CN104974033A - Method for extracting tanshinol - Google Patents
Method for extracting tanshinol Download PDFInfo
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- CN104974033A CN104974033A CN201310711708.3A CN201310711708A CN104974033A CN 104974033 A CN104974033 A CN 104974033A CN 201310711708 A CN201310711708 A CN 201310711708A CN 104974033 A CN104974033 A CN 104974033A
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Abstract
The invention discloses a method for extracting tanshinol. The method is characterized by comprising the following steps of carrying out hot dipping extraction of radix salvia miltiorrhiza by adding water, clarifying by using a clarifying agent after filtering extraction solution, and, after carrying out alcohol precipitation or/and water precipitation of the clarifying solution, concentrating to obtain an extract with the relative density of 1.30 or more. According to the invention, the phenomena of complex purifying and refining process, many impurities, incomplete purification, low finished extract content, deep prepared preparation color and the like due to high-temperature decocting and reflux extraction can be avoided; the purifying and refining process of the tanshinol extraction process can be reduced; the tanshinol content of the finished extract can be increased; the clarification degree of the preparation is increased; the colour of the preparation is light; and the method is easy to operate and is applied to industrialized mass production.
Description
Technical field:
The present invention relates to the extracting method of Salvianic acidA, espespecially the extracting method of target component Salvianic acidA in red rooted salvia.
Background technology:
Chinese: Salvianic acidA (phenol aromatic acid compound, brown color or yellow), English name: Danshensu, another name: B-(3,4-dihydroxy phenyl) lactic acid, D(+) B-(3,4-Dihydroxyphenyl) lacticacid Salvianic acid, chemical name: Propanoic acid, 3-(3,4-dihydroxyphenyl)-2-hydroxy-, molecular formula is C9H10O5, molecular weight: 198.17.
Structural formula is as follows:
Salvianic acidA has: antithrombus formation, anticoagulant and anti-freezing, atherosclerosis and the effect such as reducing blood-fat, coronary artery dilator, is the main component for the treatment of vascular conditions.
For a long time, in Salvianic acidA extraction, purifying, field of refinement, be adopt high temperature to decoct refluxing extraction to obtain liposoluble ingredient in red rooted salvia (wherein Salvianic acidA is one of liposoluble ingredient) mostly; Activated carbon decolorizing process medicinal extract is adopted to obtain light-colored preparation; But Chinese medical extract complicated component, component is more, and it is unpractical for accomplishing that the Salvianic acidA of 100% is separated and removes medicinal extract color.
Summary of the invention:
Technical problem to be solved by this invention is to carry out the effective problem that is separated for high temperature being decocted target component Salvianic acidA in the Radix Salviae Miltiorrhizae extractum of refluxing extraction in Salvianic acidA extraction, purifying, process for refining and provide a kind of hot dipping method that adopts to extract, be equipped with the extracting method of the Salvianic acidA of finings clarification, the impurity that this extracting method can effectively avoid high temperature decoction refluxing extraction to bring is many, purification refine operation is many, process is complicated, removal of impurities is not thorough, finished product medicinal extract content is low, and the preparation color configured is dark.
Technical problem to be solved by this invention can be achieved through the following technical solutions:
An extracting method for Salvianic acidA, is characterized in that, this extracting method adds water to red rooted salvia and carries out hot dipping method extraction, and extracting solution is equipped with finings clarification after filtering, clear liquor or/and after depositing in water, is concentrated into the medicinal extract that relative density is more than 1.30 through alcohol precipitation.
In a preferred embodiment of the invention, the add-on of described water is more than 10 times of red rooted salvia.
In a preferred embodiment of the invention, described water is purified water.
In a preferred embodiment of the invention, limit extraction limit forced refluence or stirring in hot dipping method leaching process.
In a preferred embodiment of the invention, hot dipping temperature is 75 DEG C ~ 85 DEG C.
In a preferred embodiment of the invention, the hot dipping time is 24 hours.
In a preferred embodiment of the invention, the add-on of described finings is 1.0 ~ 1.5g/L.
In a preferred embodiment of the invention, settling time is 24 hours.
In a preferred embodiment of the invention, clarifying temp is 20 DEG C-25 DEG C.
In a preferred embodiment of the invention, described finings is configured by natural clarifying agent and acetic acid and forms, and wherein the mass volume ratio of natural clarifying agent and acetic acid is 1000 grams: 100000ml.
In a preferred embodiment of the invention, the mass percent concentration of described acetic acid is 1%.
In a preferred embodiment of the invention, described natural clarifying agent be selected from that gelatin, sodium alginate, tannin, Citric Acid, agar, egg white, enzyme element, Sucus Glycyrrhizae, chitin and derivative, 101 fruit juice clarifiers, coacervation are clean, one or more combination in ZTC1+1 natural clarifying agent.
In a preferred embodiment of the invention, described finings is selected from chitin and derivative deep friendship converted products chitosan.
This chitin and derivative are the materials obtained after dilute acid pretreatment from arthropods shrimp and crab shells, nonpoisonous and tasteless, biodegradable, can not cause secondary pollution.This type of material can destroy the stability of Solution Dispersion system, thus accelerates settling velocity raising clarifying effect; This type of material by electrical counteract be used for remove pedesis, enable particulate near contact and aggregate and precipitate.
In a preferred embodiment of the invention, alcohol precipitation number of times is once, and depositing in water number of times is once.
In a preferred embodiment of the invention, during alcohol precipitation, alcohol content is 80%.
Owing to have employed technical scheme as above, present invention, avoiding due to high temperature that to decoct the purification refine process brought of refluxing extraction complicated, impurity is many, and removal of impurities is thorough, the phenomenons such as finished product medicinal extract content is low, and the preparation color configured is dark.
The present invention can reduce the purification refine process of Salvianic acidA extraction process, and improve finished product medicinal extract content of Danshensu, improve preparation clarity, preparation is of light color, and processing ease realizes, and is applicable to industrialized production.
Embodiment:
Can be well understood to the present invention further by specific embodiments of the invention given below, but they not limitation of the invention.
Comparative example 1:
High temperature decocts reflux extraction: get red rooted salvia, after selected, removal of impurities, cutting, take clean medicinal material 100Kg, drop in extractor, add the purified water of medicinal material consumption 10 times, boil rear insulation 2 hours, extracting solution filters, concentrating under reduced pressure, through 2 alcohol precipitations, (alcohol content reaches 75% for the first time again, second time alcohol content reaches 85%), 1 depositing in water, being concentrated into relative density is more than 1.30.Extracting solution sampling censorship, it the results are shown in following table 1:
Embodiment 1
Hot dipping method: get red rooted salvia, after selected, removal of impurities, cutting, takes clean medicinal material 100Kg, drop in extractor, add the purified water of medicinal material consumption 10 times, hot dipping (80 DEG C ± 5 DEG C) method extracts 24 hours, extraction limit, limit forced refluence, extracting solution filters, and filtrate is cooled to room temperature 20 DEG C-25 DEG C.Add finings 1.0-1.5g/L(chitosan 1000 grams, add the acetic acid 100000ml of 1%, after stirring, leave standstill 24 hours, for subsequent use) clarify centrifugal concentrating after 24 hours, concentrated solution is again through 1 alcohol precipitation (alcohol content reaches 80%), and 1 depositing in water, being concentrated into relative density is more than 1.30.Hot dipping liquid sampling censorship, it the results are shown in following table 1:
Table 1
Comparative example 2:
High temperature decocts reflux extraction: get red rooted salvia, after selected, removal of impurities, cutting, take clean medicinal material 100Kg, drop in extractor, add the purified water of medicinal material consumption 10 times, boil rear insulation 2 hours, extracting solution filters, concentrating under reduced pressure, through 2 alcohol precipitations, (alcohol content reaches 75% for the first time again, second time alcohol content reaches 85%), 1 depositing in water, being concentrated into relative density is more than 1.30.Extracting solution sampling censorship, it the results are shown in following table 2.
Embodiment 2
Hot dipping method: get red rooted salvia, after selected, removal of impurities, cutting, takes clean medicinal material 100Kg, drop in extractor, add the purified water of medicinal material consumption 10 times, hot dipping (80 DEG C ± 5 DEG C) method extracts 24 hours, extraction limit, limit forced refluence, extracting solution filters, and filtrate is cooled to room temperature 20 DEG C-25 DEG C.Add finings 1.0-1.5g/L(chitosan 1000 grams, add the acetic acid 100000ml of 1%, after stirring, leave standstill 24 hours, for subsequent use) clarify centrifugal concentrating after 24 hours, concentrated solution is again through 1 alcohol precipitation (alcohol content reaches 80%), and 1 depositing in water, being concentrated into relative density is more than 1.30.Extracting solution sampling censorship, it the results are shown in following table 2.
Table 2
Comparative example 3:
High temperature decocts reflux extraction: get red rooted salvia, after selected, removal of impurities, cutting, take clean medicinal material 100Kg, drop in extractor, add the purified water of medicinal material consumption 10 times, boil rear insulation 2 hours, extracting solution filters, concentrating under reduced pressure, through 2 alcohol precipitations, (alcohol content reaches 75% for the first time again, second time alcohol content reaches 85%), 1 depositing in water, being concentrated into relative density is more than 1.30.Extracting solution sampling censorship, it the results are shown in following table 3.
Embodiment 3
Hot dipping method: get red rooted salvia, after selected, removal of impurities, cutting, takes clean medicinal material 100Kg, drop in extractor, add the purified water of medicinal material consumption 10 times, hot dipping (80 DEG C ± 5 DEG C) method extracts 24 hours, extraction limit, limit forced refluence, extracting solution filters, and filtrate is cooled to room temperature 20 DEG C-25 DEG C.Add finings 1.0-1.5g/L(chitosan 1000 grams, add the acetic acid 100000ml of 1%, after stirring, leave standstill 24 hours, for subsequent use) clarify centrifugal concentrating after 24 hours, concentrated solution is again through 1 alcohol precipitation (alcohol content reaches 80%), and 1 depositing in water, being concentrated into relative density is more than 1.30.Extracting solution sampling censorship, it the results are shown in following table 3.
Table 3
Claims (15)
1. an extracting method for Salvianic acidA, is characterized in that, this extracting method adds water to red rooted salvia and carries out hot dipping method extraction, and extracting solution is equipped with finings clarification after filtering, clear liquor or/and after depositing in water, is concentrated into the medicinal extract that relative density is more than 1.30 through alcohol precipitation.
2. the extracting method of Salvianic acidA as claimed in claim 1, it is characterized in that, the add-on of described water is more than 10 times of red rooted salvia.
3. the extracting method of Salvianic acidA as claimed in claim 1 or 2, it is characterized in that, described water is purified water.
4. the extracting method of Salvianic acidA as claimed in claim 1, is characterized in that, limit extraction limit forced refluence or stirring in hot dipping method leaching process.
5. the extracting method of the Salvianic acidA as described in claim 1 or 4, is characterized in that, hot dipping temperature is 75 DEG C ~ 85 DEG C.
6. the extracting method of the Salvianic acidA as described in claim 1 or 4, is characterized in that, the hot dipping time is 24 hours.
7. the extracting method of Salvianic acidA as claimed in claim 1, it is characterized in that, the add-on of described finings is 1.0-1.5g/L.
8. the extracting method of Salvianic acidA as claimed in claim 1, it is characterized in that, settling time is 24 hours.
9. the extracting method of Salvianic acidA as claimed in claim 1, it is characterized in that, clarifying temp is 20 DEG C-25 DEG C
10. the extracting method of Salvianic acidA as claimed in claim 1, it is characterized in that, described finings is configured by natural clarifying agent and acetic acid and forms, wherein the mass volume ratio of natural clarifying agent and acetic acid be 1000 ~ gram: ~ 100000ml.
The extracting method of 11. Salvianic acidAs claimed in claim 1, is characterized in that, the mass percent concentration of described acetic acid is 1%.
The extracting method of 12. Salvianic acidAs claimed in claim 10, it is characterized in that, described natural clarifying agent is selected from that gelatin, sodium alginate, tannin, Citric Acid, agar, egg white, enzyme element, Sucus Glycyrrhizae, chitin and derivative, 101 fruit juice clarifiers, coacervation are clean, one or more combination in ZTC1+1 natural clarifying agent.
The extracting method of 13. Salvianic acidAs claimed in claim 10, is characterized in that, described natural clarifying agent is selected from chitin and derivative deep friendship converted products chitosan.
The extracting method of 14. Salvianic acidAs claimed in claim 1, it is characterized in that, alcohol precipitation number of times is once, and depositing in water number of times is once.
The extracting method of 15. Salvianic acidAs described in claim 1 or 14, it is characterized in that, during alcohol precipitation, alcohol content is 80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310711708.3A CN104974033A (en) | 2013-12-22 | 2013-12-22 | Method for extracting tanshinol |
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| CN201310711708.3A CN104974033A (en) | 2013-12-22 | 2013-12-22 | Method for extracting tanshinol |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105461543A (en) * | 2015-12-22 | 2016-04-06 | 贵州景峰注射剂有限公司 | Method for converting tanshinol into sodium tanshinol |
| CN105510472A (en) * | 2015-12-22 | 2016-04-20 | 贵州景峰注射剂有限公司 | Method for detecting tannin in shenxiong glucose injection |
| CN105566092A (en) * | 2015-12-22 | 2016-05-11 | 贵州景峰注射剂有限公司 | Preparation method of high-content salvianic acid A sodium |
| CN108785381A (en) * | 2018-09-17 | 2018-11-13 | 吉林四长制药有限公司 | A kind of preparation method of pharmaceutical composition for angiocardiopathy |
| CN114073673A (en) * | 2020-08-21 | 2022-02-22 | 邯郸制药股份有限公司 | Treatment method for improving clarity of traditional Chinese medicine liquid oral preparation |
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| CN1670008A (en) * | 2004-03-18 | 2005-09-21 | 中国科学院大连化学物理研究所 | Process for preparing Danshensu |
| CN103432199A (en) * | 2013-08-27 | 2013-12-11 | 江西中医学院 | Preparation method of pharmaceutical composition, and pharmaceutical composition prepared thereby |
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2013
- 2013-12-22 CN CN201310711708.3A patent/CN104974033A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1670008A (en) * | 2004-03-18 | 2005-09-21 | 中国科学院大连化学物理研究所 | Process for preparing Danshensu |
| CN103432199A (en) * | 2013-08-27 | 2013-12-11 | 江西中医学院 | Preparation method of pharmaceutical composition, and pharmaceutical composition prepared thereby |
Non-Patent Citations (1)
| Title |
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| 杜松: "心肌康注射液中丹参的精制工艺及指纹图谱的初步研究", 《中国优秀博硕士学位论文全文数据库 (硕士) 医药卫生科技辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105461543A (en) * | 2015-12-22 | 2016-04-06 | 贵州景峰注射剂有限公司 | Method for converting tanshinol into sodium tanshinol |
| CN105510472A (en) * | 2015-12-22 | 2016-04-20 | 贵州景峰注射剂有限公司 | Method for detecting tannin in shenxiong glucose injection |
| CN105566092A (en) * | 2015-12-22 | 2016-05-11 | 贵州景峰注射剂有限公司 | Preparation method of high-content salvianic acid A sodium |
| CN108785381A (en) * | 2018-09-17 | 2018-11-13 | 吉林四长制药有限公司 | A kind of preparation method of pharmaceutical composition for angiocardiopathy |
| CN114073673A (en) * | 2020-08-21 | 2022-02-22 | 邯郸制药股份有限公司 | Treatment method for improving clarity of traditional Chinese medicine liquid oral preparation |
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Application publication date: 20151014 |