CN1144810C - Extraction process of rhodiola root glycoside - Google Patents
Extraction process of rhodiola root glycoside Download PDFInfo
- Publication number
- CN1144810C CN1144810C CNB011289821A CN01128982A CN1144810C CN 1144810 C CN1144810 C CN 1144810C CN B011289821 A CNB011289821 A CN B011289821A CN 01128982 A CN01128982 A CN 01128982A CN 1144810 C CN1144810 C CN 1144810C
- Authority
- CN
- China
- Prior art keywords
- organic solvent
- rhodioloside
- product
- filter
- extraction process
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to a process for extracting salidroside. The rhizomes of herba rhodiolae are crushed, are roughly extracted for 4 to 18 hours at a temperature of 60 to 110 DEG C by using a hydrophilic organic solvent which is 4 to 20 times the volume of the rhizomes, and are filtered, and a filtrate is concentrated and dried to obtain a product roughly extracted; the product roughly extracted is dissolved for 1 to 8 hours at a temperature of 20 to 120 DEG C in a lipophilic organic solvent which is 4 to 20 times the volume of the product roughly extracted, and is filtered, and a filtrate is concentrated and dried to obtain an intermediate body of the salidroside. The intermediate body of the salidroside is dissolved in an organic solvent which is 4 to 10 times the volume of the intermediate body, and is filtered by chromatographic columns at a temperature of 65 to 80 DEG C, and 0.1 to 0.3% of active carbon is added to a transmission liquid at a temperature of 85 to 100 DEG C so as to carry out refinement; the transmission liquid is filtered when the transmission is hot, and the filtrate is concentrated so as to precipitate crystal which is filtered to obtain a refined product. The present invention has the characteristics of simple manufacturing process, stepwise operation, low cost and high product purity.
Description
Technical field
The invention belongs to the extraction process field of medicine, specifically is a kind of extraction process of rhodioloside.
Background technology
Root of Kirilow Rhodiola is a kind of herbal medicine that is distributed in the Yunnan Province of China northwestward, Tibet region, and it has the function of promoting blood circulation and stopping pain, removing heat from the lung to relieve cough, is mainly used in treatment hemoptysis, spitting of blood, pneumonia cough, women leukorrhea, wound, burn and scald etc.Rhodioloside is the effective constituent that mainly contains of rhodiola plant.Rhodioloside (salidroside) generally is to extract from Crassulaceae plant Root of Kirilow Rhodiola Rhodiola cra (PrainexHamet) Fu rhizome.Generally be directly to make capsule after Root of Kirilow Rhodiola rhizome drying, the pulverizing in the prior art, or make oral liquid medicinal extract.This product is except that multiple glucoside of Root of Kirilow Rhodiola and glucoside unit, also has the mixing system of fragrant element, fatty oils, volatile oil, amino acid, inorganic elements, triterpenes sterol, fiber, albumen, pigment sugar.
Summary of the invention
The objective of the invention is in order to remedy the deficiency of prior art, for people provide a kind of extraction process of rhodioloside, this technology is simple, the substep operation, and cost is low, the product purity height.
The objective of the invention is to realize by following technical proposals.
The extraction process of rhodioloside of the present invention is to adopt following step:
The Root of Kirilow Rhodiola rhizome is pulverized, slightly carried the Root of Kirilow Rhodiola rhizome with hydrophilic organic solvent: the weight ratio of hydrophilic organic solvent=1: 4～20, temperature is controlled at 60～110 ℃, and the time is 4～18 hours, filtered while hot, remove filter residue, concentrating filter liquor gets solids, and drying is for slightly carrying product; To slightly carry product further extracts with the lipotropy organic solvent, slightly carry product: the weight ratio of lipotropy organic solvent=1: 4～20, dissolved 1～8 hour, temperature is 20 ℃～120 ℃, is cooled to room temperature, filters, remove filter residue, filtrate is concentrated,, obtain the rhodioloside intermediate in oven dry below 80 ℃; The rhodioloside intermediate is dissolved in the organic solvent, the rhodioloside intermediate: the weight ratio of organic solvent=1: 4～10, under 65～80 ℃, filter through chromatography column; See through to add in the liquid and see through liquid and weigh 0.1～0.3% gac and make with extra care, be heated to 85～100 ℃, filtered while hot, concentrated filtrate is separated out crystallization, filter purified product, filtrate is reclaimed.
In the such scheme, purified product gets rid of filter with whizzer, and the filter limit is got rid of with 50%～95% organic solvent washing in the limit, and is dry below 80 ℃, must product.
In the such scheme, hydrophilic organic solvent is methyl alcohol, ethanol, propyl carbinol, Virahol, acetone, acetic acid, acetic anhydride, propylene glycol, glycerol, vinyl acetic monomer, N-BUTYL ACETATE, dimethyl formamide, N,N-DIMETHYLACETAMIDE.
In the such scheme, the lipotropy organic solvent is sherwood oil, ether, hexanaphthene, pimelinketone, meta-aminotoluene, Tetrabenzene methane, benzene,toluene,xylene, solvent oil, methylene dichloride, trichloromethane, tetracol phenixin.
In the such scheme, organic solvent is methyl alcohol, ethanol, vinyl acetic monomer, N-BUTYL ACETATE, propyl carbinol, Virahol, dimethyl formamide, N,N-DIMETHYLACETAMIDE, hexanaphthene, pimelinketone, acetic acid, acetic anhydride.
In the such scheme, chromatography column is wide aperture resin, resin anion(R.A), resin cation (R.C.), silica gel, polymeric amide, sephadex column.
In the extraction process of rhodioloside of the present invention, slightly carry with hydrophilic organic solvent and can remove fiber and the gentle matter of part; Further extract with the lipotropy organic solvent again, can remove impurity such as albumen, tannin, volatile oil, fatty oils; Filter through chromatography column, can remove water-soluble impurity; Again through absorbent charcoal fine purification, organic solvent washing, the content of rhodioloside can reach more than 98% in the product that obtains.
So it is simple that the present invention has technology, the substep operation, cost is low, the characteristics that product purity is high.
Embodiment
Be embodiments of the invention below, but the present invention is not limited only to described embodiment.
Embodiment one
100 gram Root of Kirilow Rhodiola rhizomes are pulverized, slightly carry with hydrophilic organic solvent, Root of Kirilow Rhodiola rhizome: the weight ratio of hydrophilic organic solvent=1: 4, hydrophilic organic solvent is a methyl alcohol, and temperature is controlled at 60 ℃, and the time is 4 hours, filtered while hot, remove filter residue, concentrating filter liquor gets solids, and drying is for slightly carrying product; To slightly carry product further extracts with the lipotropy organic solvent, slightly carry product: the weight ratio of lipotropy organic solvent=1: 4, the lipotropy organic solvent is a sherwood oil, dissolved 8 hours, temperature is 20 ℃, filters, remove filter residue, solution is concentrated,, obtain the rhodioloside intermediate in oven dry below 80 ℃; The rhodioloside intermediate is dissolved in the organic solvent, the rhodioloside intermediate: the weight ratio of organic solvent=1: 4, organic solvent are methyl alcohol, filter through chromatography column under 65 ℃, and chromatography column is a silicagel column; See through to add in the liquid and see through liquid and weigh 0.1% gac and make with extra care, be heated to 85 ℃, filtered while hot, concentrated filtrate is separated out crystallization, filter purified product, filtrate is reclaimed.
Embodiment two
100 gram Root of Kirilow Rhodiola rhizomes are pulverized, slightly carry with hydrophilic organic solvent, Root of Kirilow Rhodiola rhizome: the weight ratio of hydrophilic organic solvent=1: 20, hydrophilic organic solvent is an ethanol, and temperature is controlled at 75 ℃, and the time is 18 hours, filtered while hot, remove filter residue, concentrating filter liquor gets solids, and drying is for slightly carrying product; To slightly carry product further extracts with the lipotropy organic solvent, slightly carry product: the weight ratio of lipotropy organic solvent=1: 20, the lipotropy organic solvent is a toluene, dissolves 1 hour, and temperature is 80 ℃, be cooled to room temperature, filter, remove filter residue, solution is concentrated, in oven dry below 80 ℃, obtain the rhodioloside intermediate; The rhodioloside intermediate is dissolved in the organic solvent, the rhodioloside intermediate: the weight ratio of organic solvent=1: 10, organic solvent are vinyl acetic monomers, filter through chromatography column under 80 ℃, and chromatography column is the wide aperture resin column; See through to add in the liquid and see through liquid and weigh 0.3% gac and make with extra care, be heated to 100 ℃, filtered while hot, concentrated filtrate is separated out crystallization, filter purified product, filtrate is reclaimed.Purified product gets rid of filter with whizzer, and the filter limit is got rid of with the washing of 95% vinyl acetic monomer in the limit, and is dry below 80 ℃, must product.
Embodiment three
100 gram Root of Kirilow Rhodiola rhizomes are pulverized, slightly carry with hydrophilic organic solvent, Root of Kirilow Rhodiola rhizome: the weight ratio of hydrophilic organic solvent=1: 10, hydrophilic organic solvent is a propyl carbinol, and temperature is controlled at 110 ℃, and the time is 10 hours, filtered while hot, remove filter residue, concentrating filter liquor gets solids, and drying is for slightly carrying product; To slightly carry product further extracts with the lipotropy organic solvent, slightly carry product: the weight ratio of lipotropy organic solvent=1: 8, the lipotropy organic solvent is a solvent oil, dissolves 2 hours, and temperature is 120 ℃, be cooled to room temperature, filter, remove filter residue, solution is concentrated, in oven dry below 80 ℃, obtain the rhodioloside intermediate; The rhodioloside intermediate is dissolved in the organic solvent, the rhodioloside intermediate: the weight ratio of organic solvent=1: 8, organic solvent are Virahols, filter through chromatography column under 80 ℃, and chromatography column is a sephadex column; See through to add in the liquid and see through liquid and weigh 0.3% gac and make with extra care, be heated to 85 ℃, filtered while hot, concentrated filtrate is separated out crystallization, filter purified product, filtrate is reclaimed.Purified product gets rid of filter with whizzer, and the filter limit is got rid of with 50% washed with isopropyl alcohol in the limit, and is dry below 80 ℃, must product.
Embodiment four
100 gram Root of Kirilow Rhodiola rhizomes are pulverized, slightly carry with hydrophilic organic solvent, Root of Kirilow Rhodiola rhizome: the weight ratio of hydrophilic organic solvent=1: 14, hydrophilic organic solvent is an acetone, and temperature is controlled at 70 ℃, and the time is 12 hours, filtered while hot, remove filter residue, concentrating filter liquor gets solids, and drying is for slightly carrying product; To slightly carry product further extracts with the lipotropy organic solvent, slightly carry product: the weight ratio of lipotropy organic solvent=1: 10, the lipotropy organic solvent is a methylene dichloride, dissolves 4 hours, and temperature is 80 ℃, be cooled to room temperature, filter, remove filter residue, solution is concentrated, in oven dry below 80 ℃, obtain the rhodioloside intermediate; The rhodioloside intermediate is dissolved in the organic solvent, the rhodioloside intermediate: the weight ratio of organic solvent=1: 6, organic solvent are propyl carbinols, filter through chromatography column under 80 ℃, and chromatography column is a yin, yang ion exchange resin post; See through to add in the liquid and see through liquid and weigh 0.2% gac and make with extra care, be heated to 100 ℃, filtered while hot, concentrated filtrate is separated out crystallization, filter purified product, filtrate is reclaimed.
Embodiment five
100 gram Root of Kirilow Rhodiola rhizomes are pulverized, slightly carry with hydrophilic organic solvent, Root of Kirilow Rhodiola rhizome: the weight ratio of hydrophilic organic solvent=1: 8, hydrophilic organic solvent is a Virahol, and temperature is controlled at 100 ℃, and the time is 6 hours, filtered while hot, remove filter residue, concentrating filter liquor gets solids, and drying is for slightly carrying product; To slightly carry product further extracts with the lipotropy organic solvent, slightly carry product: the weight ratio of lipotropy organic solvent=1: 12, the lipotropy organic solvent is a dimethylbenzene, dissolves 2 hours, and temperature is 120 ℃, be cooled to room temperature, filter, remove filter residue, solution is concentrated, in oven dry below 80 ℃, obtain the rhodioloside intermediate; The rhodioloside intermediate is dissolved in the organic solvent, the rhodioloside intermediate: the weight ratio of organic solvent=1: 4, organic solvent are ethanol, filter through chromatography column under 80 ℃, and chromatography column is a polyamide column; See through to add in the liquid and see through liquid and weigh 0.3% gac and make with extra care, be heated to 85 ℃, filtered while hot, concentrated filtrate is separated out crystallization, filter purified product, filtrate is reclaimed.Purified product gets rid of filter with whizzer, and the filter limit is got rid of with 90% washing with alcohol in the limit, and is dry below 80 ℃, must product.
Embodiment six
100 gram Root of Kirilow Rhodiola rhizomes are pulverized, slightly carry with hydrophilic organic solvent, Root of Kirilow Rhodiola rhizome: the weight ratio of hydrophilic organic solvent=1: 14, hydrophilic organic solvent is an ethanol, and temperature is controlled at 75 ℃, and the time is 12 hours, filtered while hot, remove filter residue, concentrating filter liquor gets solids, and drying is for slightly carrying product; To slightly carry product further extracts with the lipotropy organic solvent, slightly carry product: the weight ratio of lipotropy organic solvent=1: 10, the lipotropy organic solvent is a sherwood oil, dissolves 6 hours, and temperature is 80 ℃, be cooled to room temperature, filter, remove filter residue, solution is concentrated, in oven dry below 80 ℃, obtain the rhodioloside intermediate; The rhodioloside intermediate is dissolved in the organic solvent, the rhodioloside intermediate: the weight ratio of organic solvent=1: 5, organic solvent are N-BUTYL ACETATEs, filter through chromatography column under 80 ℃, and chromatography column is the wide aperture resin column; See through to add in the liquid and see through liquid and weigh 0.3% gac and make with extra care, be heated to 100 ℃, filtered while hot, concentrated filtrate is separated out crystallization, filter purified product, filtrate is reclaimed.Purified product gets rid of filter with whizzer, and the filter limit is got rid of with 70% methanol wash in the limit, and is dry below 80 ℃, must product.
Embodiment seven
Hydrophilic organic solvent is a propylene glycol, and the lipotropy organic solvent is a pimelinketone, the organic solvent dimethyl formamide, and all the other are with embodiment six.
Embodiment eight
Hydrophilic organic solvent is an acetic acid, and the lipotropy organic solvent is a meta-aminotoluene, organic solvent acetic acid, and all the other are with embodiment six.
Embodiment nine
Hydrophilic organic solvent is a vinyl acetic monomer, and the lipotropy organic solvent is a Tetrabenzene methane, the organic solvent hexanaphthene, and all the other are with embodiment six.
Claims (6)
1. the extraction process of rhodioloside, it is characterized in that the Root of Kirilow Rhodiola rhizome is pulverized, slightly carry with hydrophilic organic solvent, the Root of Kirilow Rhodiola rhizome: the weight ratio of hydrophilic organic solvent=1: 4～20, temperature are controlled at 60～110 ℃, and the time is 4～18 hours, filtered while hot, remove filter residue, concentrating filter liquor gets solids, and drying is for slightly carrying product; To slightly carry product further extracts with the lipotropy organic solvent, slightly carry product: the weight ratio of lipotropy organic solvent=1: 4～20, dissolved 1～8 hour, temperature is 20 ℃～120 ℃, is cooled to room temperature, filters, remove filter residue, filtrate is concentrated,, obtain the rhodioloside intermediate in oven dry below 80 ℃; The rhodioloside intermediate is dissolved in the organic solvent, the rhodioloside intermediate: the weight ratio of organic solvent=1: 4～10, under 65～80 ℃, filter through chromatography column; See through to add in the liquid and see through liquid and weigh 0.1～0.3% gac and make with extra care, be heated to 85～100 ℃, filtered while hot, concentrated filtrate is separated out crystallization, filter purified product, filtrate is reclaimed.
2. the extraction process of rhodioloside according to claim 1 is characterized in that purified product gets rid of filter with whizzer, and the filter limit is got rid of with 50%～95% organic solvent washing in the limit, and is dry below 80 ℃, must product.
3. the extraction process of rhodioloside according to claim 1 and 2 is characterized in that hydrophilic organic solvent is methyl alcohol, ethanol, propyl carbinol, Virahol, acetone, acetic acid, acetic anhydride, propylene glycol, glycerol, vinyl acetic monomer, N-BUTYL ACETATE, dimethyl formamide, N,N-DIMETHYLACETAMIDE.
4. the extraction process of rhodioloside according to claim 1 and 2 is characterized in that the lipotropy organic solvent is sherwood oil, ether, hexanaphthene, pimelinketone, meta-aminotoluene, Tetrabenzene methane, benzene,toluene,xylene, solvent oil, methylene dichloride, trichloromethane, tetracol phenixin.
5. the extraction process of rhodioloside according to claim 1 and 2 is characterized in that organic solvent is methyl alcohol, ethanol, vinyl acetic monomer, N-BUTYL ACETATE, propyl carbinol, Virahol, dimethyl formamide, N,N-DIMETHYLACETAMIDE, hexanaphthene, pimelinketone, acetic acid, acetic anhydride.
6. the extraction process of rhodioloside according to claim 1 and 2 is characterized in that chromatography column is wide aperture resin, resin anion(R.A), resin cation (R.C.), silica gel, polymeric amide, sephadex column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011289821A CN1144810C (en) | 2001-10-19 | 2001-10-19 | Extraction process of rhodiola root glycoside |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011289821A CN1144810C (en) | 2001-10-19 | 2001-10-19 | Extraction process of rhodiola root glycoside |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1412196A CN1412196A (en) | 2003-04-23 |
| CN1144810C true CN1144810C (en) | 2004-04-07 |
Family
ID=4668790
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011289821A Expired - Fee Related CN1144810C (en) | 2001-10-19 | 2001-10-19 | Extraction process of rhodiola root glycoside |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1144810C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101766670B (en) * | 2010-02-23 | 2012-05-23 | 上海应用技术学院 | Rhodiola rosea polyphenol microcapsule and preparation method |
| CN102391316B (en) * | 2011-10-11 | 2013-11-13 | 泸州医学院 | Disaccharide compound and separation and purification method thereof |
| CN102875614A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Method for preparing salidroside from rose roots |
| CN103351416A (en) * | 2013-08-02 | 2013-10-16 | 福建中医药大学 | New crystal form A of salidroside and preparation method thereof |
| CN104017036A (en) * | 2014-06-11 | 2014-09-03 | 福建中医药大学 | Novel crystal form of rhodioloside and preparation method of novel crystal form |
| CN106083949A (en) * | 2016-06-17 | 2016-11-09 | 延边大学 | A kind of method improving rhodioside extraction ratio |
-
2001
- 2001-10-19 CN CNB011289821A patent/CN1144810C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1412196A (en) | 2003-04-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101053589B (en) | Method for extracting active constituent from Tibetan capillary | |
| CN101830849B (en) | Method for preparing simplified high-purity bulleyaconitine A | |
| CN1228968A (en) | Production method for extracting flavonoid compound extract or powder from bamboo leaf | |
| CN101781279B (en) | Preparation method of grape seed procyanidin | |
| CN103435486A (en) | Novel method for preparing high-purity chlorogenic acid in honeysuckle | |
| CN112870236B (en) | Flavone effective part of abelmoschus manihot and preparation method and application thereof | |
| CN102351819A (en) | Extraction, purification and preparation method of high-purity salvianolic acid B | |
| CN103450298A (en) | Novel method for extracting baicalin from scutellaria baicalensis | |
| CN1144810C (en) | Extraction process of rhodiola root glycoside | |
| CN102349951A (en) | Preparation method of hawthorn leaf extract | |
| CN103505492B (en) | A kind of method using ultrafiltration to prepare high anti-oxidation value Radix Rhodiolae extract | |
| CN101348474A (en) | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem | |
| CN102093326B (en) | Method for extracting and refining ginkgo flavone from ginkgo leaves | |
| CN101040950A (en) | Method of preparing Ynxingchao dropping pills compound | |
| CN101538296A (en) | Active ingredients of camptosorus sibiricus, and extraction method and use of same | |
| CN101215307B (en) | Method for preparing hydroxyl carthamus tinctorius yellow color A | |
| CN1095364C (en) | Process for refining injection 'shuanghuanglian' | |
| CN111808060B (en) | Method for extracting total coumarin from rhodiola rosea | |
| CN1687092A (en) | General glycoside extractive of xanthium and preparation method | |
| CN1470510A (en) | Epi-nutgall catechin gallic acid ester monomer purifying process | |
| CN104825538A (en) | Extraction method of lavender total flavone | |
| CN1513848A (en) | Method of extracting phenolic components from chinese medicine red sage root and its freeze dried powder injection agent | |
| CN110156601B (en) | Method for preparing high-purity chlorogenic acid from stevia rebaudiana | |
| CN107648305B (en) | Preparation method of extract with alpha-glucosidase inhibition effect | |
| CN100344298C (en) | Method for preparing eupatorium powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |