CN109206434A - 一种分离纯化青蒿素的方法 - Google Patents

一种分离纯化青蒿素的方法 Download PDF

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CN109206434A
CN109206434A CN201710511576.8A CN201710511576A CN109206434A CN 109206434 A CN109206434 A CN 109206434A CN 201710511576 A CN201710511576 A CN 201710511576A CN 109206434 A CN109206434 A CN 109206434A
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qinghaosu
entrainer
purifying
isolating
acetonitrile
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陈海
刘大伟
刘根水
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Jiangsu Hanbon Science and Technology Co Ltd
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Jiangsu Hanbon Science and Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
    • C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
    • C07D493/20—Spiro-condensed systems
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

本发明公开了一种分离纯化青蒿素的方法。本发明采用超临界流体色谱系统，以裸硅胶、C18、C8作为固定相，超临界CO2做流动相，甲醇、乙醇、乙腈做夹带剂，分离纯化得到青蒿素。本发明绿色环保，过程简单，易于操作。

Description

一种分离纯化青蒿素的方法
技术领域
本发明涉及一种天然产物的纯化方法，特别是青蒿素的纯化方法。
背景技术
青蒿素，英文名称为 Artemisinin，无色针状晶体。易溶于氯仿、丙酮、乙酸乙酯和苯，可溶于乙醇、乙醚，微溶于冷石油醚，几乎不溶于水。因其具有特殊的过氧基团，它对热不稳定，易受湿、热和还原性物质的影响而分解。
超临界流体色谱简单介绍：超临界流体色谱兼有气相色谱和液相色谱的特点。它既可分析气相色谱不适应的高沸点、低挥发性样品，又比高效液相色谱有更快的分析速度和条件。操作温度主要决定于所选用的流体，常用的有二氧化碳。超临界流体容易控制和调节，在进入检测器前可以转化为气体、液体或保持其超临界流体状态，因此可与现有任何液相或气相的检测器相连接，能与多种类型检测器相匹配，扩大了它的应用范围和分类能力，在定性、定量方面有较大的选择范围。还可以用多种梯度技术来优化色谱条件。并且比高效液相色谱法易达到更高的柱效率。
发明内容
本发明的目的在于提供一种分离纯化青蒿素的方法，以得到一种高纯度的青蒿素。
技术方案如下：以裸硅胶、十八烷基硅烷键合硅胶、辛烷基硅烷键合硅胶等硅胶基质类填料作为固定相，超临界CO2做流动相，甲醇、乙醇、乙腈做夹带剂，纯化的得到纯度大于98%的青蒿素。具体步骤如下：
（1）使用乙腈溶解青蒿素粗品，然后使用0.45um的微孔滤膜进行过滤；
（2）配置夹带剂，夹带剂是甲醇、乙醇、乙腈的混合物，其体积比为甲醇：乙醇：乙腈=2:3:2。；
（3）用超临界流体色谱系统对过滤后的粗品进行分离纯化，以裸硅胶、十八烷基硅烷键合硅胶、辛烷基硅烷键合硅胶作为固定相，以带有夹带剂的超临界CO2做流动相，对过滤后的青蒿素粗品进行分离纯化；
（4）将接收的液体流份使用旋转蒸发仪进行后处理，得到的白色粉末即为目标产物。
本发明具有以下技术效果：使用超临界流体色谱纯化得到纯度大于98%的青蒿素。此方法将使用CO2做流动相，仅添加少量有机溶剂，减少了有机溶剂对环境的污染，绿色环保，同时，制备过程简单，易于操作。
具体实施方式：
实施例1
使用乙腈溶解青蒿素粗品，然后使用0.45um的微孔滤膜进行过滤。配置甲醇：乙醇：乙腈=2:3:2的夹带剂，裸硅胶为固定相，超临界CO2：夹带剂=90:10的流动相体系平衡系统15min，然后进样，洗脱约70min后开始接收目标组分，接收约10min，然后使用高比例的夹带剂进行洗脱。将接收的液体流份使用旋转蒸发仪进行后处理，得到的白色粉末即为目标产物。
实施例2
使用乙腈溶解青蒿素粗品，然后使用0.45um的微孔滤膜进行过滤。配置甲醇：乙醇：乙腈=2:3:2的夹带剂，使用十八烷基硅烷键合硅胶作为固定相，使用超临界CO2：夹带剂=95:5的流动相体系平衡系统15min，然后进样，洗脱约70min后开始接收目标组分，接收约10min，然后使用高比例的夹带剂进行洗脱。将接收的液体流份使用旋转蒸发仪进行后处理，得到的白色粉末即为目标产物。
实施例3
使用乙腈溶解青蒿素粗品，然后使用0.45um的微孔滤膜进行过滤。配置甲醇：乙醇：乙腈=2:3:2的夹带剂，使用辛烷基硅烷键合硅胶作为固定相，使用超临界CO2：夹带剂=98:2的流动相体系平衡系统15min，然后进样，洗脱约70min后开始接收目标组分，接收约10min，然后使用高比例的夹带剂进行洗脱。将接收的液体流份使用旋转蒸发仪进行后处理，得到的白色粉末即为目标产物。

Claims (3)

1.一种分离纯化青蒿素的方法，其特征在于：
（1）使用乙腈溶解青蒿素粗品，然后使用0.45um的微孔滤膜进行过滤；
（2）配置夹带剂；
（3）用超临界流体色谱系统对过滤后的粗品进行分离纯化，以硅胶基质类填料作为固定相，以带有夹带剂的超临界CO2做流动相，对过滤后的青蒿素粗品进行分离纯化；
（4）将接收的液体流份使用旋转蒸发仪进行后处理，得到的白色粉末即为目标产物。
2.根据权利要求1所述的一种分离纯化青蒿素的方法，其特征在于所述的步骤（2）中的夹带剂是甲醇、乙醇、乙腈的混合物，其体积比为甲醇：乙醇：乙腈=2:3:2。
3.根据权利要求1所述的一种分离纯化青蒿素的方法，其特征在于所述的步骤（3）种的硅胶基质类填料为裸硅胶、十八烷基硅烷键合硅胶、辛烷基硅烷键合硅胶。
CN201710511576.8A 2017-06-29 2017-06-29 一种分离纯化青蒿素的方法 Withdrawn CN109206434A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114377432A (zh) * 2021-12-21 2022-04-22 江苏汉邦科技有限公司 一种超临界流体色谱分离雨生红球藻提取物的方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114377432A (zh) * 2021-12-21 2022-04-22 江苏汉邦科技有限公司 一种超临界流体色谱分离雨生红球藻提取物的方法
CN114377432B (zh) * 2021-12-21 2023-08-15 江苏汉邦科技有限公司 一种超临界流体色谱分离雨生红球藻提取物的方法

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Application publication date: 20190115