸杞、麦冬草、牛蒡子组合制成降血糖和血脂的的保健食品。
本发明采用野葛根提取葛根素，将危害和严重影响林木健康生长的野葛藤蔓变害为宝，工艺中的浸取温度合理，使得葛根素收率较高，生产安全，对设备要求较低，同时尾气得到回收，废碴被制成复合饲料，降低了综合成本。同时，本发明对葛根中大部分有效成分都分离提纯加以利用，大大提高了葛根的综合利用价值。特别值得一提的是，
本发明从葛根素中分离了不可利用的剧毒成分3＇氰基葛根素，但该成分在国防建设中却起着工业味精的作用，其收率3.22％(含量98.1％)，本发明提取了葛根素,大豆苷元,大豆苷,染料木素,β-胡萝卜苷和芒柄花苷等现有工艺无法分离的成分，大大提高了葛根药用价值的发挥。
本发明工艺可以提取的葛根中有效成分包括：
大豆苷元组分中：①、大豆苷元收率0.58％(含量98.g％)；②、大豆苷收率0.49％(含量99.2％)；③、染料木苷收率0.46％(含量99.5％)；④、葡萄糖大豆苷收率0.25％(含量99.8g％)
尿囊素组分：①、尿囊素牧率0.62％(含量98.87％)；②、胡萝卜素收率0.53％(含量99.8％)；③、染料木素收率0.47％(含量95.5g％)；④、8.碳一芹糖收率0.42％(含量93.3％)；⑤、谷甾醇收率0.288％(含量97.9％)。
葛根素组分：①、葛根素收率6.8％(含量99.8％)；②、3 7-氰基葛根素收率3.22％(含量98.1％)；③、芒柄素收率2.56％(含量98.89％)；④、大豆素收率2.5％(含量98％)。
特别是本发明提供的葛根复方制剂采用了肠道促进吸收剂和透皮吸收促进剂，有助于大大提高吸收率并提高功效。
具体实施方式
(1)葛根黄酮提取：称取野葛根加适量水润透，加80％乙醇超声提取2次，乙醇质量分数不低于60.0％、提取时间不低于138.0min、液固比至少11.3mL/g、提取温度70.0℃以上，过滤，合并滤液，70'C以下减压千燥，得黄褐色粉末；
(2)葛根素和大豆苷元分离：将黄色粉末加入适量湖景成水提取液，将提取液流过H103大孔树脂床，进行吸附操作；用4倍柱床体积水清洗树脂床，然后用4倍柱床体积的75％乙醇进行洗脱操作，收集洗脱液，浓缩回收乙醇；往浓缩液中加HCl至HCl浓度为2mRl/L，并在90℃水浴条件下酸解60min；酸解液趁热过滤，往滤液中加5倍体积水稀释后流过H103大孔树脂床，进行吸附操作；用4倍柱床体积水清洗树脂床，然后用4倍柱床体积的50％乙醇进行洗脱操作，收集洗脱液，并浓缩回收乙醇；浓缩液在4℃条件下贮存24h，收集沉淀得到葛根素；用4倍柱床体积的95％乙醇对树脂柱进行洗脱操作，收集洗脱液，并浓缩回收乙醇；往浓缩液中加入等体积的水，在4℃条件下贮存24h，收集沉淀得到大豆苷元；
(3)染料木素分离：a)以染料木素分子印迹聚合物微粒为填料制成固相萃取柱；b)对步骤a制备的固相萃取柱进行活化、上样，然后依次用体积比49-51％水的步骤(2)提取液加入乙腈的溶液、体积比4.9-5.1％水的乙腈溶液对萃取柱进行淋洗，最后用体积比0.18-0.22％TEA的甲醇溶液洗脱；洗脱液蒸干得染料木素。
步骤(1)所得葛根黄酮与黄芩、黄连、甘草四味药物按10-12∶1-2∶1-2∶0.5-1的重量比混合,提取物加入辅料,用于制备治疗腹泻的口服制剂。
步骤(2)中葛根素与牛磺酸制成复方口服制剂用于降低血糖，并且加入占总组分0.5-1％的壳聚糖做肠道吸收促进剂。
步骤(2)中葛根素与与银杏叶提取物配伍用于制备抗衰老外用制剂，并且加入肉桂油和丁香油做作为透皮吸收促进剂。
步骤(1)所得粉末混入山药、茯苓、淡竹叶、薏苡仁、桑椹、百合中的一种或多种后与山药、枸杞、麦冬草、牛蒡子组合制成降血糖和血脂的的保健食品。

Claims (5)

1.从葛根中萃取高纯度葛根素及多种珍稀医药成分的工艺，其特征是按照以下步骤实施：
(1)葛根黄酮提取：称取野葛根加适量水润透，加80％乙醇超声提取2次，乙醇质量分数不低于60％、提取时间不低于138.0min、液固比至少11.3mL/g、提取温度70℃以下，过滤、合并滤液，70℃以下减压干燥，得黄褐色粉末；
(2)葛根素和大豆苷元分离：将黄色粉末加入适量湖景成水提取液，将提取液流过H103大孔树脂床，进行吸附操作；用4倍柱床体积水清洗树脂床，然后用4倍柱床体积的75％乙醇进行洗脱操作，收集洗脱液，浓缩回收乙醇；往浓缩液中加HCl至HCl浓度为2mRl/L，并在90℃水浴条件下酸解60min；酸解液趁热过滤，往滤液中加5倍体积水稀释后流过H103大孔树脂床，进行吸附操作；用4倍柱床体积水清洗树脂床，然后用4倍柱床体积的50％乙醇进行洗脱操作，收集洗脱液，并浓缩回收乙醇；浓缩液在4℃条件下贮存24h，收集沉淀得到葛根素；用4倍柱床体积的95％乙醇对树脂柱进行洗脱操作，收集洗脱液，并浓缩回收乙醇；往浓缩液中加入等量体积的水，在4℃条件下贮存24h，收集沉淀得到大豆苷元；
(3)染料木素分离：a)以染料木素分子印迹聚合物微粒为填料制成固相萃取柱；b)对步骤a制备的固相萃取柱进行活化、上样，然后依次用体积比49-51％水的步骤(2)提取液加入乙腈的溶液、体积比4.9-5.1％水的乙腈溶液对萃取柱进行淋洗，最后用体积比0.18-0.22％TEA的甲醇溶液洗脱；洗脱液蒸干得染料木素。
2.根据权利要求1所述的工艺，其特征是步骤(1)所得葛根黄酮与黄芩、黄连、甘草四味药物按10-12∶1-2∶1-2∶0.5-1的重量比混合,提取物加入辅料,用于制备治疗腹泻的口服制剂。
3.根据权利要求1所述的工艺，其特征是步骤(2)中葛根素与牛磺酸制成复方口服制剂用于降低血糖，并且加入占总组分0.5-1％的壳聚糖做肠道吸收促进剂。
4.根据权利要求1所述的工艺，其特征是步骤(2)中葛根素与与银杏叶提取物配伍用于制备抗衰老外用制剂，并且加入肉桂油和丁香油做作为透皮吸收促进剂。
5.根据权利要求1所述的工艺，其特征是步骤(1)所得粉末混入山药、茯苓、淡竹叶、薏苡仁、桑椹、百合中的一种或多种后与山药、枸杞、麦冬草、牛蒡子组合制成降血糖和血脂的的保健食品。
CN201710504780.7A 2017-06-28 2017-06-28 从葛根中萃取高纯度葛根素及多种珍稀医药成分的工艺 Pending CN107353282A (zh)

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