CN107308337A - 一种去除金线莲提取液中双酯型生物碱的方法 - Google Patents
一种去除金线莲提取液中双酯型生物碱的方法 Download PDFInfo
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- CN107308337A CN107308337A CN201710547586.7A CN201710547586A CN107308337A CN 107308337 A CN107308337 A CN 107308337A CN 201710547586 A CN201710547586 A CN 201710547586A CN 107308337 A CN107308337 A CN 107308337A
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- extract solution
- diester
- terminal bud
- roxburgh anoectochilus
- anoectochilus terminal
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Abstract
本发明公开了一种去除金线莲提取液中双酯型生物碱的方法,以乌头碱含量计算金线莲提取液中双酯型生物碱的含量,往金线莲提取液加入质量为乌头碱质量1~1.5倍的三萜类有机酸,加热,回流反应1.5~2小时,自然冷却至室温,过滤,所得滤液为去除双酯型生物碱后的金线莲提取液。本发明有效地去除了金线莲提取液中双酯型生物碱,操作简单方便,使用的设备简单,运行成本低。
Description
技术领域
本发明涉及一种去除金线莲提取液中双酯型生物碱的方法。
背景技术
金线莲[Anoectochilus roxburghii(Wall.)Lindl.],又名金线兰、花叶开唇兰、金丝草、树草莲、金线虎头蕉、金线入骨消等等,为兰科开唇兰属珍稀药用植物,属于多年生的草本植物,主要分布于广东、福建、台湾等亚热带及热带地区。
金线莲在民间素有“药王”、“神草”等美称,具有广泛的药用价值。《中药大辞典》、《中药辞海》、《本草拾遗》、《中华本草》、《中国经济植物志》等著名典籍均有金线莲的记载。金线莲其性味甘平,有清热凉血、祛风除湿、解毒、降血压之功效,其药理活性作用主要表现为降血糖、降血脂、降血压、肝保护、抗炎、镇痛镇静、利尿、抗氧化等。近年来,金线莲在治疗糖尿病及肿瘤等疑难杂症方面,也引起了医药界的重视。
据报道,金线莲中含有重要药理活性的物质很多,主要有:氨基酸类(其总氨基酸以及8种人体必需氨基酸的含量均高于西洋参和野生参),石杉碱甲、乌头碱等生物碱类化合物,槲皮素、异鼠李素等黄酮类化合物,三萜与有机酸类化合物(如,木栓酮、琥珀酸、香豆酸、阿魏酸、胡萝卜苷、棕榈酸、齐墩果酸、熊果酸等),皂甙与甾体类化合物(异丙烯基胆甾醇、开唇兰甾醇、麦角甾醇、豆甾醇、菜油甾醇、β-谷甾醇等),低聚糖、还原糖等多糖类物质,以及挥发油、强心甙、牛磺酸等化学成分。
近年来,金线莲的保健功能受到人们的广泛热宠,作为历代皇宫的专用御品,现为宾馆、酒家及不少家庭的高档食材。然而,金线莲含有直接作用于心肌、对中枢神经有强烈兴奋作用的乌头碱等双酯型生物碱,口服0.2mg纯乌头碱即可中毒,3-5mg可致死。正是乌头碱等双酯型生物碱的毒性大,且金线莲中的含量较高,而致使金线莲的保健和治疗功能受到很大的限制。
由于金线莲提取液用于生命体的保健和治疗目的,不能够加入一些有毒副作用的化学物质来除去乌头碱等双酯型生物碱,即使能够加入一些毒副作用小的物质在一定程度势必会影响功效和口感,况且金线莲提取液中各种物质溶于一体,它们的分离纯化十分困难。因此,发展简便适用的技术,以保证金线莲提取液足够的保健和治疗价值和低的毒理效应,是生产金线莲提取液厂家需要解决的重要问题。
发明内容
本发明的目的是提供一种去除金线莲提取液中双酯型生物碱的方法,本方法处理效率高,工艺设备简单,操作方便,运行成本低,实现了金线莲提取液的纯化。
本发明的目的是通过以下技术方案来实现的:一种去除金线莲提取液中双酯型生物碱的方法,以乌头碱含量计算金线莲提取液中双酯型生物碱的含量,往金线莲提取液加入质量为乌头碱质量1~1.5倍的三萜类有机酸,加热至沸腾,保温回流反应1.5~2小时,自然冷却至室温,过滤,滤渣为生物碱-有机酸反应物,回收另作它用;滤液为去除双酯型生物碱后的金线莲提取液。
所述的金线莲可以是野生或者人工种植中的任何一种。
所述的双酯型生物碱可以是乌头碱、新乌头碱、次乌头碱等中的任何一种或者多种。
所述的三萜类有机酸可以是甘草酸、甘草次酸、齐墩果酸、熊果酸等中的任何一种或者多种。
所述的提取液可以是水提液或者任意体积比的乙醇-水提取液中的任何一种。
本发明的作用原理是三萜类有机酸与双酯型生物碱发生酸碱反应以及双酯型生物碱发生热分解反应的共同结果。一方面,三萜类有机酸分子中含多个羧基,属于具有较强酸性的酸性物质,双酯型生物碱分子中是含氮或者氮杂环化合物,在溶液中呈现碱性,三萜类有机酸与金线莲提取液共热时,三萜类有机酸与双酯型生物碱发生酸碱反应,形成溶解度小的产物。另一方面,双酯型生物碱在热溶液中发生分解反应,形成低毒的单酯型生物碱。分离出沉淀,即实现了从金线莲提取液中去除毒性大的双酯型生物碱。
本发明具有以下特点:
(1)效率高,该方法可除去金线莲提取液中的乌头碱、新乌头碱、次乌头碱等双酯型生物碱,三萜类有机酸处理后的金线莲提取液中没有检测出双酯型生物碱。
(2)所用原料是天然植物提取物,毒副作用小,廉价易得。
(3)工艺、设备简单,操作方便,运行成本低。
具体实施方式
下面将结合具体实施方式进一步说明本发明,但本发明要求保护的范围并不局限于下列实施方式。
实施例1
本实施例中的提取液是以水作为溶剂所制得的金线莲提取液,经检测该溶液中总生物碱(以盐酸麻黄碱计,下同)含量为34.36毫克/升,双酯型生物碱(以乌头碱计)含量为17.70毫克/升。
实施工艺操作如下:在2升圆底烧瓶中,分别加入1升金线莲提取液、100毫升含有20毫克甘草酸的水溶液,加热至沸腾,保温回流反应1.5小时,冷却至室温,过滤。滤渣回收另作它用,滤液为去除双酯型生物碱后的金线莲提取液。
经检测,甘草酸处理后的金线莲提取液中总生物碱含量为15.63毫克/升,单酯型生物碱含量(以乌头原碱计,下同)为7.37毫克/升,没有检测出双酯型的乌头碱;回收的滤渣中检测出了双酯型的乌头碱等生物碱。
本实施例中,在其它操作相同的情况下,分别用100毫升含有18毫克的甘草次酸、齐墩果酸、熊果酸水溶液代替100毫升含有20毫克甘草酸的水溶液;分别改变保温回流反应时间为1.5至2.5小时之间;均可得到与本实施例中去除双酯型生物碱净化效果相近的金线莲提取液。
实施例2
本实施例中的提取液是以乙醇作为溶剂所制得的金线莲提取液,经检测该溶液中总生物碱含量为53.68毫克/升,双酯型生物碱含量为33.17毫克/升。
实施工艺操作如下:在2升圆底烧瓶中,分别加入1升金线莲提取液、100毫升含有34毫克甘草次酸的乙醇溶液,加热至沸腾,保温回流反应1.5小时,冷却至室温,过滤。滤渣回收另作它用,滤液为去除双酯型生物碱后的金线莲提取液。
经检测,甘草次酸处理后的金线莲提取液中总生物碱含量为24.61毫克/升,单酯型生物碱含量为6.81毫克/升,没有检测出双酯型的乌头碱;回收的滤渣中检测出了双酯型的乌头碱等生物碱。
本实施例中,在其它操作相同的情况下,分别用100毫升含有40毫克甘草酸、34毫克的齐墩果酸、34毫克熊果酸乙醇溶液代替100毫升含有34毫克甘草次酸的乙醇溶液;分别改变保温回流反应时间为1.5至2.5小时之间;均可得到与本实施例中去除双酯型生物碱净化效果相近的金线莲提取液。
实施例3
本实施例中的提取液是以50%乙醇(乙醇-水体积比,下同)作为溶剂所制得的金线莲提取液,经检测该溶液中总生物碱含量为46.45毫克/升,双酯型生物碱含量为24.27毫克/升。
实施工艺操作如下:在2升圆底烧瓶中,分别加入1升金线莲提取液、100毫升含有25毫克齐墩果酸的50%乙醇溶液,加热至沸腾,保温回流反应1.5小时,冷却至室温,过滤。滤渣回收另作它用,滤液为去除双酯型生物碱后的金线莲提取液。
经检测,齐墩果酸处理后的金线莲提取液中总生物碱含量为21.65毫克/升,单酯型生物碱含量为4.69毫克/升,没有检测出双酯型的乌头碱;回收的滤渣中检测出了双酯型的乌头碱等生物碱。
本实施例中,在其它操作相同的情况下,分别用100毫升含有30毫克甘草酸、25毫克甘草次酸、25毫克熊果酸的50%乙醇溶液代替100毫升含有25毫克齐墩果酸的50%乙醇溶液;分别改变保温回流反应时间为1.5至2.5小时之间;均可得到与本实施例中去除双酯型生物碱净化效果相近的金线莲提取液。
Claims (5)
1.一种去除金线莲提取液中双酯型生物碱的方法,其特征是,以乌头碱含量计算金线莲提取液中双酯型生物碱的含量,往金线莲提取液加入质量为乌头碱质量1~1.5倍的三萜类有机酸,加热,回流反应1.5~2小时,自然冷却至室温,过滤,所得滤液为去除双酯型生物碱后的金线莲提取液。
2.根据权利要求1所述的去除金线莲提取液中双酯型生物碱的方法,其特征是,所述的金线莲为野生或者人工种植。
3.根据权利要求1所述的去除金线莲提取液中双酯型生物碱的方法,其特征是,所述的双酯型生物碱是乌头碱、新乌头碱和次乌头碱中的一种或者两种以上的组合。
4.根据权利要求1所述的去除金线莲提取液中双酯型生物碱的方法,其特征是,所述的三萜类有机酸是甘草酸、甘草次酸、齐墩果酸和熊果酸中的一种或者两种以上的组合。
5.根据权利要求1所述的去除金线莲提取液中双酯型生物碱的方法,其特征是,所述的提取液是水提液或者任意体积比的乙醇-水提取液中的一种。
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