CN101407536A - Process for preparing high-purity asiaticoside by solvent crystallization - Google Patents
Process for preparing high-purity asiaticoside by solvent crystallization Download PDFInfo
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- CN101407536A CN101407536A CNA200810162211XA CN200810162211A CN101407536A CN 101407536 A CN101407536 A CN 101407536A CN A200810162211X A CNA200810162211X A CN A200810162211XA CN 200810162211 A CN200810162211 A CN 200810162211A CN 101407536 A CN101407536 A CN 101407536A
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Abstract
The invention discloses a technique of using a solvent crystallization method to prepare asiaticoside with high purity, which has the technique steps as follows: 1) the asiaticoside is solid-liquid separated after being dissolved by a solvent I so as to obtain an asiaticoside solution; and 2) a solvent II is added in the asiaticoside solution for crystallization, two parts of solid substances and crystallized mother liquor are obtained after solid-liquid separation, and finally asiaticoside products with high purity can be obtained by vacuum drying the solid substances. Primary crystallization of the invention can prepare the asiaticoside products with purity of more than 90 percent, and the yield of the asiaticoside can reach more than 80 percent. A repeated crystallization mode can be used for preparing asiaticoside products with higher purity, for example, the asiaticoside products with purity of more than 95 percent can be obtained by twice crystallization. In addition, the crystallized mother liquor is rich in asiaticoside A and asiaticoside B, and can be used further. The technique has the advantages of simple process, low production cost, less pollution, high asiaticoside product yield, high purity and the like, and is suitable for industrialization production.
Description
Technical field
The present invention relates to a kind of technology of preparing high-purity asiaticoside by solvent crystallization.
Background technology
Herba Centellae [Centella asiatica (L.) UrBan] is a samphire, and how (Linnaeus Carolus) was included into Lawn Pennywort Herb in 1764 with Herba Centellae and belongs to (Hydrocotyle), and names the L. into Hydrocotyleasiatica the botanist woods.In 1879, with its independent from Lawn Pennywort Herb belongs to and set up Centella (Centella), be included into this genus and rename Centella asiatica (L.) Urb. as by Herba Centellae according to the rib number of the arrangement of petal and fruit for fritz UrBan.Herba Centellae mainly is distributed in the southern hemisphere and northern hemisphere torrid zone and subtropical zone, and main product ground is South Africa, India, Sri Lanka, Malaysia, Indonesia, Australia, Japan etc., and China also produces Herba Centellae.Herba Centellae for two thousand years, among the people is usually used in treating flu, tonsillitis, infectious hepatitis, dysentery, wound, furuncle swelling toxin, traumatic hemorrhage etc. at the medicinal history of China.Research of Herba Centellae modern pharmacology and application have had very great development, show that Herba Centellae can be used for treating dysthymia disorders, skin wound, stomach ulcer, infectious hepatitis, tetter and meningococcal meningitis etc.
The complex chemical composition of Herba Centellae mainly contains triterpenes, flavonoid, volatile oil, polyyne alkene class etc.Wherein triterpene compound is main effective component, comprises centella asiatica glucoside, centella asiatica glucoside A, ripple hot-die glycosides, Bo Remi glycosides, thankuniside, isothankuniside, asiatic acid, hydroxyl Herba Centellae Bo Remi acid, madasiatic acid etc.Herba Centellae total glycosides is a general name of extracting the saponins material that obtains from Herba Centellae, mainly form by triterpene glycoside material, wherein representative composition mainly contains centella asiatica glucoside (Aisaticoside, CAS No.:16830-15-2), centella asiatica glucoside A (Asaiticoside A; Madecassoside, CAS No.:34540-22-2) and centella asiatica glucoside B (Asaiticoside B, CAS No.:125265-68-1).Centella asiatica glucoside A also is asiaticoside, and centella asiatica glucoside B and centella asiatica glucoside A are a pair of isomerss.Centella asiatica glucoside A and centella asiatica glucoside B have compared a hydroxyl many with centella asiatica glucoside, polarity difference is bigger, and the difference of centella asiatica glucoside A and centella asiatica glucoside B only is that one of them methyl ownership is different, and two different ownership are in the ortho position and concern that polarity difference is less.
The structural formula of centella asiatica glucoside (a), centella asiatica glucoside A (b) and centella asiatica glucoside B (c) is as follows:
Studies show that centella asiatica glucoside has the promotion wound healing, the pharmacological action of treatment scar.
Centella asiatica glucoside has had wide practical use in fields such as medicine, makeup, and adopt column chromatography method from Herba Centellae total glycosides, to separate the preparation centella asiatica glucoside at present mostly, there are long, shortcomings such as solvent consumption is many, cost height of operational cycle in this method, cause high-purity asiaticoside price height, so be necessary very much to seek the preparation method that processing method that high efficiency separation prepares centella asiatica glucoside changes existing centella asiatica glucoside, to reduce its production cost and to improve its production efficiency.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of technology of preparing high-purity asiaticoside by solvent crystallization is provided.
Comprise the steps:
1) Herba Centellae total glycosides carries out solid-liquid separation after dissolving with solvent I, obtains Herba Centellae total glycosides solution;
2) add solvent II in the Herba Centellae total glycosides solution and carry out crystallization, obtain solid substance and crystalline mother solution two portions then after solid-liquid separation, last solid substance obtains the high-purity asiaticoside product after vacuum-drying.
Solvent I is methyl alcohol or dimethyl formamide (DMF) in the step 1), and add-on is 2.5～100mL/g Herba Centellae total glycosides.Step 2) solvent II is acetone, acetonitrile, ether, ethyl acetate or water in, and add-on is 0.5～10 times of solvent I add-on.Step 1) and step 2) in solid-liquid separating method for filtering or centrifugal.
High-purity asiaticoside among the present invention is meant that purity greater than 90% centella asiatica glucoside product, prepares by primary crystallization, and the centella asiatica glucoside yield can reach more than 80%.Temperature is little to the influence of crystallisation process, can carry out in room temperature, and crystallization time is usually more than 12 hours.If need more highly purified centella asiatica glucoside product, can adopt repeatedly crystalline mode, for example can obtain the centella asiatica glucoside product of 95% above purity through twice crystallization.In addition, crystalline mother solution is rich in centella asiatica glucoside A and centella asiatica glucoside B, can further be used.
The present invention has that process is simple, production cost is low, pollutes less, product centella asiatica glucoside yield and purity advantages of higher, is suitable for suitability for industrialized production.
Description of drawings
Accompanying drawing is a kind of process flow diagram of preparing high-purity asiaticoside by solvent crystallization.
Embodiment
Below with embodiment processing method of the present invention is further described.Protection scope of the present invention is not subjected to the restriction of embodiment, and protection scope of the present invention is determined by claims.
The Herba Centellae total glycosides raw material is available from the natural pharmaceutcal corporation, Ltd of Guangxi Chang Zhou, and wherein the centella asiatica glucoside mass content is 30.0% after testing, and centella asiatica glucoside A and centella asiatica glucoside B mass content are closed and accounted for 49.5%.
Analysis condition used among the embodiment is as follows:
Thin-layer chromatography (TLC) analysis condition: silica gel G 254 thin plates, developping agent are propyl carbinol-ethyl acetate-water=4: 1: 5 (getting upper solution uses), and developer is 10% vitriol oil ethanolic soln.
High performance liquid chromatography (HPLC) analysis condition: Agilentl 100 liquid-phase chromatographic analysis systems, chromatographic column are Phenomenex C-18 column Synergi
TMFusion-RP 80A (4 μ, 150mm * 4.60mm ID), moving phase acetonitrile-water (50: 50), flow velocity 1mL/min, 30 ℃ of column temperatures, ultraviolet detection wavelength 205nm.
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 1000mL dimethyl formamide (100mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 5000mL acetone (solvent I add-on 5 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 24h after filtration, solid substance obtains 1.1g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 93%, and the centella asiatica glucoside yield is 31%.
Embodiment 2
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 200mL methyl alcohol (20mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 800mL water (solvent I add-on 4 times) in the Herba Centellae total glycosides solution and carry out crystallization in 30 ℃, obtain solid substance behind the 18h after filtration, solid substance obtains 2.2g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 92%, and the centella asiatica glucoside yield is 67%.
Embodiment 3
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 100mL dimethyl formamide (10mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 300mL water (solvent I add-on 3 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 12h after filtration, solid substance obtains 2.2g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 92%, and the centella asiatica glucoside yield is 68%.
Embodiment 4
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 50mL methyl alcohol (5mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 100mL acetonitrile (solvent I add-on 2 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 8h after filtration, solid substance obtains 2.6g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 94%, and the centella asiatica glucoside yield is 83%.
Embodiment 5
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 33mL dimethyl formamide (3.3mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 33mL acetone (solvent I add-on 1 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 6h after filtration, solid substance obtains 3.0g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 90%, and the centella asiatica glucoside yield is 91%.
Embodiment 6
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 25mL methyl alcohol (2.5mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 12.5mL ethyl acetate (solvent I add-on 0.5 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 6h after filtration, solid substance obtains 3.2g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 85%, and the centella asiatica glucoside yield is 92%.
Embodiment 7
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 25mL dimethyl formamide (2.5mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 150mL ethyl acetate (solvent I add-on 6 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 6h after filtration, solid substance obtains 2.9g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 84%, and the centella asiatica glucoside yield is 82%.
Embodiment 8
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 33mL methyl alcohol (3.3mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 200mL water (solvent I add-on 6 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 8h after filtration, solid substance obtains 2.7g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 92%, and the centella asiatica glucoside yield is 83%.
Embodiment 9
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 50mL dimethyl formamide (5mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 350mL water (solvent I add-on 7 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 10h after filtration, solid substance obtains 2.9g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 91%, and the centella asiatica glucoside yield is 89%.
Embodiment 10
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 100mL methyl alcohol (10mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 800mL water (solvent I add-on 8 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 10h after filtration, solid substance obtains 2.8g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 87%, and the centella asiatica glucoside yield is 81%.
Embodiment 11
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 200mL dimethyl formamide (20mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 1800mL ether (solvent I add-on 9 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 12h after filtration, solid substance obtains 3.3g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 83%, and the centella asiatica glucoside yield is 91%.
Embodiment 12
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 1000mL methyl alcohol (100mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 10000mL water (solvent I add-on 10 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 36h after filtration, solid substance obtains 1.7g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 80%, and the centella asiatica glucoside yield is 45%.
Embodiment 13
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 200mL methyl alcohol (20mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 800mL acetone (solvent I add-on 4 times) in the Herba Centellae total glycosides solution and under ice-water bath, carry out crystallization, obtain solid substance behind the 12h after filtration, solid substance obtains 2.2g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 92%, and the centella asiatica glucoside yield is 67%.
Embodiment 14
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 100mL dimethyl formamide (10mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 300mL acetone (solvent I add-on 3 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 10h after filtration, solid substance obtains 2.2g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 92%, and the centella asiatica glucoside yield is 68%.
Embodiment 15
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 33mL dimethyl formamide (3.3mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 33mL acetonitrile (solvent I add-on 1 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 4h after filtration, solid substance obtains 3g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 90%, and the centella asiatica glucoside yield is 91%.
Embodiment 16
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 25mL methyl alcohol (2.5mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 12.5mL acetonitrile (solvent I add-on 0.5 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 24h after filtration, solid substance obtains 3.2g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 85%, and the centella asiatica glucoside yield is 92%.
Embodiment 17
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 33mL methyl alcohol (3.3mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 200mL ethyl acetate (solvent I add-on 6 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 18h after filtration, solid substance obtains 2.7g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 92%, and the centella asiatica glucoside yield is 83%.
Embodiment 18
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 50mL dimethyl formamide (5mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 350mL ethyl acetate (solvent I add-on 7 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 12h after filtration, solid substance obtains 2.9g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 91%, and the centella asiatica glucoside yield is 89%.
Embodiment 19
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 100mL methyl alcohol (10mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 800mL ether (solvent I add-on 8 times) in the Herba Centellae total glycosides solution and carry out crystallization in 40 ℃, obtain solid substance behind the 14h after filtration, solid substance obtains 2.8g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 87%, and the centella asiatica glucoside yield is 81%.
Embodiment 20
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 1000mL dimethyl formamide (100mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 3000mL ether (solvent I add-on 3 times) in the Herba Centellae total glycosides solution and carry out crystallization in 45 ℃, obtain solid substance behind the 24h after filtration, solid substance obtains 1.4g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 73%, and the centella asiatica glucoside yield is 35%.
Embodiment 21
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 100mL dimethyl formamide (10mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 300mL acetone (solvent I add-on 3 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 8h after filtration, solid substance obtains 2.2g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 92%, and the centella asiatica glucoside yield is 68%.
The 2.9g centella asiatica glucoside product that obtains is added in the beaker, add the 30mL dimethyl formamide, the dissolving back adds 90mL acetone and carry out secondary crystal under room temperature, obtains solid substance behind the 8h after filtration, and solid substance obtains 1.8g centella asiatica glucoside product after vacuum-drying.Detect through HPLC, purity is 96%, and the centella asiatica glucoside total recovery is 59%.
Embodiment 22
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 33mL methyl alcohol (3.3mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 200mL water (solvent I add-on 6 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 12h after filtration, solid substance obtains 2.7g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 92%, and the centella asiatica glucoside yield is 83%.
The 2.8g centella asiatica glucoside product that obtains is added in the beaker, add 10mL methyl alcohol, the dissolving back adds 60mL water and carry out secondary crystal under room temperature, obtains solid substance behind the 12h after filtration, and solid substance obtains 2.2g centella asiatica glucoside product after vacuum-drying.Detect through HPLC, purity is 96%, and the centella asiatica glucoside total recovery is 69%.
Embodiment 23
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 33mL methyl alcohol (3.3mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 200mL ethyl acetate (solvent I add-on 6 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 12h after filtration, solid substance obtains 2.7g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 92%, and the centella asiatica glucoside yield is 83%.
The 2.7g centella asiatica glucoside product that obtains is added in the beaker, add 9mL methyl alcohol, the dissolving back adds the 54mL ethyl acetate and carry out secondary crystal under room temperature, obtains solid substance behind the 12h after filtration, and solid substance obtains 2.1g centella asiatica glucoside product after vacuum-drying.Detect through HPLC, purity is 97%, and the centella asiatica glucoside total recovery is 66%.
Embodiment 24
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 1000mL dimethyl formamide (100mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 3000mL ether (solvent I add-on 3 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 12h after filtration, solid substance obtains 3.4g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 80%, and the centella asiatica glucoside yield is 90%.
The 3.4g centella asiatica glucoside product that obtains is added in the beaker, add the 340mL dimethyl formamide, the dissolving back adds the 1020mL ether and carry out secondary crystal under room temperature, obtains solid substance behind the 12h after filtration, and solid substance obtains 2.4g centella asiatica glucoside product after vacuum-drying.Detect through HPLC, purity is 97%, and the centella asiatica glucoside total recovery is 85%.
Embodiment 25
Get 10g Herba Centellae total glycosides raw material and add in the beaker, add 50mL methyl alcohol (5mL solvent I/g Herba Centellae total glycosides), the dissolving after-filtration obtains Herba Centellae total glycosides solution; Add 100mL acetonitrile (solvent I add-on 2 times) in the Herba Centellae total glycosides solution and under room temperature, carry out crystallization, obtain solid substance behind the 12h after filtration, solid substance obtains 2.6g centella asiatica glucoside product after vacuum-drying, detect through HPLC, purity is 94%, and the centella asiatica glucoside yield is 83%.
The 2.6g centella asiatica glucoside product that obtains is added in the beaker, add 15mL methyl alcohol, the dissolving back adds the 105mL acetonitrile and carry out secondary crystal under room temperature, obtains solid substance behind the 12h after filtration, and solid substance obtains 2.3g centella asiatica glucoside product after vacuum-drying.Detect through HPLC, purity is 97%, and the centella asiatica glucoside total recovery is 77%.
Claims (6)
1. the technology of a preparing high-purity asiaticoside by solvent crystallization is characterized in that comprising the steps:
1) Herba Centellae total glycosides carries out solid-liquid separation after dissolving with solvent I, obtains Herba Centellae total glycosides solution;
2) add solvent II in the Herba Centellae total glycosides solution and carry out crystallization, obtain solid substance and crystalline mother solution two portions then after solid-liquid separation, last solid substance obtains the high-purity asiaticoside product after vacuum-drying.
2. the technology of a kind of preparing high-purity asiaticoside by solvent crystallization according to claim 1 is characterized in that solvent I is methyl alcohol or dimethyl formamide in the described step 1).
3. the technology of a kind of preparing high-purity asiaticoside by solvent crystallization according to claim 1, the add-on that it is characterized in that solvent I in the described step 1) is 2.5～100mL/g Herba Centellae total glycosides.
4. the technology of a kind of preparing high-purity asiaticoside by solvent crystallization according to claim 1 is characterized in that described step 1) and step 2) in solid-liquid separating method for filtering or centrifugal.
5. the technology of a kind of preparing high-purity asiaticoside by solvent crystallization according to claim 1 is characterized in that described step 2) in solvent II be acetone, acetonitrile, ether, ethyl acetate or water.
6. the technology of a kind of preparing high-purity asiaticoside by solvent crystallization according to claim 1 is characterized in that described step 2) in the add-on of solvent II be 0.5～10 times of solvent I add-on.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101983966A (en) * | 2010-11-19 | 2011-03-09 | 浙江大学 | Process for simultaneously preparing asiaticoside and madecassoside from low asiaticoside content total glycosides |
| CN102114063A (en) * | 2011-01-29 | 2011-07-06 | 桂林普兰德生物科技有限公司 | Method for extracting and separating asiaticoside by countercurrent extraction combined with membrane separation |
| CN108395464A (en) * | 2017-02-08 | 2018-08-14 | 桂林三金药业股份有限公司 | A method of preparing asiaticosid, madecassoside and Asaiticoside B from centella |
| CN112773745A (en) * | 2021-02-06 | 2021-05-11 | 广州贝塔健康生物科技有限公司 | Preparation method of asiaticoside extract and application of asiaticoside extract in cosmetics |
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| EP0383171A3 (en) * | 1989-02-11 | 1991-07-24 | Hoechst Aktiengesellschaft | 2,3,23-trihydroxy-urs-12-ene derivatives for treating cognitive disorders |
| CN1194154A (en) * | 1997-03-24 | 1998-09-30 | 东国制药株式会社 | Asiaticoside of self asiatic and hydroxy-asiaticoside and carboxy-asiaticoside water soluble extract and its separating method |
| CN1211098C (en) * | 2001-05-29 | 2005-07-20 | 中国人民解放军第二军医大学 | Prepn process and new use of general asiaticoside |
| FR2848117B1 (en) * | 2002-12-10 | 2006-08-04 | Roche Consumer Health Ltd | PROCESS FOR THE PREPARATION OF AN EXTRACT OF CENTELLA ASIATICA RICH IN MADECASSOSIDE AND TERMINOLOSIDE |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101983966A (en) * | 2010-11-19 | 2011-03-09 | 浙江大学 | Process for simultaneously preparing asiaticoside and madecassoside from low asiaticoside content total glycosides |
| CN101983966B (en) * | 2010-11-19 | 2012-08-15 | 浙江大学 | Process for simultaneously preparing asiaticoside and madecassoside from low asiaticoside content total glycosides |
| CN102114063A (en) * | 2011-01-29 | 2011-07-06 | 桂林普兰德生物科技有限公司 | Method for extracting and separating asiaticoside by countercurrent extraction combined with membrane separation |
| CN102114063B (en) * | 2011-01-29 | 2012-05-23 | 桂林普兰德生物科技有限公司 | Method for extracting and separating asiaticoside by countercurrent extraction combined with membrane separation |
| CN108395464A (en) * | 2017-02-08 | 2018-08-14 | 桂林三金药业股份有限公司 | A method of preparing asiaticosid, madecassoside and Asaiticoside B from centella |
| CN112773745A (en) * | 2021-02-06 | 2021-05-11 | 广州贝塔健康生物科技有限公司 | Preparation method of asiaticoside extract and application of asiaticoside extract in cosmetics |
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| CN101407536B (en) | 2011-05-18 |
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