CN104387356A - 自银杏叶中提取黄酮的方法 - Google Patents

自银杏叶中提取黄酮的方法 Download PDF

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CN104387356A
CN104387356A CN201310568863.4A CN201310568863A CN104387356A CN 104387356 A CN104387356 A CN 104387356A CN 201310568863 A CN201310568863 A CN 201310568863A CN 104387356 A CN104387356 A CN 104387356A
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CN104387356B (zh
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刘忠群
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GUANGXI LAIJI BIOLOGICAL ENGINEERING CO., LTD.
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GUANGXI LAIJI BIOLOGICAL ENGINEERING Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/28Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
    • C07D311/30Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/40Separation, e.g. from natural material; Purification
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Abstract

本发明公开一种自银杏叶中提取黄酮的方法,涉及提取工艺技术领域,包括如下提取步骤:将干银杏叶进行粉碎,然后将银杏叶粉末浸入40℃-60℃的温水中进行浸提,浸提中固液比为1:10(V/W),提取时间为3小时,提取三次,提取后过滤、合并滤液;将浸提液浓缩干燥后,采用5倍体积的40℃-50℃的温水进行溶解,再采用无水乙酸乙酯溶剂进行萃取3次,继续用无水乙酸乙酯进行多次结晶处理,结晶过程中固液比为1:5,将结晶粗品经过1次超临界CO2萃取、干燥处理即可获得纯度98%以上的银杏黄酮,本发明工艺简单,直接进行浸提分离、结晶纯化,无须柱色谱等复杂、耗时、耗能工艺;使用超临界CO2萃取,银杏黄酮纯度超过98%。

Description

自银杏叶中提取黄酮的方法
技术领域
本发明涉及提取工艺技术领域,尤其是一种自银杏叶中提取黄酮的方法。
背景技术
银杏科植物银杏是我国的特有树种,又名白果树,树龄可达千年以上,是古代二叠纪孑遗植物,有植物界中的“活化石”之称,是现存种子植物中最古老的孑遗植物。
近代科学表明,银杏叶的化学成分十分复杂,其中银杏叶中含有黄酮类、萜类、酚类、有益微量元素和多种氨基酸等有效成分。银杏叶提取物含有大量的银杏黄酮和银杏内酯等物质,它能够增加脑血管流量,改善脑血管循环功能,保护脑细胞、夸张冠状动脉,防止心绞痛及心肌梗塞,防止血栓形成,提高机体免疫能力。对冠心病、心绞痛、脑动脉硬化、老年痴呆、高血压病人均十分有益。
活性物质中黄酮和内酯的含量决定着银杏叶的药用价值,想要获得较多的黄酮,关键在于银杏叶的提取方法;传统的提取过程中,溶剂在加热的条件下容易进入细胞,但可溶性物质在热的条件溶解度更高,先后被溶解而出现很高的渗透性,造成提取率低、活性成分低,而且工艺繁琐,生产周期长。
发明内容
本发明所要解决的问题是提供一种有效、高速的自银杏叶中提取黄酮的方法。
为了解决上述技术问题,本发明所采用的技术方案是:包括如下提取步骤:
(1)将干银杏叶进行粉碎,粉末过15-30目筛;
(2)将粉碎后的银杏叶粉末浸入40℃-60℃的温水中进行浸提,浸提中固液比为1:10(V/W),提取时间为3小时,提取三次,提取后过滤、合并滤液;
(3)将浸提液浓缩干燥后,采用5倍体积的40℃-50℃的温水进行溶解,再采用无水乙酸乙酯溶剂进行萃取3次,继续用无水乙酸乙酯进行多次结晶处理,结晶过程中固液比为1:5(V/W);
(4)将上述结晶粗品经过1次超临界CO2萃取、干燥处理即可获得纯度98%以上的银杏黄酮。
上述技术方案中,更具体的方案还可以是:步骤(4)中,萃取釜压力为10-20MPa,萃取温度为40℃-50℃,萃取时间为30-45分钟。
本发明的优点在于:工艺简单,直接进行浸提分离、结晶纯化,无须柱色谱等复杂、耗时、耗能工艺;使用超临界CO2萃取,银杏黄酮纯度超过98%。
具体实施方式
实施例1:
将1000g的银杏叶进行粉碎,粉末过10目筛;将粉碎后的银杏叶粉末浸入40℃的10L温水中进行浸提,提取时间为3小时,每小时提取1次,共提取三次,提取后过滤、合并滤液,将浸提液浓缩干燥后,得到固体粉末100g,采用500ml的40℃的温水进行溶解,再采用无水乙酸乙酯溶剂进行萃取3次,继续用无水乙酸乙酯进行多次结晶处理,结晶过程中固液比为1:5(V/W),将上述结晶粗品经过1次超临界CO2萃取、干燥处理,萃取釜压力为10MPa,萃取温度为40℃,萃取时间为30分钟,即可获得纯度98.7%的银杏黄酮。
实施例2:
将1000g的银杏叶进行粉碎,粉末过30目筛;将粉碎后的银杏叶粉末浸入60℃的10L温水中进行浸提,提取时间为3小时,每小时提取1次,共提取三次,提取后过滤、合并滤液,将浸提液浓缩干燥后,得到固体粉末100g,采用500ml的50℃的温水进行溶解,再采用无水乙酸乙酯溶剂进行萃取3次,继续用无水乙酸乙酯进行多次结晶处理,结晶过程中固液比为1:5(V/W),将上述结晶粗品经过1次超临界CO2萃取、干燥处理,萃取釜压力为20MPa,萃取温度为50℃,萃取时间为45分钟,即可获得纯度99.2%的银杏黄酮。 

Claims (2)

1.一种自银杏叶中提取黄酮的方法,其特征在于包括如下提取步骤:
(1)将干银杏叶进行粉碎,粉末过15-30目筛;
(2)将粉碎后的银杏叶粉末浸入40℃-60℃的温水中进行浸提,浸提中固液比为1:10(V/W),提取时间为3小时,提取三次,提取后过滤、合并滤液;
(3)将浸提液浓缩干燥后,采用5倍体积的40℃-50℃的温水进行溶解,再采用无水乙酸乙酯溶剂进行萃取3次,继续用无水乙酸乙酯进行多次结晶处理,结晶过程中固液比为1:5(V/W);
(4)将上述结晶粗品经过1次超临界CO2萃取、干燥处理即可获得纯度98%以上的银杏黄酮。
2.根据权利要求1所述的自银杏叶中提取黄酮的方法,其特征在于:步骤(4)中,萃取釜压力为10-20MPa,萃取温度为40℃-50℃,萃取时间为30-45分钟。
CN201310568863.4A 2013-11-15 2013-11-15 自银杏叶中提取黄酮的方法 Expired - Fee Related CN104387356B (zh)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105250487A (zh) * 2015-10-19 2016-01-20 潘勤霞 一种提取茄子黄酮的方法
CN105767397A (zh) * 2016-05-12 2016-07-20 广西科技大学鹿山学院 一种健脾和胃银杏茶
CN105767396A (zh) * 2016-05-12 2016-07-20 广西科技大学鹿山学院 一种降脂银杏茶
CN105876017A (zh) * 2016-05-12 2016-08-24 广西科技大学鹿山学院 一种银杏保健茶
CN105918559A (zh) * 2016-05-12 2016-09-07 广西科技大学鹿山学院 一种降血糖银杏茶
CN105994736A (zh) * 2016-05-12 2016-10-12 广西科技大学鹿山学院 一种润肺止咳银杏茶
CN105998097A (zh) * 2016-05-12 2016-10-12 广西科技大学鹿山学院 一种降血压银杏茶
CN105994735A (zh) * 2016-05-12 2016-10-12 广西科技大学鹿山学院 一种提神醒脑银杏茶
CN105994797A (zh) * 2016-05-12 2016-10-12 广西科技大学鹿山学院 一种提高免疫银杏茶
CN106309757A (zh) * 2016-09-29 2017-01-11 许超群 一种提神醒脑百香果含片
CN106420995A (zh) * 2016-09-29 2017-02-22 许超群 一种降血压百香果含片
TWI777096B (zh) * 2019-05-16 2022-09-11 大江生醫股份有限公司 銀杏癒傷組織的萃取物用於改善肌膚泛紅的用途

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CN102093326A (zh) * 2010-12-22 2011-06-15 晨光生物科技集团股份有限公司 一种从银杏叶中提取精制银杏黄酮的方法
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105250487A (zh) * 2015-10-19 2016-01-20 潘勤霞 一种提取茄子黄酮的方法
CN105767397A (zh) * 2016-05-12 2016-07-20 广西科技大学鹿山学院 一种健脾和胃银杏茶
CN105767396A (zh) * 2016-05-12 2016-07-20 广西科技大学鹿山学院 一种降脂银杏茶
CN105876017A (zh) * 2016-05-12 2016-08-24 广西科技大学鹿山学院 一种银杏保健茶
CN105918559A (zh) * 2016-05-12 2016-09-07 广西科技大学鹿山学院 一种降血糖银杏茶
CN105994736A (zh) * 2016-05-12 2016-10-12 广西科技大学鹿山学院 一种润肺止咳银杏茶
CN105998097A (zh) * 2016-05-12 2016-10-12 广西科技大学鹿山学院 一种降血压银杏茶
CN105994735A (zh) * 2016-05-12 2016-10-12 广西科技大学鹿山学院 一种提神醒脑银杏茶
CN105994797A (zh) * 2016-05-12 2016-10-12 广西科技大学鹿山学院 一种提高免疫银杏茶
CN106309757A (zh) * 2016-09-29 2017-01-11 许超群 一种提神醒脑百香果含片
CN106420995A (zh) * 2016-09-29 2017-02-22 许超群 一种降血压百香果含片
TWI777096B (zh) * 2019-05-16 2022-09-11 大江生醫股份有限公司 銀杏癒傷組織的萃取物用於改善肌膚泛紅的用途

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