CN1927265A - Process for increasing cryptotanshinone content in Danshen extract - Google Patents
Process for increasing cryptotanshinone content in Danshen extract Download PDFInfo
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- CN1927265A CN1927265A CN 200610127340 CN200610127340A CN1927265A CN 1927265 A CN1927265 A CN 1927265A CN 200610127340 CN200610127340 CN 200610127340 CN 200610127340 A CN200610127340 A CN 200610127340A CN 1927265 A CN1927265 A CN 1927265A
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- salvia miltiorrhiza
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Abstract
The invention discloses a method to increase the content of cryptotanshinone in salvia miltiorrhiza extract, the method includes the following steps: Salvia miltiorrhiza is extracted with ethanol solution by recirculation percolating and salvia miltiorrhiza ethanol extracts is obtained; remove tannins in the obtained extracts, salvia miltiorrhiza ethanol extracts with tanning removal is got, the obtained salvia miltiorrhiza ethanol extracts with tanning removal is recovered once, second recovery is done after the first one, After the second reduction, o salvia miltiorrhiza ethanol extracts is oxidized. The salvia miltiorrhiza (total) ketone content of the products got using the invention method and its cryptotanshinone content is significantly higher than that of the product using existing technology approaches, the method will create tremendous economic benefits, moreover the requirement of the variety of salvia miltiorrhiza is unstrict, and the method is simple.
Description
Technical Field
The invention relates to a method for extracting and processing traditional Chinese medicines, in particular to a method for extracting and processing salvia miltiorrhiza bunge, which can obviously improve the content of cryptotanshinone in the salvia miltiorrhiza bunge extract.
Background
Salvia miltiorrhiza is a traditional Chinese medicinalmaterial. With the development and improvement of extraction and separation processes, the pharmacological actions of the salvia miltiorrhiza extract and various components in the salvia miltiorrhiza extract are gradually clear. The salvia miltiorrhiza can be extracted by using an organic solvent such as alcohol, ether and the like, the extract contains a plurality of effective components, wherein the fat-soluble components are generally called salvianone (total) ketone, are basically phenanthrenequinone substances with sterilization and bacteriostasis functions, and mainly comprise ten monomer components, namely cryptotanshinone, dihydrotanshinone I, hydroxytanshinone IIA, tanshinone IIB, methyl salvianate, tanshinone IIA, salvianic acid neoquinone A, salvianic acid neoquinone B and salvianic acid neoquinone C. The antibacterial ability of the salvia miltiorrhiza (total) ketone is more than 10 times higher than that of the berberine, and the salvia miltiorrhiza (total) ketone still has effect on a plurality of drug-resistant staphylococcus aureus.
Among the ten substances, cryptotanshinone, which has the strongest bactericidal activity; in addition, the tanshinone IIA has the functions of resisting bacteria, inhibiting bacteria and killing bacteria, resisting oxidation and increasing arterial blood flow, can treat coronary heart disease, improve coronary artery circulation and inhibit thrombus diseases, and cryptotanshinone is a precursor of the tanshinone IIA and can be converted into the tanshinone IIA in a human body, so that the cryptotanshinone has double pharmacological functions on the human body. The excellent pharmacological action of cryptotanshinone attracts great attention of researchers and producers. Many researchers have tried to increase the cryptotanshinone content in salvia miltiorrhiza extracts or total ketones of salvia miltiorrhiza.
In fact, the monomeric substances of tanshinone can be interconverted, for example
In the existing method for extracting the salvia miltiorrhiza, the content of cryptotanshinone in the finally obtained extract can only reach about 10 percent.
Therefore, there is a strong need to provide an extraction method capable of increasing the content of cryptotanshinone in the salvia miltiorrhiza bunge extract.
Disclosure of Invention
The invention aims to provide a method for improving the content of cryptotanshinone in a salvia miltiorrhiza extract, which can obviously improve the content of cryptotanshinone in the obtained extract.
The purpose of the invention is realized by the following technical scheme.
The invention provides a method for improving the content of cryptotanshinone in a salvia miltiorrhiza extract, which comprises the following steps: extracting Saviae Miltiorrhizae radix with ethanol under reflux by percolation to obtain ethanol extractive solution of Saviae Miltiorrhizae radix; removing tannin from the obtained extractive solution to obtain ethanol extractive solution of Saviae Miltiorrhizae radix; performing primary reduction on the tanned ethanol extract of the salvia miltiorrhiza; carrying out secondary reduction on the extracting solution after the primary reduction; oxidizing the ethanol extract of the salvia miltiorrhiza after the secondary reduction. The method can also comprise concentrating, desalting and drying the oxidized extractive solution.
The method for improving the content of cryptotanshinone in the salvia miltiorrhiza bunge extract preferably further comprises the pretreatment processes of cleaning, moistening, slicing and drying the salvia miltiorrhiza bunge. If the salvia miltiorrhiza is pretreated by using a crushing mode, a large amount of salvia miltiorrhiza dander dandruff dust is generated. In fact, the exocarp fraction of salvia miltiorrhiza is the most abundant in tanshinone (total) ketone, especially tanshinone IIA. However, as can be seen by referring to the context, the present application primarily increases the cryptotanshinone content in the product by utilizing the conversion of tanshinone IIA to cryptotanshinone. If the dander dust is extracted by ethanol in a backflow way, the dander dust is accumulated together to cause that the solution cannot permeate at all, so the dander dust only needs to be discarded, thereby causing great waste and great loss of effective components. If the salvia miltiorrhiza is cleaned, moistened, sliced and dried in the sun, the generated scurf dust is obviously reduced, thereby improving the utilization rate of the raw materials.
The salvia miltiorrhiza used in the invention can be fresh salvia miltiorrhiza or dried salvia miltiorrhiza. The specific variety of Salvia miltiorrhiza is not limited at all.
In the method for improving the content of cryptotanshinone in the salvia miltiorrhiza bunge extract, the ethanol solution is used for reflux percolation extraction, and the tanshinone can be extracted to the maximum extent in a short time by the reflux percolation extraction. Theoretically, the medicinal materials can be extracted for 1.67 ten thousand times, and the liquid outlet amount is small. Compared with the existing method for decocting and extracting for 3-4 times by using ethanol, the method has the advantages of less solvent consumption, high extraction efficiency, rapid subsequent solvent evaporation treatment and other procedures, and low energy consumption. The concentration of the ethanol solution used for extraction is not particularly limited, as long as it is an aqueous solution of ethanol. However, in view of the extraction efficiency and cost, the concentration of the ethanol solution used is preferably not higher than 95%, more preferably 40 to 95%, and still more preferably 65 to 95%.
In the method for improving the content of cryptotanshinone in the salvia miltiorrhiza bunge extract, alkali is added into the ethanol extract of the salvia miltiorrhiza bunge to salt tannin in the extract, and the tannin is separated out from the extract due to low solubility of the tannin. The base to be added may be a common base such as sodium hydroxide, potassium hydroxide, calcium hydroxide, etc., and is not particularly limited. In view of the complexity of the subsequent treatment process and the compatibility with the physiological conditions of the human body, sodium hydroxide and potassium hydroxide are preferably used, and sodium hydroxide is most preferably used. Removing tannin from ethanol extract of Saviae Miltiorrhizae radix with alkali, adjusting to neutral with acid, and performing the following treatment process. The acid used may be an organic acid or an inorganic acid, and is not particularly limited. However, hydrochloric acid is preferably used in view of the subsequent treatment process.
In the method for increasing the content of cryptotanshinone in the salvia miltiorrhiza extract, the primary reduction process is carried out by using a hydrogenation catalytic reducing agent with adsorbability, for example, a mixture of activated α or η aluminium oxide powder and activated carbon powder is used, the ineffective componentsin the extracting solution are removed through the adsorption of activated carbon and aluminium oxide, for example, mainly unremoved tannin, and the oxidizing substances in the extracting solution are primarily reduced by the hydrogenation catalytic action of α or η aluminium oxide.
In the method for improving the content of cryptotanshinone in the salvia miltiorrhiza bunge extract, the secondary reduction process is to use the catalyst with hydrogenation catalysis to carry out deep hydrogenation reduction on the extracting solution, so that the oxidizing substances in the extracting solution are basically converted into reducing substances, such as cryptotanshinone. The hydrogenation reduction catalyst used is a conventional hydrogenation reduction catalyst, and is not particularly limited. For example, a catalyst such as palladium carbon, platinum carbon, chitin-palladium, raney nickel, or the like can be used.
The secondary reduction can be carried out at normal temperature and normal pressure, so the requirement on equipment is very low, and a conventional hydrogenation catalyst can be used.
The oxidation process of the method for improving the content of cryptotanshinone in the salvia miltiorrhiza bunge extract is to remove hydrogen combined with an o-keto group during hydrogenation reduction. The oxidation may be carried out by contacting the extract with an oxygen-containing gas, such as air, for example by passing air through the extract.
In the method for improving the content of cryptotanshinone in the salvia miltiorrhiza extract, the concentration process is to remove ethanol in the extracting solution and recover ethanol in constant volume, thereby obtaining thick paste mainly containing tanshinone (total) ketone.
In the method for increasing the content of cryptotanshinone in the salvia miltiorrhiza bunge extract of the present invention, the desalting process is performed to remove salt generated in the previous treatment process, and can be performed by using a conventional desalting method, such as washing with hot water.
In the method for improving the content of cryptotanshinone in the salvia miltiorrhiza extract, the thick paste of the extract can be dried in the drying process, so that the extract is easy to store and preserve.
The term "tanshinones" as used herein refers to the general term for phenanthraquinones extracted from Salvia miltiorrhiza with an ethanol solution, and includes cryptotanshinone.
The invention improves the content of cryptotanshinone in the salvia miltiorrhiza extract by improving the utilization rate of the raw medicinal materials and utilizing the interconversion relationship of the active ingredients in the total tanshinone, in particular the interconversion relationship of cryptotanshinone and tanshinone IIA.
The method for improving the content of the cryptotanshinone in the salvia miltiorrhiza extract has the advantages that the content of the tanshinone (total) in the obtained product and the content of the cryptotanshinone in the obtained product are obviously higher than those of the product obtained by the method in the prior art, the method can create huge economic benefit, the requirement on the variety of the salvia miltiorrhiza medicinal material is loose, and the method is simple.
Compared with the supercritical extraction method by using carbon dioxide, the method has extremely low cost and is easy for industrialized mass production.
Detailed Description
The invention is further described below with reference to examples. The features and advantages of the presentinvention will become more apparent as the description proceeds. These illustrative examples are merely illustrative of the present invention and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that equivalent substitutions for details and descriptions of the methods described herein may be made without departing from the spirit and scope of the invention.
Example 1
20kg of salvia miltiorrhiza root which is newly harvested for 2 years is taken, cleaned, cut off the soil, cut off the reed head, cut into slices with the thickness of about 0.5cm by a medicine cutting machine, dried in the sun, sieved by a 10-mesh sieve, and left for use, so as to obtain 12kg of dry decoction pieces.
Placing the decoction pieces into a Soxhlet extractor, placing the dandruff at the top, adding 70L 95% ethanol to immerse the decoction pieces, heating to 50 deg.C, maintaining the temperature for 3 hr, heating to 90 deg.C, reflux-extracting for 3 hr, controlling the outflow rate of the extractive solution to make the ethanol solution always immerse the decoction pieces, stopping reflux when the extractive solution is nearly colorless, and discharging the extractive solution completely.
Under stirring, 20% sodium hydroxide solution was added to the above extract to adjust the pH to 10, the stirring was stopped, the mixture was allowed to stand for 4 hours to precipitate, the precipitate was removed by filtration, and 10% hydrochloric acid was added dropwise to the filtrate to adjust the pH of the solution to 7.
Mixing 0.7kg of η type aluminum oxide powder activated at 400 ℃ in advance with 0.07kg of activated carbon powder activated at 120 ℃, loading the mixture into a column filter, saturating the mixture with hydrogen for 0.5 hour, slowly adding the neutralized filtrate at the flow rate of 5ml/cm 2. min, introducing hydrogen from below every 5min to disperse a filter layer after η type aluminum oxide becomes dark and dense until the neutralized filtrate completely passes through, washing the filter layer once with 10L of 95% ethanol, and combining the filter layer with the filtrate.
And (3) passing the obtained filtrate through a reciprocating hydrogenation catalyst filled with a CT-Pd catalyst, and reducing until hydrogen is not consumed any more.
And (3) introducing air into the reducing solution, rotationally stirring for 0.5 hour, transferring the obtained liquid substance into an ethanol recovery tower, and recovering 78L of ethanol in constant volume to obtain the total ketone of the salvia miltiorrhiza thick paste.
Adding the above soft extract into jacketed kettle containing hot water, heating to 90 deg.C, stirring, washing with water until the water washing solution contains no Cl-.
Taking out the thick paste, spreading on a baking pan, draining off water, and drying at 55 deg.C to obtain 0.3kg of Saviae Miltiorrhizae radix (total) ketone extract with cryptotanshinone content of 27%.
Example 2
Taking 15kg of dried salvia miltiorrhiza root, washing soil with clear water, cutting off the reed head, cutting into slices with the thickness of about 0.3cm by using a medicine cutting machine, drying in the sun, sieving by using a 10-mesh sieve, and keeping skin scraps for use to obtain 12kg of dried decoction pieces.
Putting the decoction pieces into a Soxhlet extractor, putting the scurf at the top, adding 70L 95% ethanol, heating to 50 deg.C, keeping the temperature for 3 hours, slowly putting into an evaporator, stopping liquid discharge when the ethanol just passes through the decoction pieces, heating the evaporator to 90 deg.C, reflux-extracting, adjusting the outflow rate of the extractive solution and the evaporation capacity of the evaporator, keeping the ethanol solution immersed in the decoction pieces all the time, refluxing for about 3 hours, stopping reflux when the extractive solution is nearly colorless, and discharging the extractive solution completely.
Under stirring, 20% sodium hydroxide solution was added to the above extract to adjust the pH to 9, the stirring was stopped, the mixture was allowed to stand for 4 hours to precipitate, the precipitate was removed by filtration, and 10% hydrochloric acid was added dropwise to the filtrate to adjust the pH of the solution to 7.
0.7kg of η type aluminium oxide powder activated at 350 ℃ and 0.07kg of activated carbon powder activated at 120 ℃ are mixed uniformly, the mixture is put into a column filter and is saturated by hydrogen for 0.5 hour, then the neutralized filtrate is slowly added, the flow rate is 5ml/cm 2. min, when the color of η type aluminium oxide becomes dark and compact, hydrogen is introduced from the lower part every 5min to disperse a filter layer until the neutralized filtrate completely passes through, the filter layer is washed once by 10L of 95% ethanol and is combined with the filtrate.
And (3) reducing the obtained filtrate by a reciprocating hydrogenation catalyst filled with a Raney nickel catalyst until the hydrogen is not consumed any more.
And (3) introducing air into the reducing solution, rotationally stirring for 0.5 hour, transferring the obtained liquid substance into an ethanol recovery tower, and recovering 78L of ethanol in constant volume to obtain the total ketone of the salvia miltiorrhiza thick paste.
Adding the above soft extract into jacketed kettle containing hot water, heating to 90 deg.C, stirring, washing with water until the water washing solution contains no Cl-.
Taking out the thick paste, spreading on a baking pan, draining off water, and drying at 55 deg.C to obtain 0.24kg of Saviae Miltiorrhizae radix (total) ketone extract with cryptotanshinone content of 26.2%.
Claims (10)
1. A method for increasing the content of cryptotanshinone in a salvia miltiorrhiza extract comprises the following steps: extracting Saviae Miltiorrhizae radix with ethanol under reflux by percolation to obtain ethanol extractive solution of Saviae Miltiorrhizae radix; removing tannin from the obtained extractive solution to obtain ethanol extractive solution of Saviae Miltiorrhizae radix; performing primary reduction on the tanned ethanol extract of the salvia miltiorrhiza; carrying out secondary reduction on the extracting solution after the primary reduction; oxidizing the ethanol extract of the salvia miltiorrhiza after the secondary reduction.
2. The method of claim 1, further comprising concentrating, desalting and drying the oxidized extract.
3. The method as claimed in claim 1 or 2, further comprising a pretreatment process of washing, moistening, slicing and sun-drying the salvia miltiorrhiza bunge.
4. The method according to any one of claims 1 to 3, wherein the ethanol solution used for the reflux extraction has a concentration of not higher than 95%.
5. A method according to any one of claims 1 to 3, wherein the tannin is removed by salting out the tannin by adding a base to an ethanol extract of Salvia miltiorrhiza.
6. The method of claim 5, wherein the base is sodium hydroxide.
7. The method according to any one of claims 1 to 3, wherein the primary reduction is carried out by using a hydrogenation catalytic reducing agent having adsorptivity, or the primary reduction process is carried out using only an adsorbable substance and not a hydrogenation reduction catalyst, i.e. only adsorption and not reduction are carried out.
8. A method according to any one of claims 1 to 3, characterized in that the secondary reduction process is carried out by using a catalyst having a hydrogenation catalytic action.
9. The method of claim 8, wherein the catalyst is palladium on carbon, platinum on carbon, chitin-palladium, or raney nickel.
10. A method according to any of claims 1-3, characterized in that the oxidation process is carried out by contacting the extract with an oxygen-containing gas.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101273406A CN100542551C (en) | 2006-09-14 | 2006-09-14 | Improve the method for cryptotanshinone content in the Radix Salviae Miltiorrhizae extract |
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| CNB2006101273406A CN100542551C (en) | 2006-09-14 | 2006-09-14 | Improve the method for cryptotanshinone content in the Radix Salviae Miltiorrhizae extract |
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| CN100542551C CN100542551C (en) | 2009-09-23 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2453807A (en) * | 2007-10-15 | 2009-04-22 | Botan Century | Purified tanshinone extracts from Salvia spp and their antibacterial effects |
| CN101584786B (en) * | 2009-07-11 | 2012-10-03 | 刘秀英 | Chinese materia medica preparation for treating chronic renal insufficiency |
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2006
- 2006-09-14 CN CNB2006101273406A patent/CN100542551C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2453807A (en) * | 2007-10-15 | 2009-04-22 | Botan Century | Purified tanshinone extracts from Salvia spp and their antibacterial effects |
| US9283256B2 (en) | 2007-10-15 | 2016-03-15 | Botanic Century (Beijing) Co. Ltd. | Antibacterial composition comprising Salvia extracts |
| CN101584786B (en) * | 2009-07-11 | 2012-10-03 | 刘秀英 | Chinese materia medica preparation for treating chronic renal insufficiency |
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| CN100542551C (en) | 2009-09-23 |
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