CN106336448B - The method that brahmic acid is extracted from centella - Google Patents
The method that brahmic acid is extracted from centella Download PDFInfo
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Abstract
The invention discloses a kind of method that brahmic acid is extracted from centella, comprise the following steps：1) centella is crushed, with 60~70v% ethanol solution refluxing extractions, extract solution filtered, filtrate recycling design, then add 40~50 DEG C of water dissolvings, filtering, filter residue is dissolved in 50~60v% ethanol solutions, obtains crude extract；2) rare-earth salts mixing is added toward crude extract, stirs evenly, obtain mixed liquor；3) by the model macroporous resin columns of X on mixed liquor 5, first it is washed to colourless, then it is 20~30v% ethanol elutions with volumetric concentration, thin-layer chromatography tracing detection, collects the ethanol eluate containing asiatic acid, again with the ethanol elution that volumetric concentration is 40~50%, thin-layer chromatography tracing detection, the ethanol eluate of hydroxyl asiatic acid is collected, reclaim ethanol, dry, obtain brahmic acid.The brahmic acid purity that the present invention extracts is high, and yield is big.
Description
Technical field
The invention belongs to technical field of biological extraction, and in particular to a kind of side that brahmic acid is extracted from centella
Method.
Background technology
Centella (Centella asiatica (L.) Urban) is Umbelliferae centella tree plant, because its leaf exactly likes horse
Shoes or half of copper coin, so also known as membranaceous marshmarigold herb, Longtube Ground Ivy Herb etc., it is among the people also to there is place to be called pennyroyal mint, marchantia grass etc..Accumulated snow
Applicating history of the grass in the traditional medicine field of many countries and regions is long, China's traditional Chinese medicine to for oral administration of centella and
External application has bimillennium history, earliest quilt《Sheng Nong's herbal classic》One book is recorded.According to《Compendium of Materia Medica》Record, centella bitter,
It is pungent, it is cold in nature, it is nontoxic, return liver,spleen,kidney, stomach, its effect is promoting blood circulation, swelling and pain relieving, and has clearing heat and detoxicating, diuresis etc..Centella
Chemical composition mainly have triterpenes, flavonoids, polyyne alkenes and volatile oil etc..Triterpenes mainly has triterpene saponin, such as
Asiaticosid, madecassoside etc., and triterpene acids, such as asiatic acid, brahmic acid.The chemical composition of centella
In, triterpene acid is that research is earliest, the most deep major class component of biological activity research.Asiatic centella triterpenoid acid
Mainly it is made up of asiatic acid and brahmic acid, they belong to the pentacyclic triterpene acids of Ursane, have treatment skin
The multiple pharmacological effect such as wound, anti-inflammatory, antidepression, antitumor and repairing nerve damage, protection cardiovascular and cerebrovascular.Brahmic acid
Extract by solvents is first typically used, is then extracted using organic solvent, silica gel chromatographic column is finally crossed, is washed with petroleum ether-acetone system
It is de-.But the above method is not only cumbersome, organic solvent is not readily separated, and the loss of target component is larger, and yield is relatively low, and is extracted
Brahmic acid purity it is also smaller.
The content of the invention
Present invention solves the technical problem that it is to provide a kind of method that brahmic acid is extracted from centella, this method
It is big to extract obtained brahmic acid yield, purity is high.
Technical scheme provided by the invention be to provide it is a kind of from centella extract brahmic acid method, including with
Lower step：
1) centella is crushed, with 60~70v% ethanol solution refluxing extractions, extract solution filtered, filtrate recycling design,
Again plus 40~50 DEG C of water dissolve, and filtering, filter residue are dissolved in into 50~60v% ethanol solutions, obtains crude extract；
2) rare-earth salts mixing is added toward crude extract, stirs evenly, obtain mixed liquor；
3) by X-5 models macroporous resin column on mixed liquor, first it is washed to colourless, is then 20~30v% with volumetric concentration
Ethanol elution, thin-layer chromatography tracing detection collect the ethanol eluate containing asiatic acid, then with volumetric concentration are 40~50%
Ethanol elution, thin-layer chromatography tracing detection, the ethanol eluate of collection hydroxyl asiatic acid, by brahmic acid eluent
Ethanol is reclaimed, dries, obtains brahmic acid.
In step 1), the dosage of ethanol is 10~20 times of centella weight, refluxing extraction 1~3 time, every time 1~3h.
Volumetric concentration is that 60~70% ethanol can fully dissolve the triterpene substance in centella, including Triterpene saponins
With triterpene acid.Due to being often combined with most glycan molecules in the molecule of asiaticoside, hydroxy number is more, can show
Certain hydrophily, but hydrophily is not strong, is slightly soluble in water, and triterpene acids polarity is smaller, it is impossible to it is 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 not dissolved in hot water, by filtrate mistake
Filter, takes filter residue to be dissolved in ethanol, can reach the purpose for removing asiatic centella total saponins.
In step 2), the rare-earth salts is rare earth-iron-boron, rare earth sulfate or rare earth nitrades.Rare earth-iron-boron can be with
It is lanthanum chloride, cerium chloride, praseodymium chloride, neodymium chloride, samarium trichloride, Europium chloride, gadolinium chloride, terbium chloride, dysprosium chloride, holmium chloride, chlorination
Erbium, thulium chloride, ytterbium chloride, lutecium chloride, scandium chloride and yttrium chloride；Rare earth sulfate can be lanthanum sulfate, cerous sulfate, praseodymium sulfate,
Dineodymium trisulfate, samarium sulphate, europium sulfate, Digadolinium trisulfate, sulfuric acid terbium, dysprosium sulfate, sulfuric acid holmium, erbium sulfate, thulium sulfate, ytterbium sulfate, sulfuric acid lutetium,
Scandium sulfate and yttrium sulfate；Rare earth nitrades can be lanthanum nitrate, cerous nitrate, praseodymium nitrate, neodymium nitrate, samaric nitrate, europium nitrate, nitric acid
Gadolinium, terbium nitrate, dysprosium nitrate, holmium nitrate, erbium nitrate, thulium nitrate, ytterbium nitrate, lutecium nitrate, scandium nitrate and yttrium nitrate.
Hydroxyl on rare earth element and triterpene acid, the oxygen atom on carboxyl formed coordinate bond and, it is affine to form chemistry
Power, according to hsab theory, because rare earth is hard acid, asiatic centella triterpenoid acids is soft base, and therefore, both combinations are not special
Wen Gu not.
The dosage of the 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.
In step 3), X-5 models macroreticular resin is non-polar resin, and particle diameter is 0.3~1.25mm, specific surface area 500
~600m2/ g, average pore size are 29~30nm.Its aperture is far longer than the molecular particle size of triterpene acid, and aperture is bigger, cuts
The material stayed is fewer, and impurity is fewer.And the ligancy of rare earth is larger, with triterpene acid carry out coordinate bond and oxygen-containing function
Group's number does not often reach its highest ligancy, therefore rare earth can also produce crosslinking with the C in macroreticular resin, to reach absorption
Effect.
In order to ensure the crosslinking of rare earth element and macroreticular resin, the upper prop speed of mixed liquor is smaller, and effect is better, through application
People's many experiments, mixed liquor upper prop speed are 0.5~0.8BV/h, and cross-linking effect is best.
Due to rare earth element and triterpene acid combination very built on the sand, and triterpene acid and ethanol is affine
Power is extremely strong, is smoothly eluted triterpene acid from resin column using ethanol solution.Again due to three positions of asiatic acid
There is hydroxyl on point, these three sites are all that coordination atom is coordinated with rare earth atom, and brahmic acid compares asiatic acid
More hydroxyls, coordination ability are stronger.Therefore, in elution, asiatic acid is first eluted, and is washed after brahmic acid
Take off.Use volumetric concentration preferentially can be eluted asiatic acid for 20~30% ethanol, without being mixed into brahmic acid,
Ethanol elution speed is that 2~2.5BV/h is advisable.Then use volumetric concentration can be by madacasso for 40~50% ethanol solution
Oxalic acid is eluted, and elution speed is advisable with 2~3BV/h.
Compared with prior art, this method carries out adsorption and desorption, the brahmic acid of extraction for target component
High income is up to more than 95%, high purity more than 99.5%.
Embodiment
The present invention is further elaborated for specific examples below, but not as a limitation of the invention.
Following percentage is percentage by volume.
Embodiment 1
1) centella is crushed, adds the 60% ethanol solution refluxing extraction 1 time, each 1h of 10 times of centella gross weight, will
Extract solution filters, filtrate recycling design, then adds 40 DEG C of water dissolvings, filtering, filter residue is dissolved in into 50v% ethanol solutions, slightly carried
Liquid；
2) the lanthanum chloride mixing of its weight 0.1% is added toward crude extract, stirs evenly, obtains mixed liquor；
3) it is 0.5BV/h by X-5 models macroporous resin column on mixed liquor, upper prop speed, is first washed to colourless, then uses body
Product concentration is 20v% ethanol elutions, elution speed 2BV/h, thin-layer chromatography tracing detection, collects the ethanol containing asiatic acid and washes
De- liquid；Again with the ethanol elution that volumetric concentration is 40%, elution speed 2BV/h, thin-layer chromatography tracing detection, hydroxyl is collected
The ethanol eluate of asiatic acid, brahmic acid eluent is reclaimed into ethanol, dries, obtains brahmic acid.
Analyzed through HLPC, the rate of recovery of brahmic acid is more than 95.20%, high purity more than 99.51%.
Embodiment 2
1) centella is crushed, adds the 70% ethanol solution refluxing extraction 3 times, each 3h of 20 times of centella gross weight, will
Extract solution merges, filtering, filtrate recycling design, then adds 50 DEG C of water dissolvings, filtering, filter residue is dissolved in into 60v% ethanol solutions, obtained
Crude extract；
2) the cerous sulfate mixing of its weight 0.5% is added toward crude extract, stirs evenly, obtains mixed liquor；
3) it is 0.8BV/h by X-5 models macroporous resin column on mixed liquor, upper prop speed, is first washed to colourless, then uses body
Product concentration is 30v% ethanol elutions, elution speed 2.5BV/h, thin-layer chromatography tracing detection, collects the ethanol containing asiatic acid
Eluent；Contain hydroxyl with the ethanol elution that volumetric concentration is 50%, elution speed 3BV/h, thin-layer chromatography tracing detection, collection again
The ethanol eluate of base asiatic acid, brahmic acid eluent is reclaimed into ethanol, dries, obtains brahmic acid.
Analyzed through HLPC, the rate of recovery of brahmic acid is more than 95.13%, high purity more than 99.53%.
Embodiment 3
1) centella is crushed, adds the 65% ethanol solution refluxing extraction 2 times, each 2h of 15 times of centella gross weight, will
Extract solution merges, filtering, filtrate recycling design, then adds 45 DEG C of water dissolvings, filtering, filter residue is dissolved in into 55v% ethanol solutions, obtained
Crude extract；
2) the praseodymium nitrate mixing of its weight 0.3% is added toward crude extract, stirs evenly, obtains mixed liquor；
3) it is 0.6BV/h by X-5 models macroporous resin column on mixed liquor, upper prop speed, is first washed to colourless, then uses body
Product concentration is 25v% ethanol elutions, elution speed 2.2BV/h, thin-layer chromatography tracing detection, collects the ethanol containing asiatic acid
Eluent；Contained again with the ethanol elution that volumetric concentration is 45%, elution speed 2.5BV/h, thin-layer chromatography tracing detection, collection
The ethanol eluate of brahmic acid, brahmic acid eluent is reclaimed into ethanol, dries, obtains brahmic acid.
Analyzed through HLPC, the rate of recovery of brahmic acid is more than 95.15%, high purity more than 99.60%.
Embodiment 4
1) centella is crushed, adds the 70% ethanol solution refluxing extraction 3 times, each 1h of 10 times of centella gross weight, will
Extract solution merges, filtering, filtrate recycling design, then adds 50 DEG C of water dissolvings, filtering, filter residue is dissolved in into 50v% ethanol solutions, obtained
Crude extract；
2) the erbium chloride mixing of its weight 0.1% is added toward crude extract, stirs evenly, obtains mixed liquor；
3) it is 0.8BV/h by X-5 models macroporous resin column on mixed liquor, upper prop speed, is first washed to colourless, then uses body
Product concentration is 20v% ethanol elutions, elution speed 2.5BV/h, thin-layer chromatography tracing detection, collects the ethanol containing asiatic acid
Eluent；Contain hydroxyl with the ethanol elution that volumetric concentration is 40%, elution speed 3BV/h, thin-layer chromatography tracing detection, collection again
The ethanol eluate of base asiatic acid, brahmic acid eluent is reclaimed into ethanol, dries, obtains brahmic acid.
Analyzed through HLPC, the rate of recovery of brahmic acid is more than 95.35%, high purity more than 99.56%.
Claims (4)
1. the method for brahmic acid is extracted from centella, it is characterised in that：Comprise the following steps：
1) centella is crushed, with 60~70v% ethanol solution refluxing extractions, extract solution filtered, filtrate recycling design, then added
40~50 DEG C of water dissolvings, filtering, are dissolved in 50~60v% ethanol solutions by filter residue, obtain crude extract；
2) lanthanum chloride, cerous sulfate, praseodymium nitrate or the erbium chloride of its weight 0.1~0.5% are added toward crude extract, stirs evenly, is mixed
Close liquid；
3) by X-5 models macroporous resin column on mixed liquor, first it is washed to colourless, is then 20~30v% ethanol with volumetric concentration
Elution, thin-layer chromatography tracing detection collect the ethanol eluate containing asiatic acid, then with the ethanol that volumetric concentration is 40~50%
Elution, thin-layer chromatography tracing detection, the ethanol eluate of hydroxyl asiatic acid is collected, brahmic acid eluent is reclaimed
Ethanol, dry, obtain brahmic acid.
2. the method according to claim 1 that brahmic acid is extracted from centella, it is characterised in that：Step 1)
In, the dosage of ethanol is 10~20 times of centella weight, refluxing extraction 1~3 time, every time 1~3h.
3. the method according to claim 1 that brahmic acid is extracted from centella, it is characterised in that：Step 3)
In, mixed liquor upper prop speed is 0.5~0.8BV/h.
4. the method according to claim 1 that brahmic acid is extracted from centella, it is characterised in that：Step 3)
In, 20~30v% ethanol elutions speed is 2~2.5BV/h, and 40~50v% ethanol elution speed is 2~3BV/h.
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