CN101759673A - Method for extracting salvianolic acid B from fresh salvia miltiorrhiza - Google Patents
Method for extracting salvianolic acid B from fresh salvia miltiorrhiza Download PDFInfo
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- CN101759673A CN101759673A CN200910233836A CN200910233836A CN101759673A CN 101759673 A CN101759673 A CN 101759673A CN 200910233836 A CN200910233836 A CN 200910233836A CN 200910233836 A CN200910233836 A CN 200910233836A CN 101759673 A CN101759673 A CN 101759673A
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- salvianolic acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a method for extracting salvianolic acid B, which has low cost, large yield and short period and is easy to realize industrialization. The process comprises the following steps: squeeze extracting, membrane concentrating and spray drying. The method for preparing the salvianolic acid B has the advantages of simple process, less energy consumption and easy production enlargement.
Description
Technical field:
The present invention relates to the extraction and purification process of salvianolic acid B, particularly a kind of method of extracting the purifying salvianolic acid B from the fresh red sage root.
Background technology:
The red sage root (Salvia miliiorrhiza Bunge) belongs to the Labiatae clary, be used as medicine with root, have effects such as promoting blood circulation to remove blood stasis, menstruction regulating and pain relieving, heat clearing and tranquillizing, be traditional Chinese medical science drug for invigorating blood circulation and eliminating stasis commonly used and treat coronary heart disease clinically and anginal specific medicament.The pharmacological component that extracts in the red sage root has a variety of, can be divided into fat-soluble and water-soluble two classes.Aqueous soluble active constituent is mainly phenolic acids, as salvianolic acid B (3,4 dihydroxy phenyl lactic acid), coffic acid, alkannic acid, Protocatechualdehyde, etc., have pharmacological action widely, wherein salvianolic acid B has its special efficacy again.
Its molecular formula and relative molecular weight: C
36H
28O
16, 718.62, molecular structure:
Salvianolic acid B is a phenolic acid, and red sage root acid B is formed by the Salvianic acidA of 3 molecules and the coffic acid condensation of 1 molecule, and in decoction, concentration process, the small part hydrolysis generates alkannic acid and Salvianic acidA, and a part of Salvianic acidA becomes rosmarinic acid under acidic conditions; Salvianolic acid A, C can changes in solution etc., see the light oxygenolysis easily of being heated under the acid-base condition all.
Content of danshinolic acid B is than height, general 3%～5% in the red sage root.And content of danshinolic acid B is between 4～6% in the fresh red sage root, and salvianolic acid B loses in a large number in the airing process.The method that extraction purifying salvianolic acid B generally uses has: water extraction method, ethanol refluxing process, water extraction and alcohol precipitation method, liquid-liquid extraction method etc.Though microwave, ultrasonic wave, etc. supplementary means can make the higher extracted rate that obtains, but these methods exist shortcomings such as energy consumption is big, seriously polluted, the organic reagent kind is many, the cycle is long, loss of effective components is big keeping aspects such as effective constituent, removal invalid components.The method of extracting the purifying salvianolic acid B as patent CN1164582 is that conventional the extraction concentrates, the big cost height of energy consumption; CN1240695 extraction preparation salvianolic acid B not only energy consumption yields poorly greatly but also has multiple organic reagent to use, and causes difficulty for recovery reagent, and difficult the amplification produces.
Summary of the invention:
The objective of the invention is in order to provide a kind of production technique simple, energy consumption is few, and cost is low, and salvianolic acid B purity is greater than 50%, and yield is more than 90%, and output is big, and the cycle is short, is easy to realize industrialized salvianolic acid B extraction process.
The object of the present invention is achieved like this:
1) squeezing is extracted: the fresh red sage root is pulverized, added deionized water and soak, cold pressing under 80～100MPa, residue is repeated to soak squeezing once, merge the pressed liquor that obtains for twice.
Salvianolic acid B is heated and sees photo-labile, and loss can be up to 70% in the dryness in the sun process, even decomposes loss fully, and extracting the used red sage root of salvianolic acid B both at home and abroad at present all is the dried red sage root.And this technology is used the fresh red sage root, and salvianolic acid B can not lose because the airing operation is arranged.
According to salvianolic acid B character soluble in water, squeezing can be taken out of with original moisture under the normal temperature, introduces impurity so can save other solvents of use herein.High-pressure compressing can extract the water miscible salvianolic acid B that has in the red sage root more up hill and dale, destroys red sage root weave construction by mechanical effect under normal temperature condition, but does not relate to chemical transformation, makes things convenient for next step purification operations.
The above-mentioned method of extracting the purifying salvianolic acid B from the fresh red sage root is characterized in that the raw material pulverizing granularity is 20～60 orders, and amount of water is 1～2: 1 than red sage root weight, soak time 1～2 hour.
The above-mentioned method of extracting the purifying salvianolic acid B from the fresh red sage root is characterized in that squeezing is extracted as twice, and squeezing machine filter grit number is 300～400 orders.
2) membrane sepn: above-mentioned pressed liquor is held back macromolecular substance by ultrafiltration membrane system earlier, collects to see through liquid, concentrate with the nanofiltration membrane concentration systems, concentrated solution;
Membrane sepn and enrichment process are according to the salvianolic acid B molecular weight, and earlier the ultra-filtration membrane filtering system with molecular weight cut-off 1000～3000 removes macromole impurity and colored component, then follow-up the needs with gac the feed liquid processing of decolouring again; Hold back salvianolic acid B at normal temperatures with the nanofiltration membrane system again, play concentrated and purified purpose.
The above-mentioned method of extracting the purifying salvianolic acid B from the fresh red sage root is characterized in that ultrafiltration, nanofiltration that described salvianolic acid B separates in concentrating all carry out at normal temperatures.
The above-mentioned method of extracting the purifying salvianolic acid B from the fresh red sage root is characterized in that it is that 1000～3000 ultra-filtration membrane and molecular weight cut-off are 500～600 nanofiltration membrane that described ultra-filtration membrane uses molecular weight cut-off.
3) spraying drying: concentrated solution enters the spray-drying tower drying, promptly.
In sum, there is following advantage in the present invention:
1) adopts the fresh red sage root, reduced the loss of salvianolic acid B in the airing process.
2) adopt the squeezing machine squeezing, this process is physical change, does not need heating, and salvianolic acid B can not lose, and physical strength is big, can extract salvianolic acid B fully again, contg fat-soluble substances not, the content of easier raising salvianolic acid B.
3) the membrane sepn process also is a physical process, need not heating and adds chemical reagent, carries out at normal temperature, has guaranteed the yield height of salvianolic acid B.
4) spraying drying speed is fast, especially to heat-sensitive substance, and can be in drying process content loss, solubility property is good.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Get the fresh red sage root of 50kg (content of danshinolic acid B 4%), pulverize 20 orders, add the 50L deionized water and soaked 1 hour, be forced into the 80MPa squeezing in the squeezing machine of packing into, the same terms is soaked squeezing once again, merge pressed liquor, filter, remove macromole impurity by the ultrafiltration membrane system of molecular weight cut-off 1000 earlier, collect and see through liquid, see through liquid and concentrate with the nanofiltration membrane of molecular weight cut-off 600 again, collect concentrated solution and carry out spraying drying, finally obtain 3.55kg content and be 53% salvianolic acid B finished product.
Embodiment 2:
Get the fresh red sage root of 50kg (content of danshinolic acid B 5%), pulverize 60 orders, add the 75L deionized water and soaked 1.5 hours, be forced into the 90MPa squeezing in the squeezing machine of packing into, the same terms is soaked squeezing once again, merge pressed liquor, filter, remove macromole impurity by the ultrafiltration membrane system of molecular weight cut-off 2000 earlier, collect and see through liquid, see through liquid and concentrate with the nanofiltration membrane of molecular weight cut-off 600 again, collect concentrated solution and carry out spraying drying, finally obtain 4.05kg content and be 56% salvianolic acid B finished product.
Embodiment 3:
Get the fresh red sage root of 60kg (content of danshinolic acid B 4%), pulverize 60 orders, add the 120L deionized water and soaked 2 hours, be forced into the 100MPa squeezing in the squeezing machine of packing into, the same terms is soaked squeezing once again, merge pressed liquor, filter, remove macromole impurity by the ultrafiltration membrane system of molecular weight cut-off 3000 earlier, collect and see through liquid, see through liquid and concentrate by the nanofiltration membrane of molecular weight cut-off 500 again, collect concentrated solution and carry out spraying drying, finally obtain 4.20kg content and be 52% salvianolic acid B finished product.
Claims (6)
1. method of extracting the purifying salvianolic acid B from the fresh red sage root is characterized in that comprising following step:
1) squeezing is extracted: the fresh red sage root is pulverized, added deionized water and soak, cold pressing under 80～100MPa, residue is repeated to soak squeezing once, merge the pressed liquor that obtains for twice;
2) membrane sepn: above-mentioned pressed liquor filters, and elder generation holds back macromolecular substance by ultrafiltration membrane system, collects to see through liquid, concentrates with the nanofiltration membrane concentration systems, gets concentrated solution;
3) spraying drying: concentrated solution enters the spray-drying tower drying, promptly.
2. according to the described method of from the fresh red sage root, extracting the purifying salvianolic acid B of claim 1, it is characterized in that described raw material is the fresh red sage root,
3. according to the described method of extracting the purifying salvianolic acid B from the fresh red sage root of claim 1, it is characterized in that described pulverizing soaking conditions is: grinding particle size is 20～60 orders, and amount of water is 1～2: 1 than red sage root weight, soak time 1～2 hour.
4. according to the described method of from the fresh red sage root, extracting the purifying salvianolic acid B of claim 1, it is characterized in that described squeezing is extracted as twice immersion squeezing.
5. according to the described method of from the fresh red sage root, extracting the purifying salvianolic acid B of claim 1, it is characterized in that ultrafiltration in the described membrane sepn, nanofiltration all carry out at normal temperatures.
6. according to the described method of extracting the purifying salvianolic acid B from the fresh red sage root of claim 1, it is characterized in that the ultra-filtration membrane of the optional molecular weight cut-off 1000～3000 of ultra-filtration membrane in the described membrane sepn, the optional molecular weight cut-off of nanofiltration membrane is 500～600 nanofiltration membrane.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910233836A CN101759673A (en) | 2009-10-22 | 2009-10-22 | Method for extracting salvianolic acid B from fresh salvia miltiorrhiza |
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| CN200910233836A CN101759673A (en) | 2009-10-22 | 2009-10-22 | Method for extracting salvianolic acid B from fresh salvia miltiorrhiza |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102475739A (en) * | 2010-11-24 | 2012-05-30 | 上海医药工业研究院 | Radix Salviae Miltiorrhizae water extract and preparation method thereof |
| CN106631767A (en) * | 2017-01-04 | 2017-05-10 | 南京中医药大学 | Method for high-efficiency enrichment of phenolic acid components in traditional Chinese medicine through nanofiltration |
| CN108148028A (en) * | 2016-12-06 | 2018-06-12 | 复旦大学 | A kind of method of tanshin polyphenolic acid B ingredient in extraction salviamiltiorrhizabung |
| CN109810082A (en) * | 2019-01-22 | 2019-05-28 | 江苏德泽生物科技有限公司 | A kind of extraction separation method of tanshin polyphenolic acid B |
-
2009
- 2009-10-22 CN CN200910233836A patent/CN101759673A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102475739A (en) * | 2010-11-24 | 2012-05-30 | 上海医药工业研究院 | Radix Salviae Miltiorrhizae water extract and preparation method thereof |
| CN102475739B (en) * | 2010-11-24 | 2014-12-31 | 上海医药工业研究院 | Radix Salviae Miltiorrhizae water extract and preparation method thereof |
| CN108148028A (en) * | 2016-12-06 | 2018-06-12 | 复旦大学 | A kind of method of tanshin polyphenolic acid B ingredient in extraction salviamiltiorrhizabung |
| CN106631767A (en) * | 2017-01-04 | 2017-05-10 | 南京中医药大学 | Method for high-efficiency enrichment of phenolic acid components in traditional Chinese medicine through nanofiltration |
| CN106631767B (en) * | 2017-01-04 | 2019-03-19 | 南京中医药大学 | A kind of method of nanofiltration efficiently concentrating Chinese medicine liposoluble ingredient |
| CN109810082A (en) * | 2019-01-22 | 2019-05-28 | 江苏德泽生物科技有限公司 | A kind of extraction separation method of tanshin polyphenolic acid B |
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Application publication date: 20100630 |