CN100506223C - Comprehensive utilizing method for red sage root super critical extract remainder - Google Patents
Comprehensive utilizing method for red sage root super critical extract remainder Download PDFInfo
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- CN100506223C CN100506223C CNB2006100525344A CN200610052534A CN100506223C CN 100506223 C CN100506223 C CN 100506223C CN B2006100525344 A CNB2006100525344 A CN B2006100525344A CN 200610052534 A CN200610052534 A CN 200610052534A CN 100506223 C CN100506223 C CN 100506223C
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Abstract
The comprehensive utilizing method of supercritical extract remainder of red sage is to preparing dried secondary extractum with the extract remainder and through solvent extraction, decompression concentration, macroporous resin separation, dynamic vacuum drying and other technological steps. The dried secondary extractum contains total salvianolic acid up to 75-83 %. The present invention raises the utilization rate of red sage resource.
Description
Technical field
The present invention relates to a kind of method of comprehensive utilization of red sage root super critical extract remainder, belong to Chinese material medicine resource and utilize the field.
Background technology
Supercritical fluid technology is that modern Chinese medicine is made one of advanced technology, compares with the Chinese medicine traditional method, has the advantage of many uniquenesses.Because operative temperature is low, supercritical CO
2Pharmaceutically active ingredient was not destroyed during extraction can be preserved more in good condition, and time biochemistry does not take place.Therefore, be particularly suitable for those, easily extractions of oxidation Decomposition destructive composition strong to heat sensitivity.At present, supercritical CO
2Extraction Chinese medicine active substance is paid attention to widely and is paid close attention to, and wherein some has obtained industrial applications, for example, extracts the method for TANSHINONES from join pellet.Supercritical CO
2The advantage that technology is extracted TANSHINONES is, extraction time is fast, with short production cycle, constant product quality, and the content of extractum TANSHINONES can 50%, therefore, is subjected to the high evaluation of industry.The application of new technique improves the Chinese medicine manufacture level, also proposes a new research topic---and how reasonably to handle the raffinate of supercritical extraction, improve the utilization rate of medical material.
Up to the present, red sage root super critical extract remainder all is to handle as a kind of garbage.Except making an addition on a small quantity in the feedstuff, most of as fertilizer, economic worth is very cheap.In fact, supercritical CO
2The just part effective ingredient of extraction also has many useful materials still to stay in the raffinate, has the potentiality of secondary development.For example, the content of pressure differential self in supercritical extractum is lower, and major part is stayed in the raffinate.
Salvianolic acid is an aqueous soluble active constituent important in the Radix Salviae Miltiorrhizae, can pass through blood brain barrier, by number of ways performance pharmacological action.It is reported that salvianolic acid can increase the ischemic region cerebral blood flow, and the blood flow in normal blood supply district is not had influence, can not produce " stealing blood " phenomenon; Salvianolic acid has stronger antiplatelet aggregative activity and certain thrombolytic effect, but blood coagulation system is not had influence, no hemorrhage risk; Salvianolic acid has stronger antioxidation, removes the free radical effect, and its antioxidation strength ratio VITE is strong at least 100～200 times; Salvianolic acid has significant protective effect to the mitochondrial injury that anoxia causes, the dosage of its protection mitochondrial injury only is one of percentage of Folium Ginkgo extract EGB761, has high efficiency; In addition, salvianolic acid can be regulated intracellular calcium concentration, suppresses apoptotic generation etc.Therefore, salvianolic acid is the raw material of FUFANG DANSHEN PIAN and Danshen root injection.
Patent CN1425659A has proposed a kind of method of extracting salvianolic acid B from salvia piece.Because directly use red rooted salvia, cost of material is higher; Moreover, because use hydrochloric acid as acidulant, higher to the requirement for anticorrosion of equipment, the stainless steel equipment that pharmacy corporation is commonly used is all not all right at present, so industrial applications is restricted.In addition, patent CN1528756A has proposed the another kind of new method of extracting salvianolic acid B from red rooted salvia, and it comprises steps such as extraction, flocculation, precipitate with ethanol, extraction, chromatography, and process route is long, production cost is high and the product yield is low.Yet there are no bibliographical information about utilizing red sage root super critical extract remainder to prepare total salvianolic acid at present.
Summary of the invention
The present invention proposes and has studied a kind of comprehensive utilization red sage root super critical CO
2The new technique of raffinate, by to the solvent extraction of raffinate, concentrate, technical processs such as chromatography and dynamic vacuum drying, obtain the secondary extract dry product of Radix Salviae Miltiorrhizae.The content of total salvianolic acid reaches 75～83% (percentage by weights) in this drying thing.
The present invention realizes by following technical scheme:
(1) solvent extraction
With the solvent extraction of red sage root super critical extract remainder with 5～20 times, extracting mode can be traditional second extraction mode (intermittent mode), and each solvent load was advisable to soak raffinate, and extracting temperature is 40～100 ℃, serves as better with 60～90 ℃ wherein.Each extraction time is 2～6 hours, serves as better with 3～5 hours wherein.In order to save solvent load, also can adopt a jar group countercurrent extraction mode.Red sage root super critical extract remainder can be selected 10～15 times solvent extraction for use.Used solvent is the mixture of water or water and organic solvent, and organic solvent is selected in methanol, ethanol, glycerol or the acetone any for use.
(2) concentrate
Merge extractive liquid,, overanxious, remove solids wherein, in single-action or multi-effect vacuum evaporator, be concentrated to 2 times of red sage root super critical extract remainder volume, thickening temperature is 40～100 ℃, wherein is advisable with 50～60 ℃.
(3) chromatography
Concentrated solution is directly at macroporous resin adsorption chromatographic column upper prop, separate by chromatographic column, the draw ratio of chromatographic column is 1:5～1:20, use compound eluant eluting then, compound eluant is the mixture of water and a kind of organic solvent, organic solvent is selected in methanol, ethanol, glycerol or the acetone any for use, wherein is better with ethanol.Eluent directly reclaims solvent and obtains extractum.
(4) drying
Because most salvia-soluble effective ingredient are heat-sensitive substances, easy decomposes or rotten, therefore, drying mode is for guaranteeing that product quality is most important, the present invention adopts dynamic drying process to obtain dry extract, and reasonably baking temperature is 40～80 ℃, serves as better with 45～55 ℃ wherein.
The used Radix Salviae Miltiorrhizae raffinate of the present invention also can be selected liquid CO for use
2Radix Salviae Miltiorrhizae raffinate after the extraction.The form of used Radix Salviae Miltiorrhizae raffinate is a graininess or Powdered.
Step (3) extracting solution separates by chromatographic column through behind the concentrating under reduced pressure, and the draw ratio of chromatographic column can be selected 1:5～1:10 for use.Used solvent is the mixture of water or water and organic solvent, and organic solvent is selected in methanol, ethanol, glycerol or the acetone any for use.The content of organic solvent is 30-70% in the used compound eluant.
The invention has the beneficial effects as follows:
1, improves the value of red rooted salvia, comprehensively extracted the fat-soluble and water miscible effective ingredient of Radix Salviae Miltiorrhizae, promoted the utilization rate of natural resources of Chinese medicinal materials, met the development need that economizing type is produced.
2, reduce supercritical CO
2The cost of extraction by the secondary resource utilization, improves the competitiveness of supercritical fluid technology.Raffinate can't reach the such cleanliness factor of supercritical extraction because conventional solvent method extracts the back, and the value of Li Yonging is lower again.
3, the inventive method is reasonable in design, and is easy and simple to handle, and cost is low.
Description of drawings
Fig. 1 is the process chart of the inventive method.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1: accurately weighing 200 restrains Powdered red sage root super critical extract remainder, puts into 5 liters of flasks, adds 2 liters of purified water, and 80 ℃ are extracted twice, extract 3 hours at every turn, filter, and merging filtrate obtains 3.9 liters of extracting solution.60 ℃ are evaporated to 0.4 liter, and standing over night if any the precipitation elimination, obtains concentrated solution.Concentrated solution by 200 milliliters of macroporous resin adsorption chromatographic columns, is used 50% ethanol elution then, collect the active component that contains salvianolic acid B, obtain 200 milliliters of eluents, eluent reclaims solvent and obtains about 40 milliliters extractum through concentrating under reduced pressure.Adopt the dynamic vacuum seasoning that gained extractum is carried out drying, baking temperature is 45～55 ℃, obtains Radix Salviae Miltiorrhizae secondary extract dry product.By analysis, the content of total salvianolic acid reaches 80.5% in this drying thing.
Embodiment 2: accurately weighing 200 restrains the graininess red sage root super critical extract remainders, puts into 5 liters of flasks, adds 2 liters of purified water, and 70 ℃ are extracted twice, extract 5 hours at every turn, filter, and merging filtrate obtains 4.0 liters of extracting solution.80 ℃ are evaporated to 0.4 liter, and standing over night if any the precipitation elimination, obtains concentrated solution.Concentrated solution by 200 milliliters of macroporous resin adsorption chromatographic columns, is used 40% ethanol elution then, collect the active component that contains salvianolic acid B, obtain 200 milliliters of eluents, eluent reclaims solvent and obtains about 40 milliliters extractum through concentrating under reduced pressure.Adopt the dynamic vacuum seasoning that gained extractum is carried out drying, baking temperature is 70～80 ℃, obtains Radix Salviae Miltiorrhizae secondary extract dry product.By analysis, the content of total salvianolic acid reaches 80.0% in this drying thing.
Embodiment 3: accurately weighing 200 restrains the graininess red sage root super critical extract remainders, puts into 5 liters of flasks, adds 1.5 liters of purified water and 0.5 Hydrargyri Oxydum Rubrum ethanol (95% content), and 75 ℃ are extracted twice, extract 6 hours at every turn, filter, and merging filtrate obtains 3.9 liters of extracting solution.40～65 ℃ are evaporated to 0.4 liter, and standing over night if any the precipitation elimination, obtains concentrated solution.Concentrated solution by 200 milliliters of macroporous resin adsorption chromatographic columns, is used 70% ethanol elution then, collect the active component that contains salvianolic acid B, obtain 200 milliliters of eluents, eluent reclaims solvent and obtains about 40 milliliters extractum through concentrating under reduced pressure.Adopt the dynamic vacuum seasoning that gained extractum is carried out drying, baking temperature is 55～65 ℃, obtains Radix Salviae Miltiorrhizae secondary extract dry product.By analysis, the content of total salvianolic acid reaches 78.0% in the dry thing.
Embodiment 4: accurately weighing 200 restrains Powdered red sage root super critical extract remainder, puts into 5 liters of flasks, adds 1 liter of purified water and 1 liter of methanol, and reflux, extract, twice was extracted 4 hours at every turn, filters, and merging filtrate is handled extracting solution according to embodiment 1 described method.Obtain Radix Salviae Miltiorrhizae secondary extract dry product through concentrated, chromatography, concentrating under reduced pressure and drying.By analysis, the content of total salvianolic acid reaches 76.5% in the dry thing.
Embodiment 5: accurately weighing 800 restrains Powdered red sage root super critical extract remainder, puts into 4 * 1.5L jar group countercurrent extractor and carries out countercurrent extraction, obtains 4 liters of extracting solution.Extract solvent and follow-up processing method with embodiment 3, obtain Radix Salviae Miltiorrhizae secondary extract dry product.By analysis, the content of total salvianolic acid reaches 82.1% in the dry thing.
The Powdered red sage root super critical extract remainder of embodiment 6:5 kilogram is put into 100 liters of extraction pot, adds 45 liters of purified water and 5 Hydrargyri Oxydum Rubrum ethanol, and 80 ℃ are extracted twice, extract 3 hours at every turn, filter, and merging filtrate obtains about 90 liters extracting solution.Adopt double effect evaporator to be evaporated to about 10 liters, standing over night if any the precipitation elimination, obtains concentrated solution.With the macroporous resin adsorption chromatographic column of concentrated solution by 10 liters, use 35% ethanol elution then, collect the active component that contains salvianolic acid B, obtain 12 liters of eluents, eluent reclaims solvent and obtains about 1 liter extractum through concentrating under reduced pressure.Adopt the dynamic vacuum seasoning that gained extractum is carried out drying, obtain Radix Salviae Miltiorrhizae secondary extract dry product.By analysis, the content of total salvianolic acid reaches 83.0% in this drying thing.
Claims (9)
1, a kind of method of comprehensive utilization of red sage root super critical extract remainder, it is characterized in that: by to the solvent extraction of red sage root super critical extract remainder, concentrate, chromatography and dynamic vacuum drying, obtain the secondary extract dry product of Radix Salviae Miltiorrhizae, the weight percentage of total salvianolic acid is 75～83% in this drying thing, and used Radix Salviae Miltiorrhizae raffinate is selected liquid CO for use
2Radix Salviae Miltiorrhizae raffinate after the extraction, concrete steps are:
(1) solvent extraction
With the solvent extraction of red sage root super critical extract remainder with 5～20 times, extracting mode is selected intermittent mode for use, and each solvent load soaked raffinate, and extracting temperature is 40～100 ℃, and extraction time is 2～10 hours;
(2) concentrate
Merge extractive liquid,, overanxious, remove solids wherein, in single-action or multi-effect vacuum evaporator, be concentrated to 2 times of red sage root super critical extract remainder volume, thickening temperature is 40～100 ℃;
(3) chromatography
Concentrated solution separates by chromatographic column directly at macroporous resin adsorption chromatographic column upper prop, uses compound eluant eluting then, and compound eluant is the mixture of water and a kind of organic solvent, and eluent directly reclaims solvent and obtains extractum;
(4) drying
Adopt dynamic drying means to obtain dry extract, baking temperature is 40～80 ℃.
2, according to the method for comprehensive utilization of right 1 described red sage root super critical extract remainder, it is characterized in that: red sage root super critical extract remainder is selected 10～15 times solvent extraction for use in the step (1).
3, according to the method for comprehensive utilization of right 1 described red sage root super critical extract remainder, it is characterized in that: the used solvent of step (1) is the mixture of water or water and organic solvent, and organic solvent is selected in methanol, ethanol, glycerol or the acetone any for use.
4, according to the method for comprehensive utilization of right 1 described red sage root super critical extract remainder, it is characterized in that: the used extracting mode of step (1) is selected a jar group countercurrent extraction mode for use.
5, according to the method for comprehensive utilization of right 1 described red sage root super critical extract remainder, it is characterized in that: the form of the used Radix Salviae Miltiorrhizae raffinate of step (1) is a graininess or Powdered.
6, according to right 1 described Radix Salviae Miltiorrhizae raffinate method of comprehensive utilization, it is characterized in that: step (3) extracting solution separates by chromatographic column through behind the concentrating under reduced pressure, and the draw ratio of chromatographic column is 1:5～1:20.
7, according to right 1 or 7 described Radix Salviae Miltiorrhizae raffinate method of comprehensive utilization, it is characterized in that: the draw ratio of chromatographic column is 1:5～1:10.
8, according to the method for comprehensive utilization of right 1 described red sage root super critical extract remainder, it is characterized in that: the used solvent of step (3) is the mixture of water and organic solvent, and organic solvent is selected in methanol, ethanol, glycerol or the acetone any for use.
9, according to the method for comprehensive utilization of right 1 described red sage root super critical extract remainder, it is characterized in that: the content of organic solvent is 30-70% in the used compound eluant of step (3).
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| CN100506223C true CN100506223C (en) | 2009-07-01 |
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Non-Patent Citations (4)
| Title |
|---|
| 加热方式对丹酚酸提取物质量的影响. 倪力军，邬科芳，张立国.中药新药与临床药理，第17卷第1期. 2006 |
| 加热方式对丹酚酸提取物质量的影响. 倪力军，邬科芳，张立国.中药新药与临床药理，第17卷第1期. 2006 * |
| 超临界萃取结合水煎煮法提取丹参中有效成分的研究. 张，虹，柳正良，王洪泉，杨，莺.中草药，第35卷第12期. 2004 |
| 超临界萃取结合水煎煮法提取丹参中有效成分的研究. 张，虹，柳正良，王洪泉，杨，莺.中草药，第35卷第12期. 2004 * |
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