CN110179841A - A kind of industrial extraction method of high level of water soluble asiaticoside - Google Patents
A kind of industrial extraction method of high level of water soluble asiaticoside Download PDFInfo
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- CN110179841A CN110179841A CN201910588539.6A CN201910588539A CN110179841A CN 110179841 A CN110179841 A CN 110179841A CN 201910588539 A CN201910588539 A CN 201910588539A CN 110179841 A CN110179841 A CN 110179841A
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- asiaticoside
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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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- 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
- A61K2236/30—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
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated 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
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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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
A kind of industrial extraction method of high level of water soluble asiaticoside, refluxing extraction is carried out using alkaline ethanol first, concentration, water is heavy, takes supernatant to be enriched with macroreticular resin, active carbon decoloring, finally use ethyl acetate recrystallization technology, the high level of water soluble asiaticoside that content is 95% or more is extracted, which has better water solubility, and purposes is more extensive.The advantages such as this process step simple, low energy consumption, high conversion rate, DNA purity height simultaneously, can be used in actual industrial production.
Description
Technical field
The present invention relates to technical field of extraction of Chinese traditional medicine more particularly to a kind of industrialization of high level of water soluble asiaticoside
Extracting method.
Background technique
Centella, Chinese medicine name are that the drying of umbelliferae centella [Centella asiatica (L.) UrBan] is complete
Grass, bitter, acrid, cold have clearing heat and promoting diuresis, and the efficacy of removing toxicity for detumescence effect is usually used in jaundice with damp-heat pathogen, heatstroke diarrhea, stone drenchs blood, carbuncle swells
Sore, injury from falling down.
The complex chemical composition of centella mainly has triterpenes, flavonoids, volatile oil, polyyne alkenes etc., asiatic centella total
Glycosides is main ingredient in Gotu Kola P.E, mainly by material compositions such as asiaticosid, madecassoside, Asaiticoside Bs.
It is widely used in medicine, cosmetic field；Wherein, the knot of asiaticosid (1), madecassoside (2), Asaiticoside B (3)
Structure formula is as follows:
Industrial abstract asiaticoside, because ratio is not between the different gained asiaticoside content of technique, each ingredient
Together, especially impurity effect asiaticoside dissolved clarity in water, causes asiaticoside in application by office
Limit.
Summary of the invention
Technical problem solved by the invention is that the industrialization for providing a kind of high level of water soluble asiaticoside is extracted
Method, to solve the disadvantage in above-mentioned background technique.
Technical problem solved by the invention is realized using following technical scheme:
A kind of industrial extraction method of high level of water soluble asiaticoside, the specific steps are as follows:
1) appropriate centella is taken, with alcohol content 70%~80%, pH value for alkaline ethanol refluxing extraction 2~3 times of 8~9,
Cream is received in concentration, obtains a medicinal extract；
2) water is carried out to a medicinal extract to sink, take supernatant；
3) supernatant is enriched with using macroreticular resin, while is rinsed with water to color is light and obtains washing lotion, be in neutrality to washing lotion
When, then eluted with 70% ethyl alcohol 100L, collect eluent；
4) to eluent concentration, receipts cream, secondary medicinal extract is obtained, ethyl acetate and active carbon, reflux are added in secondary medicinal extract
Decoloration, filters, stands still for crystals, obtain crystal；
5) crystal is centrifuged, obtains solid content and the mother liquor for replacing ethyl acetate in equivalent step 4), then
Solid content is dried under reduced pressure to get high-purity water dissolubility asiaticoside.
In the present invention, in step 1), the alkaline ethanol dosage being added every time is 6~10 times of centella dosage.
In the present invention, in step 1), the medicinal extract density of concentration receives cream when being 1.15~1.35.
In the present invention, in step 2), the heavy water that 6~10 times of a medicinal extract volume amounts are added of water stands 18~24 hours.
In the present invention, in step 3), macroreticular resin model includes: HPD100, HPD200, D101.
In the present invention, in step 4), the medicinal extract density of eluent concentration receives cream when being 1.15~1.35.
In the present invention, in step 4), the ethyl acetate and 0.05 times of amount of 5 times of secondary medicinal extract amounts are added in secondary medicinal extract
Active carbon, reflux decoloration；Its ethyl acetate is using mother liquor equivalent substitution in step 5).
In the present invention, in step 4), crystallisation by cooling temperature is to be placed in -10 DEG C~10 DEG C.
In the present invention, in step 4), solid content be dried under reduced pressure temperature in 85 DEG C of temperature conditions hereinafter, vacuum degree be-
0.05MPa~-0.09MPa.
In the present invention, Diluted Alcohol is collected in the concentration process of step 1) and step 4), then is recycled through alcohol distillation column
After reuse.
The utility model has the advantages that the industrialization extractive technique that the present invention uses, makes asiaticoside content be up to 95% or more, effectively
Improve asiaticoside dissolved clarity in water；Meanwhile the etoh solvent and ethyl acetate used in production process can
It recycles and reuses, production cost is effectively reduced, reduce pollution of the solvent discharge to environment.
Detailed description of the invention
Fig. 1 is the flow chart of the present embodiment.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Conjunction is specifically illustrating, and the present invention is further explained.
In the examples below, centella is harvested by Guangxi, is calculated by dry product, (the C containing asiaticosid48H78O19) and hydroxyl
Base asiaticosid (C48H78O20) total amount be 3.1%；
Analysis condition used is as follows in embodiment:
A, according to high effective liquid chromatography for measuring
Chromatographic condition and system suitability: using octadecylsilane chemically bonded silica as filler, with acetonitrile -2mmol/
L betadex solution (24:76) is mobile phase, and Detection wavelength 205nm, number of theoretical plate should not be low by the calculating of asiaticosid peak
In 4000；
B, the preparation of reference substance solution: taking madecassoside reference substance and asiaticosid reference substance appropriate, accurately weighed,
Add methanol be made every 1ml respectively the solution containing 0.2mg to get；
C, the preparation of test solution: taking this product about 50mg, accurately weighed, sets in 50ml measuring bottle, methanol is added to make to dissolve, and
Be diluted to scale, shake up, filter, take subsequent filtrate to get；
D, measuring method: it is accurate respectively to draw reference substance solution and each 10 μ l of test solution, liquid chromatograph is injected, is surveyed
It is fixed to get.
Embodiment 1
It takes in centella 100kg investment multi-function extractor, the 70% alkaline ethanol 600L of pH=8, refluxing extraction 2 is added
It is secondary, 2 hours every time, then filtrate is merged to be concentrated into when heat surveys density 1.20 (60 DEG C) and receives cream, obtains a medicinal extract 25.6L；?
In medicinal extract plus water 160L water is heavy, stands 19 hours, takes supernatant, and pretreated 50kg pairs of D101 macroreticular resin using progress
Supernatant is enriched with, flow velocity 0.5BV/h, at the same be rinsed with water to color it is light washing lotion, when washing lotion is in neutrality, then with 70% second
Alcohol 100L is eluted with the flow velocity of 0.5BV/h, collects eluent, ethyl alcohol is recovered under reduced pressure, when being concentrated into heat survey density 1.20 (60 DEG C)
Cream is received, secondary medicinal extract 8.8L is obtained, ethyl acetate 44L and active carbon 440g, reflux decoloration 30min, mistake are added in secondary medicinal extract
Filter, filtrate is cooled to 2 DEG C, stands still for crystals 12 hours, is centrifuged, obtains solid content 1.25kg and a mother liquor, -0.07MPa~-
Solid content is dried under reduced pressure to get high-purity water dissolubility asiaticoside 1.11kg, yield under the conditions of 0.08MPa, 80 DEG C of temperature
1.11%, content 94.7%.
Embodiment 2
It takes in centella 100kg investment multi-function extractor, the 70% alkaline ethanol 600L of pH=8, refluxing extraction 2 is added
It is secondary, 2 hours every time, then filtrate is merged to be concentrated into when heat surveys density 1.21 (60 DEG C) and receives cream, obtains a medicinal extract 24.7L；?
In medicinal extract plus water 150L water is heavy, stands 20 hours, takes supernatant, and pretreated 50kg pairs of D101 macroreticular resin using progress
Supernatant is enriched with, flow velocity 0.5BV/h, at the same be rinsed with water to color it is light washing lotion, when washing lotion is in neutrality, then with 70% second
Alcohol 100L is eluted with the flow velocity of 0.5BV/h, collects eluent, ethyl alcohol is recovered under reduced pressure, when being concentrated into heat survey density 1.21 (60 DEG C)
Receive cream, obtain secondary medicinal extract 8.2L, in secondary medicinal extract be added embodiment 1 in be centrifuged after a mother liquor 37L, ethyl acetate 4L and
Active carbon 410g, reflux decoloration 30min, filtering, filtrate are cooled to 2 DEG C, stand still for crystals 12 hours, is centrifuged, obtains solid content
1.47kg and secondary mother liquid are dried under reduced pressure to get high-purity solid content under the conditions of -0.07MPa~-0.08MPa, 80 DEG C of temperature
Spend water-soluble asiaticoside 1.24kg, yield 1.24%, content 92.2%.
Embodiment 3
It takes in centella 100kg investment multi-function extractor, the 75% alkaline ethanol 600L of pH=8, refluxing extraction 2 is added
It is secondary, 2 hours every time, then filtrate is merged to be concentrated into when heat surveys density 1.20 (60 DEG C) and receives cream, obtains a medicinal extract 26.2L；?
In medicinal extract plus water 160L water is heavy, stands 20 hours, takes supernatant, and pretreated 50kg pairs of D101 macroreticular resin using progress
Supernatant is enriched with, flow velocity 0.5BV/h, at the same be rinsed with water to color it is light washing lotion, when washing lotion is in neutrality, then with 70% second
Alcohol 100L is eluted with the flow velocity of 0.5BV/h, collects eluent, ethyl alcohol is recovered under reduced pressure, when being concentrated into heat survey density 1.20 (60 DEG C)
Cream is received, secondary medicinal extract 8.9L is obtained, secondary mother liquid 38L, ethyl acetate 6.5L after being centrifuged in embodiment 2 are added in secondary medicinal extract
It is filtered with active carbon 445g, reflux decoloration 30min, filtrate is cooled to 2 DEG C, stands still for crystals 14 hours, is centrifuged, obtains solid content
1.52kg and three times mother liquor are dried under reduced pressure to get high-purity solid content under the conditions of -0.07MPa~-0.08MPa, 80 DEG C of temperature
Spend water-soluble asiaticoside 1.27kg, yield 1.27%, content 91.2%.
Embodiment 4
It takes in centella 100kg investment multi-function extractor, the 75% alkaline ethanol 600L of pH=8, refluxing extraction 2 is added
It is secondary, 2 hours every time, then filtrate is merged to be concentrated into when heat surveys density 1.20 (60 DEG C) and receives cream, obtains a medicinal extract 26.0L；?
In medicinal extract plus water 160L water is heavy, stands 21 hours, takes supernatant, and pretreated 50kg pairs of D101 macroreticular resin using progress
Supernatant is enriched with, flow velocity 0.5BV/h, be rinsed with water to color it is light washing lotion, when washing lotion is in neutrality, then with 70% ethyl alcohol
100L is eluted with the flow velocity of 0.5BV/h, collects eluent, ethyl alcohol is recovered under reduced pressure, and is concentrated into when heat surveys density 1.20 (60 DEG C) and is received
Cream obtains secondary medicinal extract 8.8L, and ethyl acetate 44L and active carbon 440g is added in secondary medicinal extract, and reflux decoloration 30min is filtered,
Filtrate is cooled to 2 DEG C, stands still for crystals 13 hours, centrifugation, obtain solid content 1.21kg and four mother liquors, -0.07MPa~-
Solid content is dried under reduced pressure to get high-purity water dissolubility asiaticoside 1.02kg, yield under the conditions of 0.08MPa, 80 DEG C of temperature
1.02%, content 95.1%.
Embodiment 5
It takes in centella 100kg investment multi-function extractor, the 75% alkaline ethanol 600L of pH=8, refluxing extraction 2 is added
It is secondary, 2 hours every time, then filtrate is merged to be concentrated into when heat surveys density 1.20 (60 DEG C) and receives cream, obtains a medicinal extract 25.5L；?
In medicinal extract plus water 160L water is heavy, stands 21 hours, takes supernatant, and pretreated 50kg pairs of D101 macroreticular resin using progress
Supernatant is enriched with, flow velocity 0.5BV/h, be rinsed with water to color it is light washing lotion, when washing lotion is in neutrality, then with 70% ethyl alcohol
100L is eluted with the flow velocity of 0.5BV/h, collects eluent, ethyl alcohol is recovered under reduced pressure, and is concentrated into when heat surveys density 1.20 (60 DEG C) and is received
Cream obtains secondary medicinal extract 8.7L, in secondary medicinal extract be added embodiment 4 in be centrifuged after four mother liquor 35L, ethyl acetate 8.5L and
Active carbon 435g, reflux decoloration 30min, filtering, filtrate are cooled to 2 DEG C, stand still for crystals 13 hours, is centrifuged, obtains solid content
1.35kg and five mother liquor is dried under reduced pressure to get high-purity solid content under the conditions of -0.07MPa~-0.08MPa, 80 DEG C of temperature
Spend water-soluble asiaticoside 1.23kg, yield 1.23%, content 93.2%.
Claims (10)
1. a kind of industrial extraction method of high level of water soluble asiaticoside, which is characterized in that specific step is as follows:
1) appropriate centella is taken, it is dense with alcohol content 70%~80%, alkaline ethanol refluxing extraction 2~3 times that pH value is 8~9
Cream is received in contracting, obtains a medicinal extract；
2) water is carried out to a medicinal extract to sink, take supernatant；
3) supernatant is enriched with using macroreticular resin, while is rinsed with water to color is light and obtains washing lotion, when washing lotion is in neutrality, then
It is eluted with 70% ethyl alcohol 100L, collects eluent；
4) to eluent concentration, receipts cream, secondary medicinal extract is obtained, ethyl acetate and active carbon are added in secondary medicinal extract, reflux is decolourized,
It filters, stand still for crystals, obtain crystal；
5) crystal is centrifuged, obtains solid content and the mother liquor for replacing ethyl acetate in equivalent step 4), then to solid
Shape object is dried under reduced pressure to get high-purity water dissolubility asiaticoside.
2. a kind of industrial extraction method of high level of water soluble asiaticoside according to claim 1, feature exist
In in step 1), the alkaline ethanol dosage being added every time is 6~10 times of centella dosage.
3. a kind of industrial extraction method of high level of water soluble asiaticoside according to claim 1, feature exist
In in step 1), the medicinal extract density of concentration receives cream when being 1.15~1.35.
4. a kind of industrial extraction method of high level of water soluble asiaticoside according to claim 1, feature exist
In in step 2), the heavy water that 6~10 times of a medicinal extract volume amounts are added of water stands 18~24 hours.
5. a kind of industrial extraction method of high level of water soluble asiaticoside according to claim 1, feature exist
In in step 3), macroreticular resin model includes: HPD100, HPD200, D101.
6. a kind of industrial extraction method of high level of water soluble asiaticoside according to claim 1, feature exist
In in step 4), the medicinal extract density of eluent concentration receives cream when being 1.15~1.35.
7. a kind of industrial extraction method of high level of water soluble asiaticoside according to claim 1, feature exist
In in step 4), ethyl acetate and 0.05 times of active carbon measured, the reflux that 5 times of secondary medicinal extract amounts are added in secondary medicinal extract are de-
Color；Its ethyl acetate is using mother liquor equivalent substitution in step 5).
8. a kind of industrial extraction method of high level of water soluble asiaticoside according to claim 1, feature exist
In in step 4), crystallisation by cooling temperature is to be placed in -10 DEG C~10 DEG C.
9. a kind of industrial extraction method of high level of water soluble asiaticoside according to claim 1, feature exist
In in step 4), solid content is dried under reduced pressure temperature in 85 DEG C of temperature conditions hereinafter, vacuum degree is -0.05MPa~-0.09MPa.
10. a kind of industrial extraction method of high level of water soluble asiaticoside according to claim 1, feature exist
In collecting Diluted Alcohol in the concentration process of step 1) and step 4), then reuse after alcohol distillation column recycles.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111285916A (en) * | 2020-02-14 | 2020-06-16 | 浏阳朗林生物科技有限公司 | Preparation method of centella asiatica extract with high content of total asiaticosides |
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| 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 |
| CN102617696A (en) * | 2012-03-16 | 2012-08-01 | 广州汉方现代中药研究开发有限公司 | Preparation method of asiaticoside |
| CN109320579A (en) * | 2018-10-30 | 2019-02-12 | 天峨县科学技术情报研究所 | The extracting method of Gotu Kola P.E |
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2019
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| 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 |
| CN101948501A (en) * | 2010-09-01 | 2011-01-19 | 桂林莱茵生物科技股份有限公司 | Preparation method of hydroxyl asiaticoside |
| CN102617696A (en) * | 2012-03-16 | 2012-08-01 | 广州汉方现代中药研究开发有限公司 | Preparation method of asiaticoside |
| CN109320579A (en) * | 2018-10-30 | 2019-02-12 | 天峨县科学技术情报研究所 | The extracting method of Gotu Kola P.E |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111285916A (en) * | 2020-02-14 | 2020-06-16 | 浏阳朗林生物科技有限公司 | Preparation method of centella asiatica extract with high content of total asiaticosides |
| CN111285916B (en) * | 2020-02-14 | 2021-07-02 | 浏阳朗林生物科技有限公司 | Preparation method of centella asiatica extract with high content of total asiaticosides |
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