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

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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
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extract
ethanol
same
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ethyl acetate
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虞春艳
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虞春艳
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    • 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

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  • 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.

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Chemical & Material Sciences (AREA)
  • Veterinary Medicine (AREA)
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  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
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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)

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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

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