CN102188465A - Preparation method of hedera plant extractives and purposes thereof - Google Patents
Preparation method of hedera plant extractives and purposes thereof Download PDFInfo
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- CN102188465A CN102188465A CN 201110096180 CN201110096180A CN102188465A CN 102188465 A CN102188465 A CN 102188465A CN 201110096180 CN201110096180 CN 201110096180 CN 201110096180 A CN201110096180 A CN 201110096180A CN 102188465 A CN102188465 A CN 102188465A
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Abstract
The invention provides a preparation method of hedera plant extractives and purposes thereof. The preparation method comprises steps of extracting hedera plants with an extraction solvent, absorbing resin of an extracting solution with large holes, and drying alcohol eluent to obtain extractives, wherein the total saponin content in the extractives is not lower than 30%. The extractives can be solely used or matched with other extractives. The preparation method is used for preparing medicines for treating rheumatic arthritis, respiratory system diseases, hepatitis, and the like.
Description
Technical field
The invention belongs to the Chinese medicine research field, relate to a kind of preparation method of extract and uses thereof.
Background technology
The Hedera plant contains the triterpene saponin constituents more.Hederacoside C and Hederacoside are two common chemical constituents, and its content is usually also than higher.Hederacoside has α and two kinds of configurations of β, wherein is configured as main with α.Helexin also is one of common composition of Hedera.The floristic difference of Hedera can cause chemical constituent kind and content to be distinguished to some extent, but generally speaking its chemical component difference is very not big, thereby these plants has essentially identical activity.The Hedera plant mainly contains Caulis Hederae Sinensis, Hedera rhombea, Hedera helix, H.canariensis, Hedera nepalensis K. Koch, Hedera nepalensis K.Koch var.sinensis, Hedera rhombea, Hedera helix, Hedera canariensis, Hedera nepalensis K.Koch in China.Wherein China's traditional drugs kind is Caulis Hederae Sinensis Hedera nepalensis K.Koch var.sinensis.Theory of Chinese medical science thinks that it has the effect of expelling wind and removing dampness, promoting blood circulation and detumescence, suppressing the hyperactive liver, detoxifcation, be used for the treatment of rheumatic arthritis, lumbago, traumatic injury, hepatitis, dizziness, mouthful eye snail tiltedly, diseases such as epistaxis, corneal nebula, acute conjunctivitis, oedema due to nephritis, amenorrhea, swollen ulcer drug, urticaria, eczema.Treat hepatitis as among the people with Caulis Hederae Sinensis and Herba Patriniae decocting.Hedera nepalensis K. Koch, Hedera helix are cultivated more in China.Extract that there are some researches prove Hedera helix Hedera helix helps bronchus spasmolysis, thereby is used for the treatment of respiratory system disease abroad.All can be used as medicine in a plurality of positions of Hedera plant, the stem or the Herb of using Caulis Hederae Sinensis as China tradition are used as medicine, external then use the leaf of Hedera helix.Chemical research shows that its chemical constituent of the leaf of Hedera plant, stem or Herb all is based on triterpene saponin, but the position difference, and the kind of monomer whose composition or content have certain difference.
By certain method, active component in the enrichment medical material not only helps reducing the drug administration amount, can also increase curative effect, improves the quality control level of preparation.This is an important content of Chinese medicine research.Applicant is by studies have shown that, adopt macroporous adsorbent resin can effectively enrichment Hedera plant in triterpenes components, help the exploitation of original new drug.The present invention will provide a kind of feasible method for Hedera plant extract refining.
Summary of the invention
The invention provides process for purification of a kind of Hedera plant extract and uses thereof.The sample of this method preparation, total saponin content is no less than 30%, and through the technology after optimizing, total saponin content is no less than 50%.And in the made sample, the content of Hederacoside C or Hederacoside is often more than 10%, and through the technology after optimizing, monomer component content can reach more than 25%.This preparation method is with the core that is applied as of macroporous adsorbent resin, if without the macroporous adsorbent resin resin, total saponin content is difficult to reach more than 45%.Whether not crucial sample drying is.
The mensuration of total saponin content both can adopt spectrophotography in the patent of the present invention, and also the content that can adopt high-efficient liquid phase technique to measure a plurality of compositions sums up.The assay of monomer component both can adopt high performance liquid chromatography, also can adopt thin layer chromatography scanning.
The extract that the present invention is prepared can be directly used in diseases such as treatment rheumatic arthritis, respiratory system disease, hepatitis, also can with other medicines and extract compatibility thereof, be used for diseases such as rheumatic arthritis, respiratory system disease, hepatitis.
The specific embodiment
1, the Herb 2kg of Caulis Hederae Sinensis adds water 20L, decoct 3 times, and each 2 hours, each 20L, merge extractive liquid, filters last macroporous adsorbent resin D101 (amount of resin is 2L).Wash macroporous adsorbent resin with 2 times of water gagings, discard water lotion, wash resin with 4 times of volumes of 70% ethanol then, merge 70% ethanol elution.Decompression recycling ethanol, drying under reduced pressure gets extract 52g.Through the colorimetry assay, total saponin content is 64% in the extract; Through HPLC method assay, Hederacoside C content is 18%.This extract and Herba Patriniae extract share, and can be used for the treatment of hepatitis B.
2, the leaf 5kg of Hedera nepalensis K. Koch adds 50% ethanol 20L, pulverizes, soaked 5 hours, diafiltration 24 hours, constantly add in the infiltration process 50% to cumulative volume be 40L.Merge percolate, reclaim ethanol, filter last macroporous adsorbent resin AB-8 (resinae is 8L).Wash macroporous adsorbent resin with 2 times of water gagings, discard water lotion, wash resin with 2 times of volumes of 15% ethanol then, 4 times of volumes of reuse 80% ethanol are washed resin, merge 80% ethanol elution.Decompression recycling ethanol concentrates, and gets concentrated solution 500ml.Through the colorimetry assay, total saponins accounts for 52% of total solid matters in this extracting solution; Through HPLC method assay, α-Hederacoside content is 17%.This concentrated solution cooperates other pharmaceutical adjunct to make oral liquid, can be directly used in the treatment respiratory system disease.
3, the leaf 2kg of Hedera helix adds 70%20L, soaks 3 hours, decoct 2 times, and each 1.5 hours, add 70%18L for the second time, merge extractive liquid, reclaims ethanol to there not being the alcohol flavor, filters last macroporous adsorbent resin HP20 (amount of resin is 2L).Wash macroporous adsorbent resin with 2 times of water gagings, discard water lotion, wash resin with 4 times of volumes of 70% ethanol then, merge 70% ethanol elution.Decompression recycling ethanol concentrates, and gets concentrated solution 300ml.Through the colorimetry assay, total saponins accounts for 52% of total solid matters in this extracting solution; Through HPLC method assay, α-Hederacoside content is 21%.This concentrated solution cooperates other pharmaceutical adjunct to make oral liquid, can be directly used in the treatment respiratory system disease.。
4, the stem 2kg of Caulis Hederae Sinensis, with 80% ethanol extraction 3 times, each 1.5 hours, each 16L, merge extractive liquid,, decompression recycling ethanol to pure content is lower than 10%, filters last macroporous adsorbent resin SPD100 (amount of resin is 2L).Wash macroporous adsorbent resin with 2 times of water gagings, discard water lotion, wash resin with 4 times of volumes of 70% ethanol then, merge 70% ethanol elution.Decompression recycling ethanol, drying under reduced pressure gets extract 66g.Through the colorimetry assay, total saponin content is 58% in the extract; Through HPLC method assay, Hederacoside C content is 11%, and α-Hederacoside content is 13%.This extract can be directly used in treatment rheumatic arthritis.
5, the fresh leaf 2kg of Caulis Hederae Sinensis, with 50% ethanol extraction 3 times, each 1.5 hours, each 16L, merge extractive liquid,, decompression recycling ethanol to pure content is lower than 10%, filters last macroporous adsorbent resin HP20 (amount of resin is 2L).Wash macroporous adsorbent resin with 2 times of water gagings, discard water lotion, wash resin with 4 times of volumes of 70% ethanol then, merge 70% ethanol elution.Decompression recycling ethanol, drying under reduced pressure gets extract 92g.Through the colorimetry assay, total saponin content is 61% in the extract; Through HPLC method assay, Hederacoside C content is 15%.This extract can be directly used in the treatment respiratory system disease.
Claims (10)
1. the preparation method of a Hedera plant extract is characterized in that this method comprises following one or several step:
A) adopt the extraction solvent to extract, obtain extracting solution
B) extracting solution carries out enrichment with macroporous adsorbent resin, obtains the higher enrichment solution of component content
C) enrichment solution carries out drying, obtains extract.
2. according to claim 1, it is characterized in that this plant origin one or several in following plant: Caulis Hederae Sinensis, Hedera rhombea, Hedera helix, H.canariensis, Hedera nepalensis K. Koch, Hedera nepalensis K.Koch var.sinensis, Hedera rhombea, Hedera helix, Hedera canariensis, Hedera nepalensis K.Koch.
3. according to claim 1 and 2, it is characterized in that employed raw material is one or several in the following position: leaf, stem or Herb.
4. according to claim 1, it is characterized in that comprising in the step a) following one or several key element:
I) extracting solvent is water/pure system, and water is 0: 100～100: 0 with the proportionate relationship of alcohol, and the extraction solvent load is 1～100 times of raw material;
Ii) extraction time is 5～600 minutes, and extraction time is 1～10 time, and extracting temperature is 10～110 degree
Before iii) extracting, soaked 0～6000 minute
Iv) extracting method is reflux, extract,, diafiltration, warm macerating, supersound extraction or countercurrent extraction.
5. according to claim 1, it is characterized in that comprising in the step b) following one or several step:
I) the extracting solution determining alcohol that can be used for sample is not higher than 20%; If be higher than 20%, then need processing such as process distillation earlier, volatilization, make pure content be lower than 20%
II) on the extracting solution behind the sample, carry out eluting with the water of 0～200 times of column volume
III) on the extracting solution behind the sample, carry out eluting with 40% alcoholic solution that is not higher than of 0～200 times of column volume
IV) behind the water elution, carries out eluting with not being higher than 40% alcoholic solution
V) be not higher than 40% alcoholic solution eluting after, carry out eluting with being not less than 10% alcoholic solution
VI) behind the water elution, carries out eluting with being not less than 10% alcoholic solution.
6. according to claim 4 and 5, it is characterized in that used alcohol is C
1～C
10Alcohol.
7. according to claim 1, drying means is used dry means on the galenic pharmacies such as constant pressure and dry, drying under reduced pressure, spray drying, belt drying.
8. according to claim 1 to 7, it is characterized in that prepared extract has following one or several feature:
1. total saponin content is not less than 30%
2. certain monomer saponin content is not less than 10%.
9. described according to Claim 8, it is characterized in that certain monomer saponin is meant a kind of in Hederagenin C or the Hederacoside.
10. according to claim 1 to 9, it is characterized in that this extract can be separately or prescription be applied to treat rheumatic arthritis, respiratory system disease and hepatitis etc.
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| CN 201110096180 CN102188465A (en) | 2011-04-18 | 2011-04-18 | Preparation method of hedera plant extractives and purposes thereof |
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| CN 201110096180 CN102188465A (en) | 2011-04-18 | 2011-04-18 | Preparation method of hedera plant extractives and purposes thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588832A (en) * | 2013-11-26 | 2014-02-19 | 陕西嘉禾植物化工有限责任公司 | Method for separating hederacoside C and aglycone from hedera helix leaf |
| CN104306416A (en) * | 2014-10-20 | 2015-01-28 | 华东理工大学 | Medicine for treating bronchitis, pneumonia and asthma and preparation method thereof |
| CN114805466A (en) * | 2022-04-15 | 2022-07-29 | 湖南朗林生物资源股份有限公司 | Preparation method of ivy extract |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235068A (en) * | 2007-01-29 | 2008-08-06 | 中南大学 | Method for preparing hederacoside C from bindwood |
-
2011
- 2011-04-18 CN CN 201110096180 patent/CN102188465A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235068A (en) * | 2007-01-29 | 2008-08-06 | 中南大学 | Method for preparing hederacoside C from bindwood |
Non-Patent Citations (1)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 20080215 童星 中华常春藤中皂苷类成分和挥发油分离分析研究 第13、24-33页 1-7 , 第2期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588832A (en) * | 2013-11-26 | 2014-02-19 | 陕西嘉禾植物化工有限责任公司 | Method for separating hederacoside C and aglycone from hedera helix leaf |
| CN103588832B (en) * | 2013-11-26 | 2017-01-04 | 陕西嘉禾生物科技股份有限公司 | Hederacoside C and the method for aglycon is separated from Rhizoma Calystegiae Hederaceae |
| CN104306416A (en) * | 2014-10-20 | 2015-01-28 | 华东理工大学 | Medicine for treating bronchitis, pneumonia and asthma and preparation method thereof |
| CN104306416B (en) * | 2014-10-20 | 2017-08-04 | 浙江康恩贝中药有限公司 | A kind of medicine for treating bronchitis, pneumonia and asthma and preparation method thereof |
| CN114805466A (en) * | 2022-04-15 | 2022-07-29 | 湖南朗林生物资源股份有限公司 | Preparation method of ivy extract |
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Application publication date: 20110921 |