CN105461543A - Method for converting tanshinol into sodium tanshinol - Google Patents
Method for converting tanshinol into sodium tanshinol Download PDFInfo
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- CN105461543A CN105461543A CN201510973247.6A CN201510973247A CN105461543A CN 105461543 A CN105461543 A CN 105461543A CN 201510973247 A CN201510973247 A CN 201510973247A CN 105461543 A CN105461543 A CN 105461543A
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- tanshinol
- sodium
- salvianic acida
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a new converting method for preparing sodium tanshinol. The method for converting anshinol into the sodium tanshinol is characterized in that the method is the one for carrying out hot acid water extraction on salvia miltiorrhiza and converting the salvia miltiorrhiza into salt in a heating way by matching with sodium hydroxide to regulate the pH (potential of Hydrogen). According to the method disclosed by the invention, the problems that many impurities are brought by high-temperature boiling, reflux extraction and high-temperature concentration, tanshinol is seriously damaged, the transfer rate is low, many purification processes are needed, the process is complex, the period is long, impurity removing is not complete, the content of the sodium tanshinol in a finished product is low, the stability is extremely poor, and the like are effectively avoided; oxidation and degradation on the tanshinol during an extracting process can be reduced, the content of the tanshinol in an extracting solution is increased, the tanshinol is furthest converted into the sodium tanshinol which is extremely stable, the damage from high temperature to the tanshinol is avoided, no any antioxidant is added, the storage stability of the sodium tanshinol in an acid environment is ensured, the operation is easily realized, and the method is suitable for industrialized large-scale production.
Description
Technical field:
The present invention relates to Salvianic acidA preparing technical field, espespecially relate to and effective constituent Salvianic acidA in red rooted salvia is changed into the method for Sodium Danshensu.
Background technology:
Sodium Danshensu, Chinese: 3-(3', 4'-dihydroxy phenyl) Sodium.alpha.-hydroxypropionate; English name: SodiumDanshensu, Sodium Danshensu CAS accession number: 67920-52-9, molecular formula: C
9h
9naO
5, molecular weight: 220.16.White, needle-shaped crystals; Be dissolved in methyl alcohol, water, be insoluble to chloroform, ether; Fusing point 255 ~ 258 DEG C.
Structural formula is as follows:
Sodium Danshensu has: anticoagulant and anticoagulation, antisepsis and anti-inflammation and enhancing body immunization, atherosclerosis and reducing blood lipid, anti-thrombosis function, the effect for the treatment of liver injury, anti-cerebral ischemia damnification effect etc.
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.
In red rooted salvia, one of liposoluble ingredient Salvianic acidA is at occurring in nature extremely unstable, therefore it is prepared into sodium salt (Sodium Danshensu), and effect is the same with Salvianic acidA, and physico-chemical property is comparatively stable.Be used for promoting blood circulation and removing blood stasis, regulating QI to relieve pain, feel oppressed for chest, stenocardia.
The content of Salvianic acidA in red rooted salvia is very low, Salvianic acidA is main in leaching process generates Salvianic acidA by salvianolic acid B hydrolysis, for a long time, at Salvianic acidA extraction, purification art, adopt high temperature to decoct refluxing extraction, concentrate to obtain effective constituent Salvianic acidA in red rooted salvia mostly, such Salvianic acidA is heated for a long time and easily degrades and oxidation, and Salvianic acidA ultimate yield is very low; Red rooted salvia component is more, complicated component, mutual dynamic conversion between composition, accomplishes that the Salvianic acidA of 100% is separated extremely unrealistic, therefore can not get high-purity salvianic acid A, extractive content is low, add Salvianic acidA in aqueous with there is environment change and extremely unstable, extract is depositing also easily degraded and oxidation in process, therefore is prepared into comparatively stable Sodium Danshensu, effect is the same with Salvianic acidA, is convenient to stably stored.But current technique improves the content of Danshensu in medicinal extract.
Summary of the invention:
Technical problem to be solved by this invention is to extract for Salvianic acidA, high temperature cannot be decocted refluxing extraction in purifying process, in the Radix Salviae Miltiorrhizae extractum that high temperature is concentrated, target component Salvianic acidA is effectively separated, Salvianic acidA long-time hot environment in purge process cannot be avoided to be degraded and to be oxidized, the problem of its stability in storage cannot be ensured and a kind of method Salvianic acidA being converted into Sodium Danshensu is provided, transform a step just can complete, this method for transformation effectively avoids high temperature and decocts refluxing extraction, it is many that high temperature concentrates the impurity brought, Salvianic acidA destroys serious, the rate of transform is low, purification refine operation is many, cycle is long, process is complicated, removal of impurities is not thorough, finished product medicinal extract content of Danshensu is low, the problems such as stability extreme difference.
Technical problem to be solved by this invention can be achieved through the following technical solutions:
Salvianic acidA is transformed a method for Sodium Danshensu, it is characterized in that, comprise the steps:
(1) Salvianic acidA proposes step
Medicinal material amount 10 ~ 20 times of purified water are added in extractor, adding acid regulates its pH value to be 2.5 ~ 5.5, opens stirring, condenser, with steam, water is heated to 50 DEG C ~ 70 DEG C, the medicinal material weighed up is dropped in extractor and repeats extraction 1 ~ 3 time, merge each filtrate after filtering and obtain extracting solution;
(2) step of converting
Extracting solution prepared by step (1) is proceeded in converting apparatus, adding alkali to pH value is 10 ~ 12, and be heated to 100 DEG C ~ 120 DEG C, converting apparatus internal pressure maintains 0.1Mpa ~ 0.2Mpa, after boiling, insulation guarantor 4-6 hours, changes into Sodium Danshensu by the Salvianic acidA in extracting solution.
In a preferred embodiment of the invention, the filtration in step (1) adopts 100 eye mesh screens to filter.
In a preferred embodiment of the invention, the leaching process of step (1) under agitation carries out.?
In a preferred embodiment of the present invention, the acid in step (1) is hydrochloric acid.
In a preferred embodiment of the invention, the alkali in step (2) is sodium hydroxide.
In a preferred embodiment of the invention, described converting apparatus material is enamel pot.
Owing to have employed technical scheme as above, present invention, avoiding that high temperature decocts refluxing extraction, that high temperature concentrates the impurity brought is many, Salvianic acidA destroys serious, the rate of transform is low, and purification procedures is many, and process is complicated, production cycle is long, removal of impurities is not thorough, the problems such as finished product medicinal extract content of Danshensu is low, stability extreme difference.
The present invention can reduce the purge process of Salvianic acidA extraction process, with short production cycle, improve finished product medicinal extract Sodium Danshensu content, improve Sodium Danshensu yield, purge process avoids the destruction of high temperature to Salvianic acidA, does not add any oxidation inhibitor, transform a step just can complete, in sour environment, ensure that the stability in storage of Salvianic acidA, 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, takes clean medicinal material 30Kg, drops in extractor, adds the purified water of medicinal material consumption 15 times, boil rear insulation 2 hours, extracts 1 time, extracting solution filtration.Sampling detects Sodium Danshensu content, and it the results are shown in following table 1:
Embodiment 1
Extract: in extractor, add medicinal material amount 10 times of purified water, regulate its pH value to be 4.5, open stirring, condenser, with steam, water is heated to 65 DEG C, the 30Kg medicinal material weighed up is dropped in extractor, extracts 1.5 hours temperature 65 DEG C, extract 1 time, Keep agitation in leaching process, filter.Proceed in enamel pot, add Sodium hydroxide q. s, transform 1 time, pH regulator to 10.5, is heated to 105 degree, and tank internal pressure maintains 0.14Mpa, insulation guarantor 4 hours after boiling.Sampling detects Sodium Danshensu content, and it the results are shown in following table 1:
Embodiment 2
Extract: in extractor, add medicinal material amount 15 times of purified water, regulate its pH value to be 4.9, open stirring, condenser, with steam, water is heated to 68 DEG C, the 30Kg medicinal material weighed up is dropped in extractor, extracts 2 hours temperature 68 DEG C, extract 2 times, Keep agitation in leaching process, filter.Proceed in enamel pot, add Sodium hydroxide q. s, transform 1 time, pH regulator to 11.0, is heated to 110 degree, and tank internal pressure maintains 0.16Mpa, insulation guarantor 5 hours after boiling.Sampling detects Sodium Danshensu content, and it the results are shown in following table 1:
Embodiment 3
Extract: in extractor, add medicinal material amount 20 times of purified water, regulate its pH value to be 4.6, open stirring, condenser, with steam, water is heated to 70 DEG C, the 30Kg medicinal material weighed up is dropped in extractor, extracts 2.5 hours at temperature 70 C, extract 3 times, Keep agitation in leaching process, filter.Proceed in enamel pot, add Sodium hydroxide q. s, transform 1 time, pH regulator to 11.5, is heated to 115 degree, and tank internal pressure maintains 0.18Mpa, insulation guarantor 6 hours after boiling.Sampling detects Sodium Danshensu content, and it the results are shown in following table 1:
Table 1
Claims (6)
1. Salvianic acidA is transformed a method for Sodium Danshensu, it is characterized in that, comprise the steps:
(1) Salvianic acidA proposes step
Medicinal material amount 10 ~ 20 times of purified water are added in extractor, adding acid regulates its pH value to be 2.5 ~ 5.5, opens stirring, condenser, with steam, water is heated to 50 DEG C ~ 70 DEG C, the medicinal material weighed up is dropped in extractor and repeats extraction 1 ~ 3 time, merge each filtrate after filtering and obtain extracting solution;
(2) step of converting
Extracting solution prepared by step (1) is proceeded in converting apparatus, adding alkali to pH value is 10 ~ 12, and be heated to 100 DEG C ~ 120 DEG C, converting apparatus internal pressure maintains 0.1Mpa ~ 0.2Mpa, after boiling, insulation guarantor 4-6 hours, changes into Sodium Danshensu by the Salvianic acidA in extracting solution.
2. method Salvianic acidA being transformed Sodium Danshensu as claimed in claim 1, is characterized in that, the filtration in step (1) adopts 100 eye mesh screens to filter.
3. method Salvianic acidA being transformed Sodium Danshensu as claimed in claim 1, it is characterized in that, the leaching process of step (1) under agitation carries out.
4. method Salvianic acidA being transformed Sodium Danshensu as claimed in claim 1, it is characterized in that, the acid in step (1) is hydrochloric acid.
5. method Salvianic acidA being transformed Sodium Danshensu as claimed in claim 1, it is characterized in that, the alkali in step (2) is sodium hydroxide.
6. method Salvianic acidA being transformed Sodium Danshensu as claimed in claim 1, it is characterized in that, described converting apparatus material is enamel pot.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510973247.6A CN105461543A (en) | 2015-12-22 | 2015-12-22 | Method for converting tanshinol into sodium tanshinol |
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| CN201510973247.6A CN105461543A (en) | 2015-12-22 | 2015-12-22 | Method for converting tanshinol into sodium tanshinol |
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| CN105461543A true CN105461543A (en) | 2016-04-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108362663A (en) * | 2018-04-18 | 2018-08-03 | 贵州景峰注射剂有限公司 | The extracting method of method of quality control and Sodium Danshensu in red sage root extract purification process |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289385A (en) * | 2008-06-12 | 2008-10-22 | 中国人民解放军第二军医大学 | Process for abstracting high-purity tanshinol form salvia |
| CN101289386A (en) * | 2008-06-12 | 2008-10-22 | 南京泽朗医药科技有限公司 | Method for preparing sodium tanshinol |
| CN101445451A (en) * | 2008-12-30 | 2009-06-03 | 合肥紫金医药科技有限公司 | Method for preparing high-purity salvianic acid A sodium |
| EP2415749A1 (en) * | 2009-03-30 | 2012-02-08 | Tianjin Tasly Pharmaceutical Co. Ltd. | New salvianolic acid compound l, preparation method and use thereof |
| 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 |
| CN103058854A (en) * | 2012-12-21 | 2013-04-24 | 贵州景峰注射剂有限公司 | Method for converting danshinolic acid B into tanshinol in shenxiong glucose injection preparation process |
| CN103145548A (en) * | 2013-03-27 | 2013-06-12 | 苏州市职业大学 | Method for rapidly separating and purifying tanshinol in salvia miltiorrhiza medicinal materials |
| CN104974033A (en) * | 2013-12-22 | 2015-10-14 | 贵州景峰注射剂有限公司 | Method for extracting tanshinol |
-
2015
- 2015-12-22 CN CN201510973247.6A patent/CN105461543A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289385A (en) * | 2008-06-12 | 2008-10-22 | 中国人民解放军第二军医大学 | Process for abstracting high-purity tanshinol form salvia |
| CN101289386A (en) * | 2008-06-12 | 2008-10-22 | 南京泽朗医药科技有限公司 | Method for preparing sodium tanshinol |
| CN101445451A (en) * | 2008-12-30 | 2009-06-03 | 合肥紫金医药科技有限公司 | Method for preparing high-purity salvianic acid A sodium |
| EP2415749A1 (en) * | 2009-03-30 | 2012-02-08 | Tianjin Tasly Pharmaceutical Co. Ltd. | New salvianolic acid compound l, preparation method and use thereof |
| 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 |
| CN103058854A (en) * | 2012-12-21 | 2013-04-24 | 贵州景峰注射剂有限公司 | Method for converting danshinolic acid B into tanshinol in shenxiong glucose injection preparation process |
| CN103145548A (en) * | 2013-03-27 | 2013-06-12 | 苏州市职业大学 | Method for rapidly separating and purifying tanshinol in salvia miltiorrhiza medicinal materials |
| CN104974033A (en) * | 2013-12-22 | 2015-10-14 | 贵州景峰注射剂有限公司 | Method for extracting tanshinol |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108362663A (en) * | 2018-04-18 | 2018-08-03 | 贵州景峰注射剂有限公司 | The extracting method of method of quality control and Sodium Danshensu in red sage root extract purification process |
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