WO2019051749A1 - 一种山梨猕猴桃根抗肿瘤提取物的制备方法 - Google Patents

一种山梨猕猴桃根抗肿瘤提取物的制备方法 Download PDF

Info

Publication number
WO2019051749A1
WO2019051749A1 PCT/CN2017/101815 CN2017101815W WO2019051749A1 WO 2019051749 A1 WO2019051749 A1 WO 2019051749A1 CN 2017101815 W CN2017101815 W CN 2017101815W WO 2019051749 A1 WO2019051749 A1 WO 2019051749A1
Authority
WO
WIPO (PCT)
Prior art keywords
extract
ethanol
same
preparation
ethyl acetate
Prior art date
Application number
PCT/CN2017/101815
Other languages
English (en)
French (fr)
Inventor
虞春艳
Original Assignee
虞春艳
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 虞春艳 filed Critical 虞春艳
Publication of WO2019051749A1 publication Critical patent/WO2019051749A1/zh

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P35/00—Antineoplastic agents

Definitions

  • the invention belongs to the field of medicine, and particularly relates to a preparation method of an anti-tumor extract of yam kiwi root.
  • Yamanashi kiwifruit is a kiwifruit (Actinidiaceae genus Actin-idialindl plant), which is produced in Debao, Longsheng and other counties in the poverty-stricken mountainous areas of Guangxi. Its root has been used as a folk Chinese herbal medicine. The root has an anti-cancer effect, especially for gastrointestinal tumors.
  • the wild kiwifruit resources in Guangxi are very rich, and the research and development of kiwifruit plants, especially the anti-cancer effect, has significant social and economic benefits.
  • the object of the present invention is to provide a method for preparing an anti-tumor extract of yam kiwi root.
  • the invention relates to a method for preparing an anti-tumor extract of yam kiwi root, comprising the steps of: extracting the root of kiwifruit kiwifruit by cold soaking with a volume fraction of 65-75% ethanol for 2-4 times, each time for one day, combining the extracts, and decompressing the extract.
  • the extract is concentrated to obtain an extract; the obtained extract is diluted with water, extracted with petroleum ether, ethyl acetate and water-saturated n-butanol, and concentrated under reduced pressure to obtain petroleum ether extract, ethyl acetate extract and n-butanol extract, respectively.
  • the ethyl acetate extract was dissolved in water, filtered, and separated by macroporous adsorption resin column chromatography, first 10-12 column volumes were washed with 10% ethanol to remove the polar components, and then eluted with 70% ethanol for 8-10 samples. Column volume, 70% eluate was collected, and then separated by silica gel column chromatography, and eluted with chloroform-methanol in a volume ratio of 45:1, 25:1, 15:1, and 5:1, and 15:1 elution fraction was collected. Concentrate.
  • the preparation method it is extracted by cold soaking with 70% ethanol.
  • the macroporous adsorption resin column is of the D101 type.
  • the preparation method of the anti-tumor extract of Yamanashi kiwi root provided by the invention is simple and easy, and the obtained extract has remarkable anticancer activity.
  • the invention relates to a method for preparing an anti-tumor extract of yam kiwi root, comprising the steps of: extracting the root of kiwifruit of sorbus by cold soaking with a volume fraction of 70% ethanol for 3 days, combining the extracts, and extracting the extract under reduced pressure to obtain an extract.
  • the obtained extract was diluted with water, extracted with petroleum ether, ethyl acetate and water-saturated n-butanol, and concentrated under reduced pressure to obtain petroleum ether extract, ethyl acetate extract and n-butanol extract respectively;
  • the ester extract was dissolved in water, filtered, and separated by D101 macroporous adsorption resin column chromatography, first 11 volumes of 10% ethanol were used to remove the polar components, and then eluted with 70% ethanol for 9 column volumes, 70% wash was collected.
  • the mixture was deliquored and separated by silica gel column chromatography, and eluted with chloroform-methanol in a volume ratio of 45:1, 25:1, 15:1, and 5:1, and a 15:1 fraction was collected and concentrated.
  • the invention relates to a method for preparing an anti-tumor extract of yam kiwi root, comprising the steps of: extracting the root of kiwifruit kiwifruit by cold soaking with a volume fraction of 65% ethanol for 1 day, combining the extracts, and extracting the extract under reduced pressure to obtain an extract.
  • the obtained extract was diluted with water, extracted with petroleum ether, ethyl acetate and water-saturated n-butanol, and concentrated under reduced pressure to obtain petroleum ether extract, ethyl acetate extract and n-butanol extract respectively;
  • the ester extract was dissolved in water, filtered, and separated by D101 macroporous adsorption resin column chromatography, first 10 column volumes were washed with 10% ethanol to remove the polar components, and then 7 column volumes were eluted with 70% ethanol to collect 70% of the wash.
  • the mixture was deliquored and separated by silica gel column chromatography, and eluted with chloroform-methanol in a volume ratio of 45:1, 25:1, 15:1, and 5:1, and a 15:1 fraction was collected and concentrated.
  • the invention relates to a method for preparing an anti-tumor extract of yam kiwi root, comprising the steps of: extracting the root of kiwifruit of sorbus by cold soaking with a volume fraction of 75% ethanol for 4 days, combining the extracts, and extracting the extract under reduced pressure to obtain an extract.
  • the obtained extract was diluted with water, extracted with petroleum ether, ethyl acetate and water-saturated n-butanol, and concentrated under reduced pressure to obtain petroleum ether extract, ethyl acetate extract and n-butanol extract respectively;
  • the ester extract was dissolved in water, filtered, and separated by D101 macroporous adsorption resin column chromatography.
  • the preparation method of the anti-tumor extract of Yamanashi kiwi root provided by the invention is simple and easy, and the obtained extract has remarkable anticancer activity.

Landscapes

  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Chemical & Material Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Medicinal Chemistry (AREA)
  • Biotechnology (AREA)
  • Engineering & Computer Science (AREA)
  • Microbiology (AREA)
  • Epidemiology (AREA)
  • Medical Informatics (AREA)
  • Botany (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Mycology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

一种山梨猕猴桃根抗肿瘤提取物的制备方法，该制备方法包括如下步骤：将山梨猕猴桃根用体积分数65-75％乙醇冷浸提取2-4次，每次1天，合并提取液，提取液减压浓缩得到浸膏；将所得浸膏用水稀释，依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取，减压浓缩，分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物；取乙酸乙酯萃取物用水溶解，过滤，用大孔吸附树脂柱色谱分离，先用10％乙醇冲洗10-12个柱体积除去大极性成分，再用70％乙醇洗脱8-10个柱体积，收集70％洗脱液，再经硅胶柱色谱分离，依次用体积比45:1、25:1、15:1、5:1的氯仿-甲醇洗脱，收集15:1洗脱部分，浓缩即得，该制备方法简单易行，得到的提取物具有显著的抗癌活性。

Description

一种山梨猕猴桃根抗肿瘤提取物的制备方法 技术领域
本发明属于医药领域，具体涉及一种山梨猕猴桃根抗肿瘤提取物的制备方法。
背景技术
山梨猕猴桃是猕猴桃(猕猴桃科Actinidiaceae猕猴桃属Actin-idialindl植物)，产于广西贫困山区德保、龙胜等县，其根一直作为民间中草药使用。根有抗癌作用，尤对胃肠道肿瘤疗效较佳。广西野生猕猴桃植物资源十分丰富，研究开发猕猴桃属植物，特别是研究其抗癌作用，有着显著的社会效益和经济效益。
发明内容
本发明的目的在于提供一种山梨猕猴桃根抗肿瘤提取物的制备方法。
本发明通过下面技术方案实现：
一种山梨猕猴桃根抗肿瘤提取物的制备方法，包括如下步骤：将山梨猕猴桃根用体积分数65-75％乙醇冷浸提取2-4次，每次1天，合并提取液，提取液减压浓缩得到浸膏；将所得浸膏用水稀释，依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取，减压浓缩，分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物；取乙酸乙酯萃取物用水溶解，过滤，用大孔吸附树脂柱色谱分离，先用10％乙醇冲洗10-12个柱体积除去大极性成分，再用70％乙醇洗脱8-10个柱体积，收集70％洗脱液，再经硅胶柱色谱分离，依次用体积比45:1、25:1、15:1、5:1的氯仿-甲醇洗脱，收集15:1洗脱部分，浓缩即得。
进一步地，所述的制备方法中，用70％的乙醇冷浸提取。
进一步地，所述的制备方法中，冷浸提取3次。
进一步地，所述的制备方法中，用10％乙醇冲洗11个柱体积除去大极性成分。
进一步地，所述的制备方法中，用70％乙醇洗脱9个柱体积。
进一步地，所述的制备方法中，1kg山梨猕猴桃根用8-10L溶剂进行提取。
进一步地，所述的制备方法中，1g乙酸乙酯萃取物用5-7mL水溶解。
进一步地，所述的制备方法中，大孔吸附树脂柱为D101型。
本发明技术效果：
本发明提供的山梨猕猴桃根抗肿瘤提取物的制备方法简单易行，得到的提取物具有显著的抗癌活性。
具体实施方式
下面结合实施例具体介绍本发明的实质性内容。
实施例1
一种山梨猕猴桃根抗肿瘤提取物的制备方法，包括如下步骤：将山梨猕猴桃根用体积分数70％乙醇冷浸提取3次，每次1天，合并提取液，提取液减压浓缩得到浸膏；将所得浸膏用水稀释，依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取，减压浓缩，分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物；取乙酸乙酯萃取物用水溶解，过滤，用D101大孔吸附树脂柱色谱分离，先用10％乙醇冲洗11个柱体积除去大极性成分，再用70％乙醇洗脱9个柱体积，收集70％洗脱液，再经硅胶柱色谱分离，依次用体积比45:1、25:1、15:1、5:1的氯仿-甲醇洗脱，收集15:1洗脱部分，浓缩即得。
其中，1kg山梨猕猴桃根用9L溶剂进行提取，1g乙酸乙酯萃取物用8mL水溶解。
实施例2
一种山梨猕猴桃根抗肿瘤提取物的制备方法，包括如下步骤：将山梨猕猴桃根用体积分数65％乙醇冷浸提取2次，每次1天，合并提取液，提取液减压浓缩得到浸膏；将所得浸膏用水稀释，依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取，减压浓缩，分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物；取乙酸乙酯萃取物用水溶解，过滤，用D101大孔吸附树脂柱色谱分离，先用10％乙醇冲洗10个柱体积除去大极性成分，再用70％乙醇洗脱8个柱体积，收集70％洗脱液，再经硅胶柱色谱分离，依次用体积比45:1、25:1、15:1、5:1的氯仿-甲醇洗脱，收集15:1洗脱部分，浓缩即得。
其中，1kg山梨猕猴桃根用8L溶剂进行提取，1g乙酸乙酯萃取物用5mL水溶解。
实施例3
一种山梨猕猴桃根抗肿瘤提取物的制备方法，包括如下步骤：将山梨猕猴桃根用体积分数75％乙醇冷浸提取4次，每次1天，合并提取液，提取液减压浓缩得到浸膏；将所得浸膏用水稀释，依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取，减压浓缩，分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物；取乙酸乙酯萃取物用水溶解，过滤，用D101大孔吸附树脂柱色谱分离，先用10％乙醇冲洗12个柱体积除去大极性成分，再用70％乙醇洗脱10个柱体积，收集70％洗脱液，再经硅胶柱色谱分离，依次用体积比45:1、25:1、15:1、5:1的氯仿-甲醇洗脱，收集15:1洗脱部分，浓缩即得。
其中，1kg山梨猕猴桃根用10L溶剂进行提取，1g乙酸乙酯萃取物用7mL水溶解。
本发明提供的山梨猕猴桃根抗肿瘤提取物的制备方法简单易行，得到的提取物具有显著的抗癌活性。

Claims (8)

  1. 一种山梨猕猴桃根抗肿瘤提取物的制备方法，其特征在于，包括如下步骤：将山梨猕猴桃根用体积分数65-75％乙醇冷浸提取2-4次，每次1天，合并提取液，提取液减压浓缩得到浸膏；将所得浸膏用水稀释，依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取，减压浓缩，分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物；取乙酸乙酯萃取物用水溶解，过滤，用大孔吸附树脂柱色谱分离，先用10％乙醇冲洗10-12个柱体积除去大极性成分，再用70％乙醇洗脱8-10个柱体积，收集70％洗脱液，再经硅胶柱色谱分离，依次用体积比45:1、25:1、15:1、5:1的氯仿-甲醇洗脱，收集15:1洗脱部分，浓缩即得。
  2. 根据权利要求1所述的制备方法，其特征在于：用70％的乙醇冷浸提取。
  3. 根据权利要求1所述的制备方法，其特征在于：冷浸提取3次。
  4. 根据权利要求1所述的制备方法，其特征在于：用10％乙醇冲洗11个柱体积除去大极性成分。
  5. 根据权利要求1所述的制备方法，其特征在于：用70％乙醇洗脱9个柱体积。
  6. 根据权利要求1所述的制备方法，其特征在于：1kg山梨猕猴桃根使用8-10L溶剂进行提取。
  7. 根据权利要求1所述的制备方法，其特征在于：1g乙酸乙酯萃取物用5-7mL水溶解。
  8. 根据权利要求1所述的制备方法，其特征在于：大孔吸附树脂柱为D101型。
PCT/CN2017/101815 2017-09-14 2017-09-15 一种山梨猕猴桃根抗肿瘤提取物的制备方法 WO2019051749A1 (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201710825558 2017-09-14
CN2017108255587 2017-09-14

Publications (1)

Publication Number Publication Date
WO2019051749A1 true WO2019051749A1 (zh) 2019-03-21

Family

ID=65722323

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2017/101815 WO2019051749A1 (zh) 2017-09-14 2017-09-15 一种山梨猕猴桃根抗肿瘤提取物的制备方法

Country Status (1)

Country Link
WO (1) WO2019051749A1 (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115192616A (zh) * 2022-07-13 2022-10-18 遵义医药高等专科学校 一种猕猴桃根提取物的制备及制备抗结肠癌耐药药物中的应用

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101352462A (zh) * 2008-09-08 2009-01-28 湖南老爹农业科技开发股份有限公司 一种猕猴桃根三萜类化合物及其提取方法
CN105669816A (zh) * 2015-12-29 2016-06-15 吴金凤 一种新的甾体类化合物及其制备方法和医药用途

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101352462A (zh) * 2008-09-08 2009-01-28 湖南老爹农业科技开发股份有限公司 一种猕猴桃根三萜类化合物及其提取方法
CN105669816A (zh) * 2015-12-29 2016-06-15 吴金凤 一种新的甾体类化合物及其制备方法和医药用途

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
LIANG, JIE ET AL.: "Study on Anti-tumor Effect of Extractions from Roots of Actinidia deliciosa", JOURNAL OF CHINESE MEDICINAL MATERIALS, vol. 30, no. 10, 31 October 2007 (2007-10-31), pages 1279 - 1282 *
SUN, XUEFEI ET AL.: "Effect of Radix Actinidiae Extractive on Apoptosis and Cell Cycle of Lung Cancer A549 Cells", CHINESE JOURNAL OF GERONTOLOGY, vol. 31, no. 20, October 2011 (2011-10-01), pages 4001 - 4004 *
WEI, JINYU ET AL.: "Experimental study on antineoplastic effects of the aerial parts of Actinidia indochinensis", GUANGXI MEDICAL JOURNAL, vol. 26, no. 02, 29 February 2004 (2004-02-29), pages 164 - 166 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115192616A (zh) * 2022-07-13 2022-10-18 遵义医药高等专科学校 一种猕猴桃根提取物的制备及制备抗结肠癌耐药药物中的应用
CN115192616B (zh) * 2022-07-13 2023-11-21 遵义医药高等专科学校 一种猕猴桃根提取物的制备及制备抗结肠癌耐药药物中的应用

Similar Documents

Publication Publication Date Title
CN106967137B (zh) 一种大孔树脂联用制备液相色谱分离高纯度橄榄苦苷的方法
CN103450120A (zh) 一种从红豆杉中提取紫杉醇的制备方法
CN103304613B (zh) 一种从瓜蒌皮中分离纯化4种核苷类化学成分的方法
WO2020063894A1 (zh) 一种甜叶菊的工业化利用方法及其甜菊糖苷和绿原酸
CN103550273A (zh) 一种从人参中提取低农残人参皂苷的方法
CN104857259B (zh) 一种贝母花提取物及其制备方法和应用
CN108042590B (zh) 一种低农残人参茎叶提取物及其制备方法
CN106349324A (zh) 从油橄榄叶中提取分离山楂酸的方法
CN109021046B (zh) 一种从罗汉果茎叶中同时提取槲皮苷和山萘苷的方法
CN102924537B (zh) 从罗布麻叶中同时制备金丝桃苷和异槲皮苷的方法
CN104262446A (zh) 从罗汉果中提取罗汉果甜甙v的方法
CN104910216B (zh) 一种用制备液相法同时得到多种淫羊藿黄酮的分离方法
CN104356105B (zh) 一种egcg的制备方法
WO2019051749A1 (zh) 一种山梨猕猴桃根抗肿瘤提取物的制备方法
CN101284861B (zh) 一种三萜皂苷类化合物及制备方法及用途
CN106674312A (zh) 高纯度单体獐牙菜苷系列成分的分离纯化方法
CN104230871B (zh) 一种分离枳实中多甲氧基黄酮、橙皮苷和辛弗林的方法
CN102432656A (zh) 一种蛹虫草子实体中虫草素提取纯化的方法
CN104800414A (zh) 广东紫珠中总黄酮葡萄糖醛酸苷和总苯乙醇苷的分离方法
CN104483431B (zh) 从红肉桃中分离提纯花色素苷的方法
CN109824658B (zh) 一种从忧遁草中提取、分离纯化3种黄酮苷的方法
CN109336942B (zh) 一种从人参中提取纯化竹节参皂苷ⅵ的方法
CN107353296B (zh) 一种从东革阿里中提取活性蛋白和宽缨酮的方法
CN104193793A (zh) 采用模拟移动床制备西洋参果中人参皂苷Rb3的方法
CN109053851A (zh) 一种含冬青素a的提取物及其提取方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17925233

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 17925233

Country of ref document: EP

Kind code of ref document: A1

32PN Ep: public notification in the ep bulletin as address of the adressee cannot be established

Free format text: NOTING OF LOSS OF RIGHTS PURSUANT TO RULE 112(1) EPC (EPO FORM 1205A DATED 01.10.2020)

122 Ep: pct application non-entry in european phase

Ref document number: 17925233

Country of ref document: EP

Kind code of ref document: A1