CN106214710A - The method extracting triterpene acid from Herba Centellae - Google Patents
The method extracting triterpene acid from Herba Centellae Download PDFInfo
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- CN106214710A CN106214710A CN201610727718.XA CN201610727718A CN106214710A CN 106214710 A CN106214710 A CN 106214710A CN 201610727718 A CN201610727718 A CN 201610727718A CN 106214710 A CN106214710 A CN 106214710A
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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)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
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- A—HUMAN NECESSITIES
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention discloses a kind of method extracting triterpene acid from Herba Centellae, comprise the following steps: 1) Herba Centellae is pulverized, by 60～70v% ethanol solution reflux, extract, extracting solution is filtered, filtrate recycling design, then add 40～50 DEG C of water dissolutioies, filter, filtering residue is dissolved in 50～60v% ethanol solution, obtains crude extract；2) add rare-earth salts mixing toward crude extract, stir evenly, obtain mixed liquor；3) by X on mixed liquor 5 model macroporous resin column, first it is washed to colourless, is then 50～70v% ethanol elutions by volumetric concentration, collect ethanol elution, reclaim ethanol, be dried, obtain triterpene acid.The triterpene acids material purity that the present invention extracts is high, and yield is big.
Description
Technical field
The invention belongs to technical field of biological extraction, be specifically related to a kind of side extracting triterpene acid from Herba Centellae
Method.
Background technology
Herba Centellae (Centella asiatica (L.) Urban) is Umbelliferae Herba Centellae tree plant, because its leaf exactly likes horse
Shoes or half copper coin, so having another name called Herba Calthae Membranaceae, Herba Glechomae etc., among the people also have place to be called pennyroyal mint, marchantia grass etc..Accumulated snow
Grass applicating history in the traditional medicine field of many countries and regions is long, China's Chinese medicine Herba Centellae take with
The existing bimillennium history of external, is recorded by Shennong's Herbal one book the earliest.Record according to Compendium of Material Medica, Herba Centellae bitter in the mouth,
Pungent, cold in nature, nontoxic, return liver,spleen,kidney, stomach warp, its effect for invigorating blood circulation, reducing swelling and alleviating pain, and have heat-clearing and toxic substances removing, diuresis etc..Herba Centellae
Chemical composition mainly have triterpenes, flavonoid, polyacetylene alkenes and volatile oil etc..Triterpenes mainly has triterpene saponin, as
Asiaticoside, asiaticoside etc., and triterpene acids, such as asiatic acid, Madecassic acid etc..The chemical composition of Herba Centellae
In, triterpene acid is to study the earliest, the big class component that biological activity research is the most deep.Asiatic centella triterpenoid acid
Mainly being made up of asiatic acid and Madecassic acid, they belong to the pentacyclic triterpene acids of Ursane, have treatment skin
Wound, the multiple pharmacological effect such as antiinflammatory, antidepressant, antitumor and repairing nerve damage, protection cardiovascular and cerebrovascular vessel.Asiatic centella triterpenoid acid
Class the most first with extract by solvents, then uses organic solvent extraction, finally crosses silica gel chromatographic column, by petroleum ether-acetone system
Eluting.But said method is the most loaded down with trivial details, organic solvent is not readily separated, and the loss of target component is relatively big, and yield is relatively low, Er Qieti
The purity of the triterpene acid taken is the least.
Summary of the invention
Present invention solves the technical problem that and be to provide a kind of method extracting triterpene acid from Herba Centellae, the method
Extracting the triterpene acids Physical yield obtained big, purity is high.
The present invention provide technical scheme be to provide a kind of from Herba Centellae extract triterpene acid method, including with
Lower step:
1) Herba Centellae is pulverized, by 60～70v% ethanol solution reflux, extract, extracting solution is filtered, filtrate recycling design,
Add 40 again～50 DEG C of water dissolutioies, filter, filtering residue is dissolved in 50～60v% ethanol solution, obtains crude extract；
2) add rare-earth salts mixing toward crude extract, stir evenly, obtain mixed liquor；
3) by X-5 model macroporous resin column on mixed liquor, first it is washed to colourless, is then 50～70v% by volumetric concentration
Ethanol elution, collects ethanol elution, reclaims ethanol, is dried, obtains triterpene acid.
Step 1) in, the consumption of ethanol is 10～20 times of Herba Centellae weight, reflux, extract, 1～3 times, each 1～3h.
Volumetric concentration is the ethanol triterpene substance that can fully dissolve in Herba Centellae of 60～70%, including Triterpene saponins
With triterpene acid.Owing to being often combined with most glycan molecule in the molecule of asiaticoside, hydroxy number is many, can show
Certain hydrophilic, but hydrophilic is not strong, is slightly soluble in water, and triterpene acids polarity is less, it is impossible to be soluble in water.Therefore adopt
Asiatic centella total saponins can be helped to dissolve with 40～50 DEG C of warm water, asiatic centella triterpenoid acid is insoluble in hot water, by filtrate mistake
Filter, takes filtering residue and is dissolved in ethanol, can reach the purpose removing asiatic centella total saponins.
Step 2) in, described rare-earth salts is rare earth chloride, rare earth sulfate or rare earth nitrate.Rare earth chloride is permissible
It is lanthanum chloride, cerium chloride, praseodymium chloride, Neodymium chloride, samarium trichloride, Europium chloride, Gadolinium trichloride, terbium chloride, Dysprosium trichloride, Holmium trichloride, chlorination
Erbium, thulium chloride, Ytterbium trichloride, lutecium chloride, Scium chloride (Sc4Cl12) and Yttrium chloride(Y2Cl6)；Rare earth sulfate can be lanthanum sulfate, cerous sulfate, Dipraseodymium trisulfate,
Dineodymium trisulfate, samarium sulphate, europium sulfate, Digadolinium trisulfate, sulphuric acid terbium, Dysprosium sesquisulfate, sulphuric acid holmium, erbium sulfate, thulium sulfate, Ytterbium Sulfate, sulphuric acid lutecium,
Scium sulfate (Sc2(SO4)3) and Yttrium sesquisulfate；Rare earth nitrate can be Lanthanum (III) nitrate, cerous nitrate, praseodymium nitrate, neodymium nitrate, samaric nitrate, europium nitrate, nitric acid
Gadolinium, Terbium nitrate (Tb(NO3)3), Dysprosium trinitrate, holmium nitrate, Erbium trinitrate, thulium nitrate, Ytterbium(III) nitrate., lutecium nitrate, Scium nitrate(Sc(NO3)3) and Yttrium trinitrate.
On rare earth element and triterpene acid the oxygen atom on hydroxyl, carboxyl formed coordinate bond and, form chemistry affine
Power, according to hsab theory, owing to rare earth is hard acid, asiatic centella triterpenoid acids is soft base, and therefore, both combinations are not special
The most firm.
The consumption of described rare-earth salts is the 0.1～0.5% of crude extract weight.Now, rare earth element can be with triterpene acids thing
Matter is fully coordinated.
Step 3) in, X-5 model macroporous resin is non-polar resin, and particle diameter is 0.3～1.25mm, and specific surface area is 500
～600m2/ g, average pore size is 29～30nm.Its aperture is far longer than the molecular particle size of triterpene acid, and aperture is the biggest, cuts
The material stayed is the fewest, and impurity is the fewest.And the ligancy of rare earth is relatively big, carry out the oxygen-containing functional group number of coordinate bond sum with it often
Not reaching its highest ligancy, therefore rare earth also can produce crosslinking with the C in macroporous resin, to reach the effect of absorption.
In order to ensure the crosslinking of rare earth element and macroporous resin, the upper prop speed of mixed liquor is the least, and effect is the best, through application
People's great many of experiments, mixed liquor upper prop speed is 0.5～0.8BV/h, and cross-linking effect is best.
Due to rare earth element and triterpene acid combination the most built on the sand, and triterpene acid and ethanol is affine
Power is extremely strong, use volumetric concentration be 50～70% ethanol triterpene acid can be eluted smoothly from resin column, eluting
Agent consumption is 1～2BV, and elution speed is 2～2.5BV/h.
Compared with prior art, this method carries out adsorption and desorption for target component, the triterpene acid of extraction
Yield is up to more than 97%, high purity more than 99.5%.
Detailed description of the invention
The present invention is further elaborated for specific examples below, but not as a limitation of the invention.
Following percent is percentage by volume.
Embodiment 1
1) Herba Centellae is pulverized, 60% ethanol solution reflux, extract, of addition Herba Centellae gross weight 10 times 1 time, each 1h, will
Extracting solution filters, filtrate recycling design, then adds 40 DEG C of water dissolutioies, filters, filtering residue is dissolved in 50v% ethanol solution, is slightly carried
Liquid；
2) add the lanthanum chloride mixing of its weight 0.1% toward crude extract, stir evenly, obtain mixed liquor；
3) by X-5 model macroporous resin column on mixed liquor, upper prop speed is 0.5BV/h, is first washed to colourless, then uses body
Volume concentrations is 50% ethanol elution, and the consumption of ethanol is 1BV, and elution speed is 2BV/h, collects ethanol elution, reclaims ethanol,
It is dried, obtains triterpene acid.Analyzing through HLPC, the response rate of triterpene acid is more than 97.24%, high purity
More than 99.50%.
Embodiment 2
1) Herba Centellae is pulverized, 70% ethanol solution reflux, extract, of addition Herba Centellae gross weight 20 times 3 times, each 3h, will
Extracting solution merges, and filters, filtrate recycling design, then adds 50 DEG C of water dissolutioies, filters, filtering residue is dissolved in 60v% ethanol solution, obtains
Crude extract；
2) add the cerous sulfate mixing of its weight 0.5% toward crude extract, stir evenly, obtain mixed liquor；
3) by X-5 model macroporous resin column on mixed liquor, upper prop speed is 0.8BV/h, is first washed to colourless, then uses body
Volume concentrations is 70% ethanol elution, and the consumption of ethanol is 2BV, and elution speed is 2.5BV/h, collects ethanol elution, reclaims second
Alcohol, is dried, obtains triterpene acid.
Analyzing through HLPC, the response rate of triterpene acid is more than 97.33%, high purity more than 99.58%.
Embodiment 3
1) Herba Centellae is pulverized, 65% ethanol solution reflux, extract, of addition Herba Centellae gross weight 15 times 2 times, each 2h, will
Extracting solution merges, and filters, filtrate recycling design, then adds 45 DEG C of water dissolutioies, filters, filtering residue is dissolved in 55v% ethanol solution, obtains
Crude extract；
2) add the praseodymium nitrate mixing of its weight 0.3% toward crude extract, stir evenly, obtain mixed liquor；
3) by X-5 model macroporous resin column on mixed liquor, upper prop speed is 0.6BV/h, is first washed to colourless, then uses body
Volume concentrations is 60% ethanol elution, and the consumption of ethanol is 1.5BV, and elution speed is 2.5BV/h, collects ethanol elution, reclaims
Ethanol, is dried, obtains triterpene acid.
Analyzing through HLPC, the response rate of triterpene acid is more than 97.18%, high purity more than 99.55%.
Embodiment 4
1) Herba Centellae is pulverized, 70% ethanol solution reflux, extract, of addition Herba Centellae gross weight 10 times 3 times, each 1h, will
Extracting solution merges, and filters, filtrate recycling design, then adds 50 DEG C of water dissolutioies, filters, filtering residue is dissolved in 50v% ethanol solution, obtains
Crude extract；
2) add the Erbium trichloride mixing of its weight 0.1% toward crude extract, stir evenly, obtain mixed liquor；
3) by X-5 model macroporous resin column on mixed liquor, upper prop speed is 0.8BV/h, is first washed to colourless, then uses body
Volume concentrations is 50% ethanol elution, and the consumption of ethanol is 2BV, and elution speed is 2BV/h, collects ethanol elution, reclaims ethanol,
It is dried, obtains triterpene acid.
Analyzing through HLPC, the response rate of triterpene acid is more than 97.09%, high purity more than 99.63%.
Claims (6)
1. the method extracting triterpene acid from Herba Centellae, it is characterised in that: comprise the following steps:
1) Herba Centellae is pulverized, by 60～70v% ethanol solution reflux, extract, extracting solution is filtered, filtrate recycling design, then add
40～50 DEG C of water dissolutioies, filter, filtering residue are dissolved in 50～60v% ethanol solution, obtain crude extract；
2) add rare-earth salts mixing toward crude extract, stir evenly, obtain mixed liquor；
3) by X-5 model macroporous resin column on mixed liquor, first it is washed to colourless, is then 50～70v% ethanol by volumetric concentration
Eluting, collects ethanol elution, reclaims ethanol, is dried, obtains triterpene acid.
The method extracting triterpene acid from Herba Centellae the most according to claim 1, it is characterised in that: step 1)
In, the consumption of ethanol is 10～20 times of Herba Centellae weight, reflux, extract, 1～3 times, each 1～3h.
The method extracting triterpene acid from Herba Centellae the most according to claim 1, it is characterised in that: step 2)
In, described rare-earth salts is rare earth chloride, rare earth sulfate or rare earth nitrate.
The method extracting triterpene acid from Herba Centellae the most according to claim 1, it is characterised in that: step 2)
In, the consumption of described rare-earth salts is the 0.1～0.5% of crude extract weight.
The method extracting triterpene acid from Herba Centellae the most according to claim 1, it is characterised in that: step 3)
In, mixed liquor upper prop speed is 0.5～0.8BV/h.
The method extracting triterpene acid from Herba Centellae the most according to claim 1, it is characterised in that: step 3)
In, the consumption of ethanol is 1～2BV, and elution speed is 2～2.5BV/h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109006227A (en) * | 2018-09-05 | 2018-12-18 | 山西农业大学 | A kind of membranous milkvetch stem and leaf returning to the field ecology planting method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101991578A (en) * | 2009-08-24 | 2011-03-30 | 赵全成 | Application of asiatic acid and madecassic acid in preparation of alpha-glucosidase inhibitor drugs |
| CN101991624A (en) * | 2009-08-27 | 2011-03-30 | 上海新康制药厂 | Method for preparing total asiatic acid, asiatic acid and madecassic acid from asiatic pennywort herb and use of prepared product |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101991578A (en) * | 2009-08-24 | 2011-03-30 | 赵全成 | Application of asiatic acid and madecassic acid in preparation of alpha-glucosidase inhibitor drugs |
| CN101991624A (en) * | 2009-08-27 | 2011-03-30 | 上海新康制药厂 | Method for preparing total asiatic acid, asiatic acid and madecassic acid from asiatic pennywort herb and use of prepared product |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109006227A (en) * | 2018-09-05 | 2018-12-18 | 山西农业大学 | A kind of membranous milkvetch stem and leaf returning to the field ecology planting method |
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Application publication date: 20161214 |