CN108676176A - A kind of preparation method of kadsura longepedunculata lignin ingredient - Google Patents
A kind of preparation method of kadsura longepedunculata lignin ingredient Download PDFInfo
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- CN108676176A CN108676176A CN201810819175.3A CN201810819175A CN108676176A CN 108676176 A CN108676176 A CN 108676176A CN 201810819175 A CN201810819175 A CN 201810819175A CN 108676176 A CN108676176 A CN 108676176A
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- A—HUMAN NECESSITIES
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/12—Antivirals
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic materials
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Abstract
The invention discloses a kind of preparation methods of kadsura longepedunculata lignin ingredient, and steps are as follows：Kadsura longepedunculata is extracted 13 times with 65 75% ethyl alcohol cold soaking of volume fraction, 3 5d, merges extracting solution every time, and extracting solution is concentrated under reduced pressure to give medicinal extract；Gained medicinal extract is diluted with water, uses petroleum ether, ethyl acetate and water saturated extracting n-butyl alcohol successively, is concentrated under reduced pressure, obtains acetic acid ethyl ester extract；By acetic acid ethyl ester extract large pore resin absorption column chromatographic isolation, first 7 column volumes are rinsed with 10% ethyl alcohol and remove big polar components, then use 75% ethanol elution, 10 column volumes, 75% eluent is collected, then detach through silica gel column chromatography, successively with volume ratio 46:1、23:1、17:1、5:1 chloroform methanol elution, collects 17:1 elution fraction, concentrates to obtain the final product.Preparation method is simple for this, and obtained lignin ingredient has significant antitumor, antiviral activity, can be used for drug preparation.
Description
Technical field
The present invention relates to a kind of preparation methods of kadsura longepedunculata lignin ingredient.
Background technology
KadsuraKadsuraKaempf. ex Juss. are under the jurisdiction of Magnoliaceae（Magnoliaceae）Schisandra chinensis is sub-
Section（Schisandroideae）, in recent years also there are many plant classification scholar tend to Schisandraceae separately as a section into
Row classification.Kadsura has 29 kinds of plant, and main product is in east Asia and the southeast.China has 10 kinds, originates in China southeast
And the provinces such as west and south, including Yunnan, Guizhou, Sichuan, Guangdong, Guangxi, Fujian.The stem of Kadsura is commonly referred to as civil
For wind rattan, glaucousback threewingnut root-bark etc., it is mainly used for promoting blood circulation and stopping pain, dispelling wind and eliminating dampness etc..Kadsura longepedunculata is Kadsura Central China five tastes
Son（Schisandra sphenantheraRehd. Et Wils.）Dry mature fruit, trade name, which is practised, claims the western five tastes
Son has convergence astringent method, nourishing generate fluid, kidney calming and other effects.Early stage is only used as certified products Schisandra chinensis（Fructus schisandrae, the southern five tastes
Son）A kind of recorded extensively in various Chinese medicine monographs and each version pharmacopeia.Since the kind is in habitats distribution, chemical composition, group
At and drug effect etc. and fructus schisandraeSchisandra chinensis (Turcz.) Baill. has a certain difference,
Therefore it is individually listed and is recorded in pharmacopeia one by version pharmacopeia in 2000.The rhizome of kadsura longepedunculata is as Caulis Kadsurae quilt《Middle traditional Chinese medicines
Allusion quotation》Version is recorded within 2010, using its as the preparation compound Caulis Kadsurae cream of raw material also by《Chinese Pharmacopoeia》Version is recorded within 2010, is cured mainly
Obstruction of collaterals by blood stasis, irregular menstruation.
Kadsura longepedunculata main chemical compositions are more single, and lignanoid and triterpenes are its characteristic constituents.In addition should
Plant also contains a small amount of sesquiterpenoids ingredient.Lignanoid is the main active of kadsura longepedunculata, can be divided according to its framework types
For 5 major class：（1）Cyclohexyl biphenyl octene class；（2）Spiral shell benzofuran type cyclohexyl biphenyl octene class；（3）Aryl-tetralin class；（4）Dibenzyl
Butanes；（5）Tetrahydrofuran derivatives.In addition, Kadsura also contains a small amount of Ne olignan.
Modern pharmacological studies have shown that there is the platymiscium anti-leukocythemia, anti-oxidant, resistance of hepatitis B, antagonism blood platelet to live
Change the factor（PAF）The effects that.In recent years, the platymiscium is antitumor, activity of anti-virus aspect is especially concerned by people.These pharmacology
Activity is mainly related with the lignanoid and triterpenes components that it contains.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of kadsura longepedunculata lignin ingredient.
The present invention is realized by following technical solution：
A kind of preparation method of kadsura longepedunculata lignin ingredient, includes the following steps：By kadsura longepedunculata volume fraction 65-
75% ethyl alcohol cold soaking extracts 1-3 times, each 3-5d, merges extracting solution, and extracting solution is concentrated under reduced pressure to give medicinal extract；Gained medicinal extract is used
Water dilutes, and uses petroleum ether, ethyl acetate and water saturated extracting n-butyl alcohol successively, is concentrated under reduced pressure, obtains acetic acid ethyl ester extract；
By acetic acid ethyl ester extract large pore resin absorption column chromatographic isolation, first with 10% ethyl alcohol rinse 7 column volumes remove big polarity at
Point, then 75% ethanol elution, 10 column volumes are used, 75% eluent is collected, then is detached through silica gel column chromatography, successively with volume ratio 46:
1、23:1、17:1、5:1 chloroform-methanol elution, collects 17:1 elution fraction, concentrates to obtain the final product.
Preferably, in the preparation method, kadsura longepedunculata 70% ethyl alcohol cold soaking of volume fraction is extracted.
Preferably, in the preparation method, cold soaking extracts 2 times.
Preferably, in the preparation method, 4d is extracted every time.
Preferably, in the preparation method, 1kg kadsura longepedunculatas are extracted using 8-10L solvents.
Preferably, in the preparation method, large pore resin absorption column is D101 types.
The technology of the present invention effect：
Preparation method is simple for this, and obtained lignin ingredient has significant antitumor, antiviral activity, can be used for medicine
It is prepared by product.
Specific implementation mode
The essentiality content of the present invention is specifically introduced with reference to embodiment.
Embodiment 1
A kind of preparation method of kadsura longepedunculata lignin ingredient, includes the following steps：By kadsura longepedunculata 70% second of volume fraction
Alcohol cold soaking extracts 2 times, each 4d, merges extracting solution, and extracting solution is concentrated under reduced pressure to give medicinal extract；Gained medicinal extract is diluted with water, according to
Secondary petroleum ether, ethyl acetate and water saturated extracting n-butyl alcohol, are concentrated under reduced pressure, obtain acetic acid ethyl ester extract；By acetic acid second
Ester extract D101 type large pore resin absorption column chromatographic isolations, first with 10% ethyl alcohol rinse 7 column volumes remove big polarity at
Point, then 75% ethanol elution, 10 column volumes are used, 75% eluent is collected, then is detached through silica gel column chromatography, successively with volume ratio 46:
1、23:1、17:1、5:1 chloroform-methanol elution, collects 17:1 elution fraction, concentrates to obtain the final product.
Wherein, 1kg kadsura longepedunculatas are extracted using 9L solvents.
Embodiment 2
A kind of preparation method of kadsura longepedunculata lignin ingredient, includes the following steps：By kadsura longepedunculata 65% second of volume fraction
Alcohol cold soaking extracts 1 time, each 3d, merges extracting solution, and extracting solution is concentrated under reduced pressure to give medicinal extract；Gained medicinal extract is diluted with water, according to
Secondary petroleum ether, ethyl acetate and water saturated extracting n-butyl alcohol, are concentrated under reduced pressure, obtain acetic acid ethyl ester extract；By acetic acid second
Ester extract D101 type large pore resin absorption column chromatographic isolations, first with 10% ethyl alcohol rinse 7 column volumes remove big polarity at
Point, then 75% ethanol elution, 10 column volumes are used, 75% eluent is collected, then is detached through silica gel column chromatography, successively with volume ratio 46:
1、23:1、17:1、5:1 chloroform-methanol elution, collects 17:1 elution fraction, concentrates to obtain the final product.
Wherein, 1kg kadsura longepedunculatas are extracted using 8L solvents.
Embodiment 3
A kind of preparation method of kadsura longepedunculata lignin ingredient, includes the following steps：By kadsura longepedunculata 75% second of volume fraction
Alcohol cold soaking extracts 3 times, each 5d, merges extracting solution, and extracting solution is concentrated under reduced pressure to give medicinal extract；Gained medicinal extract is diluted with water, according to
Secondary petroleum ether, ethyl acetate and water saturated extracting n-butyl alcohol, are concentrated under reduced pressure, obtain acetic acid ethyl ester extract；By acetic acid second
Ester extract D101 type large pore resin absorption column chromatographic isolations, first with 10% ethyl alcohol rinse 7 column volumes remove big polarity at
Point, then 75% ethanol elution, 10 column volumes are used, 75% eluent is collected, then is detached through silica gel column chromatography, successively with volume ratio 46:
1、23:1、17:1、5:1 chloroform-methanol elution, collects 17:1 elution fraction, concentrates to obtain the final product.
Wherein, 1kg kadsura longepedunculatas are extracted using 10L solvents.
Preparation method is simple for this, and obtained lignin ingredient has significant antitumor, antiviral activity, can use
It is prepared in drug.
Claims (6)
1. a kind of preparation method of kadsura longepedunculata lignin ingredient, it is characterised in that include the following steps：Kadsura longepedunculata is used
Volume fraction 65-75% ethyl alcohol cold soakings extract 1-3 times, each 3-5d, merge extracting solution, and extracting solution is concentrated under reduced pressure to give medicinal extract；It will
Gained medicinal extract is diluted with water, and uses petroleum ether, ethyl acetate and water saturated extracting n-butyl alcohol successively, is concentrated under reduced pressure, obtains acetic acid
Ethyl ester extract；By acetic acid ethyl ester extract large pore resin absorption column chromatographic isolation, first 7 column volumes are rinsed with 10% ethyl alcohol
It removes big polar component, then with 75% ethanol elution, 10 column volumes, collects 75% eluent, then detach through silica gel column chromatography, according to
It is secondary to use volume ratio 46:1、23:1、17:1、5:1 chloroform-methanol elution, collects 17:1 elution fraction, concentrates to obtain the final product.
2. preparation method according to claim 1, it is characterised in that：By kadsura longepedunculata 70% ethyl alcohol cold soaking of volume fraction
Extraction.
3. preparation method according to claim 2, it is characterised in that：Cold soaking extracts 2 times.
4. preparation method according to claim 3, it is characterised in that：Extraction 4d every time.
5. preparation method according to claim 1, it is characterised in that：1kg kadsura longepedunculatas are carried using 8-10L solvents
It takes.
6. preparation method according to claim 1, it is characterised in that：Large pore resin absorption column is D101 types.
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| CN201810819175.3A CN108676176A (en) | 2018-07-24 | 2018-07-24 | A kind of preparation method of kadsura longepedunculata lignin ingredient |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912619A (en) * | 2021-11-26 | 2022-01-11 | 沈阳药科大学 | Sesquiterpene compound extracted and separated from schisandra chinensis and method and application thereof |
| CN115707482A (en) * | 2021-08-19 | 2023-02-21 | 常熟雷允上制药有限公司 | Method for refining pulse-activating injection |
-
2018
- 2018-07-24 CN CN201810819175.3A patent/CN108676176A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115707482A (en) * | 2021-08-19 | 2023-02-21 | 常熟雷允上制药有限公司 | Method for refining pulse-activating injection |
| CN115707482B (en) * | 2021-08-19 | 2024-04-26 | 常熟雷允上制药有限公司 | Refining method of Shengmai injection |
| CN113912619A (en) * | 2021-11-26 | 2022-01-11 | 沈阳药科大学 | Sesquiterpene compound extracted and separated from schisandra chinensis and method and application thereof |
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Application publication date: 20181019 |