CN101434534A - Preparation of salvianic acid A sodium pure product - Google Patents
Preparation of salvianic acid A sodium pure product Download PDFInfo
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- CN101434534A CN101434534A CN 200710166154 CN200710166154A CN101434534A CN 101434534 A CN101434534 A CN 101434534A CN 200710166154 CN200710166154 CN 200710166154 CN 200710166154 A CN200710166154 A CN 200710166154A CN 101434534 A CN101434534 A CN 101434534A
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Abstract
The invention discloses a preparation method of a pure product of Salvianic acid A sodium, which comprises processing steps: 1. salvia miltiorrhizae is extracted by a hydrothermal method, and an extracting solution is condensed, deposited in alcohol and filtered; 2. a filtrate is condensed, deposited in alcohol and filtered; 3. the filtrate is condensed, added with water and filtered, and the filtrate is put into a macroporous absorption resin column and washed by water; 4. after a water lotion is condensed, the step is carried out in accordance with step (5); or the water lotion is put into a polyamide column and washed by water, and after the water lotion is condensed, the step is carried out according to step (5); 5. the water lotion after condensation is mixed with silicon gel, dried, column-packed and eluted by an organic solvent, and then an eluent is collected, recovered to be dry to obtain dry paste; and 6. the dry paste is taken and dissolved by the organic solvent, and PH value is adjusted, and then the material is stood and crystallized; or the dry paste is taken and dissolved by a solvent, and then put into a Sephadex LH-20 column or reversed-phase silica gel column. The PH value is adjusted by the eluent, and standing and crystallizing are carried out. The Salvianic acid A sodium prepared by the method has purity of more than or equal to 98 percent (standardized by NICPBP in respect of standard substances). Furthermore, the method has low cost, less pollution to environment and easily industrialized production.
Description
Technical field
The preparation method who the present invention relates to extraction from salviamiltiorrhizabung, separates, makes with extra care Sodium Danshensu.
Background technology
The red sage root is a conventional Chinese medicine, and the beginning is stated from Shennong's Herbal, classifies as top grade.Chinese Pharmacopoeia (version in 2005) the regulation red sage root is the dry root and rhizome of labiate red sage root Salvia miltiorrhiza Bge..
Salvianic acidA is one of aqueous soluble active constituent in the red sage root, have many-sided pharmacological action [You Jingke, from Rong Bing, Jiang Ronghai, Chinese practical medical science, 2002; 4 (23)].1. 2. atherosclerosis protects liver cell, and 3. 4. anti-inflammatory and enhancing body immunity protect heart, 5. microcirculation improvement and anti-freezing, 6. diastole coronary artery, 7. anticoagulant, 8. hypoxia tolerance.
At present, the patent of preparation Sodium Danshensu mainly contains four:
(1) application number: 01126883.2 absorption with macroporous adsorbent resin, extraction again
(2) application number: 200510043608.3 earlier with weakly base resin absorption, uses the low-pole resin absorption again
(3) application number: 200410021414.9 ultrafiltration, organic solvent extraction, normal-phase chromatography separates
(4) application number: 200610117931.5 sour water ethanol-extracteds, cross macroporous adsorptive resins, cross polyamide column,
Or mistake Sephadex LH-20 post, MCI GEL CHP20P post, C
4, C
8Or C
18Bonding phase silicagel column.
These four Sodium Danshensus that patent is prepared, its purity does not reach 98%, and the patent that has is not suitable for suitability for industrialized production.
Method provided by the invention can make the purity of Sodium Danshensu reach 98% (middle inspection institute standard substance demarcate), be fit to suitability for industrialized production again, and cost is low, and environmental pollution is little.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, provide that a kind of cost is low, purity is high, yield is high, be easy to the preparation method of the Sodium Danshensu of suitability for industrialized production.
The preparation method of Sodium Danshensu of the present invention is to be carried with hydro-thermal by the red sage root substantially, alcohol precipitation, and macroporous adsorptive resins separates; Perhaps polyamide column separates, and silicagel column separates, Sephadex LH-20 post or oppositely silicagel column separation, and steps such as crystallization are formed.
The present invention is implemented by following technical proposals:
(a) red sage root is carried with hydro-thermal, and extracting solution concentrates, and adds the ethanol alcohol precipitation, filters;
(b) filtrate concentrates, and adds the ethanol alcohol precipitation, filters;
(c) filtrate concentrates, and adds water, filters, and macroporous adsorptive resins on the filtrate washes with water;
(d) after water lotion concentrated, (e) carried out set by step; Perhaps polyamide column on the water lotion washes with water, and is dense
After the shrink washing lotion, (e) carries out set by step;
(e) water lotion after concentrating is mixed silica gel, oven dry, and the dress post, with containing organic acid organic solvent wash-out, the collection elutriant is recycled to driedly, gets dry extract.
(f) get dried cream, use organic solvent dissolution, transfer pH value, place crystallization; Perhaps get dried cream, water, moisture or anhydrous methanol, moisture or anhydrous alcohol solution, last Sephadex LH-20 post or reverse phase silica gel post (Rp-2, Rp-8, Rp-18), water, moisture or anhydrous methanol, moisture or dehydrated alcohol are washed chromatographic column, collect elutriant, merge elutriant according to TLC, be recycled on a small quantity, add an amount of organic solvent, transfer pH value with appropriate alkaline liquor, place crystallization.
Wherein, in the step (a), boiling 2-4 times, each 4-8 hours, amount of water is 5-8 times of amounts of red sage root weight, and merging filtrate is concentrated in right amount, adds 95% ethanol, containing the alcohol amount to solution is 40-60%, places 6-24 hours (the best is 8-15 hours), filters;
In the step (b), filtrate is concentrated in right amount, adds 95% ethanol, and containing the alcohol amount to solution is 70-85%, places 6-24 hours (the best is 8-15 hours), filters;
In the step (c), filtrate is concentrated in right amount, adds 2-6 times of amounts of water (the best is 2-4 times of amounts), filters, and macroporous adsorptive resins on the filtrate washes with water;
In the step (d), after water lotion concentrated, (e) carried out set by step; Perhaps polyamide column on the water lotion washes with water, and after the condensed water washing lotion, (e) carries out set by step;
In the step (e), the water lotion after concentrating is mixed silica gel (60-400 order) (the best is 100-200 orders), oven dry (30-120 ℃) (the best is 50-70 ℃); Organic solvent is acetone, ethyl acetate, chloroform, and organic acid is formic acid and acetic acid;
In the step (f), get dried cream, with methyl alcohol or dissolve with ethanol, hydro-oxidation sodium, yellow soda ash, sodium bicarbonate aqueous solution transfer pH value to weakly alkaline, place crystallization; Perhaps get dried cream, with 5-95% (the best is 20-60%) methyl alcohol or aqueous ethanolic solution dissolving, last Sephadex LH-20 post or reverse phase silica gel post (Rp-2, Rp-8, Rp-18), with 5-95% (the best is 20-60%) methyl alcohol or ethanol aqueous wash chromatographic column, collect elutriant, merge elutriant according to TLC, be recycled on a small quantity, add an amount of methyl alcohol or ethanol, transfer pH value to weakly alkaline with sodium hydroxide, yellow soda ash or sodium bicarbonate aqueous solution, place crystallization.
The Sodium Danshensu of making according to method of the present invention, its purity can be used for treating coronary heart disease, stenocardia, chb hepatic fibrosis, atherosclerosis etc. more than or equal to 98% (middle inspection institute standard substance demarcation); Can be made into said formulation on any pharmaceutics, also can cooperate other medicines or component to make preparation together and use.Advantage of the present invention and characteristics
1, cost is low, and environmental pollution is little, is easy to suitability for industrialized production
(1) in the technology, a large amount of solvents that use are second alcohol and waters, can reclaim repeatedly and use.
(2) macroporous adsorbent resin and polymeric amide can use repeatedly.
(3) washing organic solvent that silicagel column uses can reclaim repeatedly and use.
(4) Sephadex LH-20 and reverse phase silica gel filler can use repeatedly, and eluent can reclaim repeatedly and use.
2, product purity height
With the Sodium Danshensu of method preparation of the present invention, its purity is more than or equal to 98%.Calculate with one point external standard method, standard substance are provided by the calibrating of Chinese biological goods.
Embodiment
Following each embodiment only is used to the present invention is described but not limitation of the present invention:
Embodiment one
The red sage root (individual sub-goods) 3kg adds poach 3 times, adds 7 times of amounts of water for the first time, boils 8 hours, and back secondary respectively adds 5 times of amounts of water, respectively boils 4 hours, filters, and merges three times filtrate; Be concentrated in right amount, be cooled to room temperature, add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 50%; After room temperature is placed 12 hours, to filter, filtrate is concentrated in right amount, is cooled to room temperature; Add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 80%, after room temperature is placed 12 hours, filters; Filtrate is concentrated in right amount, is cooled to room temperature, adds the water of 4 times of amounts, and the limit edged stirs, and places 1-2 hours, filters; Macroporous adsorptive resins on the filtrate (AB-8,800g), the water wash-out is collected elutriant, polyamide column on the elutriant (60-100 orders, 250g), the water wash-out is collected elutriant; Concentrate eluant is mixed silica gel 1000g (100-200 order) to an amount of, dries (65 ℃) to baking oven.Silica gel dress post, use ethyl acetate: formic acid (50:0.1) is washed silicagel column, and the collection elutriant is recycled to driedly, gets dry extract.Get dried cream, add dissolve with methanol, transfer pH value to weakly alkaline with sodium bicarbonate aqueous solution, place, crystallization gets Sodium Danshensu crystallization (98.85%).
Embodiment two
The red sage root (individual sub-goods) 3kg adds poach 3 times, adds 7 times of amounts of water for the first time, boils 8 hours, and back secondary respectively adds 5 times of amounts of water, respectively boils 4 hours, filters, and merges three times filtrate; Be concentrated in right amount, be cooled to room temperature, add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 50%; After room temperature is placed 12 hours, to filter, filtrate is concentrated in right amount, is cooled to room temperature; Add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 80%, after room temperature is placed 12 hours, filters; Filtrate is concentrated in right amount, is cooled to room temperature, adds the water of 4 times of amounts, and the limit edged stirs, and places 1-2 hours, filters; Macroporous adsorptive resins on the filtrate (AB-8,800g), the water wash-out is collected elutriant; Concentrate eluant is mixed silica gel 1000g (100-200 order) to an amount of, dries (65 ℃) to baking oven.Silica gel dress post, use ethyl acetate: formic acid (50:0.1) is washed silicagel column, and the collection elutriant is recycled to driedly, gets dry extract.Get dried cream, add dissolve with methanol, transfer pH value to weakly alkaline with sodium bicarbonate aqueous solution, place, crystallization gets Sodium Danshensu crystallization (98.25%).
Embodiment three
The red sage root (medicine materical crude slice) 3kg adds poach 3 times, adds 6 times of amounts of water for the first time, boils 6 hours, and back secondary respectively adds 5 times of amounts of water, respectively boils 4 hours, filters, and merges three times filtrate; Be concentrated in right amount, be cooled to room temperature, add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 40%; After room temperature is placed 12 hours, to filter, filtrate is concentrated in right amount, is cooled to room temperature; Add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 70%, after room temperature is placed 12 hours, filters; Filtrate is concentrated in right amount, is cooled to room temperature, adds the water of 3 times of amounts, and the limit edged stirs, and places 1-2 hours, filters; Macroporous adsorptive resins on the filtrate (D101,800g), the water wash-out is collected elutriant, polyamide column on the elutriant (60-100 orders, 250g), the water wash-out is collected elutriant; Concentrate eluant is mixed silica gel 1000g (100-200 order) to an amount of, dries (65 ℃) to baking oven.Silica gel dress post, use acetone: acetic acid (50: 0.05) is washed silicagel column, and the collection elutriant is recycled to driedly, gets dry extract.Get dried cream, with the dissolving of 20% methanol aqueous solution, last Sephadex LH-20 post is washed chromatographic column with 20% methanol aqueous solution, collect elutriant, merge elutriant according to TLC, be recycled on a small quantity, add an amount of methyl alcohol, transfer pH value to weakly alkaline with aqueous sodium hydroxide solution, place, crystallization gets Sodium Danshensu crystallization (99.95%).
Embodiment four
The red sage root (individual sub-goods) 3kg adds poach 3 times, adds 6 times of amounts of water for the first time, boils 6 hours, and back secondary respectively adds 5 times of amounts of water, respectively boils 4 hours, filters, and merges three times filtrate; Be concentrated in right amount, be cooled to room temperature, add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 60%; After room temperature is placed 12 hours, to filter, filtrate is concentrated in right amount, is cooled to room temperature; Add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 85%, after room temperature is placed 12 hours, filters; Filtrate is concentrated in right amount, is cooled to room temperature, adds the water of 4 times of amounts, and the limit edged stirs, and places 1-2 hours, filters; Macroporous adsorptive resins on the filtrate (D101,800g), the water wash-out is collected elutriant, polyamide column on the elutriant (60-100 orders, 250g), the water wash-out is collected elutriant; Concentrate eluant is mixed silica gel 1000g (100-200 order) to an amount of, dries (65 ℃) to baking oven.Silica gel dress post, use chloroform: acetic acid (50:1) is washed silicagel column, and the collection elutriant is recycled to driedly, gets dry extract.Get dried cream, with the dissolving of 40% aqueous ethanolic solution, last reverse phase silica gel post (Rp-18) is with 40% ethanol aqueous wash chromatographic column, collect elutriant, merge elutriant according to TLC, be recycled on a small quantity, add an amount of methyl alcohol, transfer pH value to weakly alkaline with aqueous sodium carbonate, place, crystallization gets Sodium Danshensu crystallization (99.25%).
Embodiment five
The red sage root (medicine materical crude slice) 3kg adds poach 3 times, adds 6 times of amounts of water for the first time, boils 8 hours, and back secondary respectively adds 5 times of amounts of water, respectively boils 4 hours, filters, and merges three times filtrate; Be concentrated in right amount, be cooled to room temperature, add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 40%; After room temperature is placed 12 hours, to filter, filtrate is concentrated in right amount, is cooled to room temperature; Add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 70%, after room temperature is placed 12 hours, filters; Filtrate is concentrated in right amount, is cooled to room temperature, adds the water of 3 times of amounts, and the limit edged stirs, and places 1-2 hours, filters; Macroporous adsorptive resins on the filtrate (H103,800g), the water wash-out is collected elutriant; Concentrate eluant is mixed silica gel 1000g (100-200 order) to an amount of, dries (65 ℃) to baking oven.Silica gel dress post, use ethyl acetate: acetic acid (50:0.5) is washed silicagel column, and the collection elutriant is recycled to driedly, gets dry extract.Get dried cream, with the dissolving of 60% aqueous ethanolic solution, last SephadexLH-20 post is with 60% ethanol aqueous wash chromatographic column, collect elutriant, merge elutriant according to TLC, be recycled on a small quantity, add an amount of ethanol, transfer pH value to weakly alkaline with aqueous sodium carbonate, place, crystallization gets Sodium Danshensu crystallization (99.81%).
Embodiment six
The red sage root (medicine materical crude slice) 3kg adds poach 3 times, adds 8 times of amounts of water for the first time, boils 8 hours, and back secondary respectively adds 5 times of amounts of water, respectively boils 5 hours, filters, and merges three times filtrate; Be concentrated in right amount, be cooled to room temperature, add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 50%; After room temperature is placed 12 hours, to filter, filtrate is concentrated in right amount, is cooled to room temperature; Add 95% ethanol, the limit edged stirs, and containing the alcohol amount to solution is 80%, after room temperature is placed 12 hours, filters; Filtrate is concentrated in right amount, is cooled to room temperature, adds the water of 4 times of amounts, and the limit edged stirs, and places 1-2 hours, filters; Macroporous adsorptive resins on the filtrate (H103,800g), the water wash-out is collected elutriant; Concentrate eluant is mixed silica gel 1000g (100-200 order) to an amount of, dries (65 ℃) to baking oven.Silica gel dress post, use chloroform: formic acid (50:0.8) is washed silicagel column, and the collection elutriant is recycled to driedly, gets dry extract.Get dried cream, with the dissolving of 30% methanol aqueous solution, last reverse phase silica gel post (Rp-18) is washed chromatographic column with 30% methanol aqueous solution, collect elutriant, merge elutriant according to TLC, be recycled on a small quantity, add an amount of ethanol, transfer pH value to weakly alkaline with sodium bicarbonate aqueous solution, place, crystallization gets Sodium Danshensu crystallization (99.05%).
Claims (8)
1, a kind of preparation method of salvianic acid A sodium pure product is characterized in that, comprises the steps:
(a) red sage root is carried with hydro-thermal, and extracting solution concentrates, and adds the ethanol alcohol precipitation, filters;
(b) filtrate concentrates, and adds the ethanol alcohol precipitation, filters;
(c) filtrate concentrates, and adds water, filters, and macroporous adsorptive resins on the filtrate washes with water;
(d) after water lotion concentrated, (e) carried out set by step; Perhaps polyamide column on the water lotion washes with water, and after the condensed water washing lotion, (e) carries out set by step.
(e) water lotion after concentrating is mixed silica gel, oven dry, and the dress post use the organic solvent wash-out, and the collection elutriant is recycled to driedly, gets dry extract.
(f) get dried cream, use organic solvent dissolution, transfer pH value, place crystallization; Perhaps get dried cream, use dissolution with solvents, last Sephadex LH-20 post or reverse phase silica gel post, elutriant is transferred pH value, places crystallization.
2, preparation method according to claim 1, it is characterized in that, also comprise red sage root boiling 2-4 times in the step (a), each 4-8 hours, amount of water is 5-8 times of amounts of red sage root weight, and merging filtrate is concentrated into an amount of, add 95% ethanol or dehydrated alcohol, containing the alcohol amount to solution is 40-60%, places 6-24 hours, filters; Comprise also in the step (b) that filtrate is concentrated in right amount, add 95% ethanol or dehydrated alcohol, containing the alcohol amount to solution is 70-85%, places 6-24 hours, filters; Comprise also in the step (c) that filtrate is concentrated in right amount, add 2-6 times of amounts of water, filter, macroporous adsorptive resins on the filtrate washes with water; Comprise also in the step (d) that after water lotion concentrated, (e) carried out set by step; Perhaps polyamide column on the water lotion washes with water, and after the condensed water washing lotion, (e) carries out set by step.Comprise also in the step (e) that the water lotion after concentrating is mixed silica gel (60-400 order), oven dry (30-120 ℃), the dress post is washed chromatographic column with containing the organic acid organic solvent, and the collection elutriant is recycled to driedly, gets dry extract; Also comprise in the step (f), get dried cream,, add appropriate alkaline liquor and transfer pH value, place crystallization with methyl alcohol, ethanol or acetone solution; Perhaps get dried cream, water, moisture or anhydrous methanol, moisture or anhydrous alcohol solution, last Sephadex LH-20 post or reverse phase silica gel post (Rp-2, Rp-8, Rp-18), water, moisture or anhydrous methanol, moisture or dehydrated alcohol are washed chromatographic column, collect elutriant, merge elutriant according to TLC, be recycled on a small quantity, add an amount of methyl alcohol, ethanol or acetone, transfer pH value with appropriate alkaline liquor, place crystallization.
3, preparation method according to claim 2 is characterized in that, also comprises in the step (a), adds 95% ethanol alcohol precipitation, places 8-15 hours; Also comprise in the step (b), add 95% ethanol alcohol precipitation, placed 8-15 hours; Comprise also in the step (c) that add 2-4 times of amounts of water, described macroporous adsorbent resin is a styrene type; Polymeric amide described in the step (d) is polycaprolactam (nylon-6).
4, preparation method according to claim 2, it is characterized in that, also comprise in the step (e), silica gel is 100-200 orders, bake out temperature is 50-70 ℃, and organic solvent comprises: methyl alcohol, ethanol, acetone, ethyl acetate, chloroform, ether, propyl carbinol, isopropylcarbinol, normal hexane, hexanaphthene, sherwood oil; Organic acid comprises: formic acid, acetic acid, propionic acid, butyric acid, oxalic acid, propanedioic acid, Succinic Acid.
5, preparation method according to claim 2 is characterized in that, comprises that also organic solvent comprises in the step (e): acetone, ethyl acetate, chloroform, and organic acid comprises: formic acid, acetic acid; Also comprise in the step (f), get dried cream, with methyl alcohol or dissolve with ethanol, hydro-oxidation sodium, yellow soda ash, sodium bicarbonate aqueous solution transfer pH value to weakly alkaline.
6, preparation method according to claim 2 is characterized in that, also comprises in the step (f), gets dried cream, and with 5-95% methyl alcohol or aqueous ethanolic solution dissolving, last chromatographic column is with 5-95% methyl alcohol or ethanol aqueous wash chromatographic column.
7, preparation method according to claim 2 is characterized in that, also comprises in the step (f), get dried cream, with 20-60% methyl alcohol or aqueous ethanolic solution dissolving, last Sephadex LH-20 post or reverse phase silica gel post (Rp-2, Rp-8, Rp-18), with 20-60% methyl alcohol or ethanol aqueous wash chromatographic column, collect elutriant, merge elutriant, be recycled to a small amount of according to TLC, add an amount of methyl alcohol or ethanol, transfer pH value to weakly alkaline with sodium hydroxide, yellow soda ash or sodium bicarbonate aqueous solution, place crystallization.
8, according to the Sodium Danshensu of the described method of claim 2 preparation, its purity is more than or equal to 98% (middle inspection institute standard substance demarcation).
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| CN 200710166154 CN101434534B (en) | 2007-11-12 | 2007-11-12 | Preparation of salvianic acid A sodium pure product |
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| CN101434534B CN101434534B (en) | 2013-04-03 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336652A (en) * | 2010-07-16 | 2012-02-01 | 湖南康普医药研究院 | Method for scale preparation of high-purity Danshensu sodium |
| CN102464581A (en) * | 2010-11-12 | 2012-05-23 | 天津天士力制药股份有限公司 | Method for preparing high-purity sodium danshensu |
| US9061979B2 (en) | 2011-07-29 | 2015-06-23 | Insight High Technology (Beijing) Co. Ltd. | Mercapto benzophenone compounds, compositions and preparations method thereof |
| CN107827737A (en) * | 2017-10-31 | 2018-03-23 | 齐芳 | A kind of alcohol extracting method for reducing danshensu loss |
| CN116143615A (en) * | 2022-09-14 | 2023-05-23 | 上海其光药业有限公司 | Salvianic acid A sodium I crystal form and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100502901C (en) * | 2003-05-20 | 2009-06-24 | 天津天士力制药股份有限公司 | Extraction method for effective parts of salvia |
| CN1868994B (en) * | 2005-05-24 | 2010-06-23 | 山东绿叶制药有限公司 | Preparation method of sodium danshensu |
-
2007
- 2007-11-12 CN CN 200710166154 patent/CN101434534B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336652A (en) * | 2010-07-16 | 2012-02-01 | 湖南康普医药研究院 | Method for scale preparation of high-purity Danshensu sodium |
| CN102464581A (en) * | 2010-11-12 | 2012-05-23 | 天津天士力制药股份有限公司 | Method for preparing high-purity sodium danshensu |
| CN102464581B (en) * | 2010-11-12 | 2015-02-25 | 天士力制药集团股份有限公司 | Method for preparing high-purity sodium danshensu |
| US9061979B2 (en) | 2011-07-29 | 2015-06-23 | Insight High Technology (Beijing) Co. Ltd. | Mercapto benzophenone compounds, compositions and preparations method thereof |
| US9409861B2 (en) | 2011-07-29 | 2016-08-09 | Insight High Technology (Beijing) Co. Ltd. | Mercapto benzophenone compounds, compositions and preparation method thereof |
| CN107827737A (en) * | 2017-10-31 | 2018-03-23 | 齐芳 | A kind of alcohol extracting method for reducing danshensu loss |
| CN116143615A (en) * | 2022-09-14 | 2023-05-23 | 上海其光药业有限公司 | Salvianic acid A sodium I crystal form and preparation method thereof |
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| CN101434534B (en) | 2013-04-03 |
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