CN101759555A - Method for extracting and purifying salvianic acid A from fresh salvia miltiorrhiza - Google Patents
Method for extracting and purifying salvianic acid A from fresh salvia miltiorrhiza Download PDFInfo
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- CN101759555A CN101759555A CN200910233835A CN200910233835A CN101759555A CN 101759555 A CN101759555 A CN 101759555A CN 200910233835 A CN200910233835 A CN 200910233835A CN 200910233835 A CN200910233835 A CN 200910233835A CN 101759555 A CN101759555 A CN 101759555A
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- red sage
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- salvianic acida
- exchange resin
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Abstract
The invention relates to a method for extracting and purifying salvianic acid A, which has low cost, large yield and short period and is easy to realize industrialization. The process comprises the following steps: squeezing, iron exchange resin adsorbing, membrane concentrating and spray drying. The method for preparing the salvianic acid A has the advantages of simple process, less energy consumption and high purity.
Description
Technical field:
The present invention relates to the extraction and purification process of Salvianic acidA, particularly a kind of method of extracting the purifying Salvianic acidA 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 portions.Aqueous soluble active constituent is mainly phenolic acids, as Salvianic acidA (3,4 dihydroxy phenyl lactic acid), coffic acid, alkannic acid, Protocatechualdehyde, salvianolic acid B etc., has pharmacological action widely, and wherein Salvianic acidA has its special efficacy again.
The Salvianic acidA molecular weight is 198.17, and its structure is:
Salvianic acidA is a phenolic acid, sees that light is heated easy the decomposition, and soluble in water, solubleness is bigger in weak caustic solution, and character is more stable.Content of Danshensu is lower in the red sage root, and general 0.3%～0.5%.And content of Danshensu is between 0.2～0.5% in the fresh red sage root, and Salvianic acidA loses in a large number in the airing process.
The method that extraction purifying Salvianic acidA generally uses has: water extraction method, ethanol refluxing process, water extraction and alcohol precipitation method, liquid-liquid extraction method, silicagel column look general partition method etc.These methods exist shortcomings such as energy consumption is big, 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.Extract the purifying Salvianic acidA as document spent ion exchange resin and machine reagent extraction (Chinese patent CN1161317) method of reporting for work, though purity is high, still, energy consumption is big, yield is low, also introduce organic reagent, be difficult in and control solvent residual amount in the pharmacy, also had extraction and chromatograph joint used extraction purifying Salvianic acidA (as Chinese patent CN303053), organic reagent and silicagel column use, be difficult to amplify aborning, output is very low, the cost height.
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 Salvianic acidA purity is greater than 75%, and yield is more than 80%, and output is big, and the cycle is short, is easy to realize industrialized Salvianic acidA extraction and purification process.
The object of the present invention is achieved like this:
1) squeezing is extracted: the fresh red sage root is pulverized, added saturated limewater and soak, cold pressing under pressurization 80～100MPa, residue is repeated to soak squeezing once, merge the pressed liquor that obtains.
Salvianic acidA is heated and sees photo-labile, and loss can be up to 60% in the dryness in the sun process, even decomposes loss fully, and extracting the used red sage root of Salvianic acidA both at home and abroad at present all is the dried red sage root, oven dry cost height.And this technology is used the fresh red sage root, and Salvianic acidA can not lose because the airing operation is arranged.
More be soluble in the character of buck according to Salvianic acidA, under the normal temperature pulverizing medicinal materials added a small amount of saturated limewater and soak high-pressure compressing.Under normal temperature condition, destroy red sage root weave construction by powerful mechanical effect, can more up hill and dale the Salvianic acidA in the red sage root be extracted.
The above-mentioned method of extracting the purifying Salvianic acidA from the fresh red sage root is characterized in that fresh salvia miltiorrhiza raw material grinding particle size is 30～80 orders, and adding the saturated limewater amount is 1～2: 1 than red sage root weight, soak time 1～2 hour.
2) ion exchange resin absorption: pressed liquor is regulated pH to 6～7, filter, filtrate adds the strongly basic anion exchange resin post and carries out saturated absorption, use the deionized water removal of impurities during wash-out, use the saturated limewater eluant solution again, collect the Salvianic acidA eluting liquid, the Salvianic acidA eluting liquid adds the strong acidic ion resin post again, collects the post effluent liquid.
Stepwise elution is adopted in the saturated absorption of strongly basic anion exchange resin post back, compares the plurality of impurities of removing up hill and dale wherein with deionized water earlier, and then with saturated limewater eluant solution Salvianic acidA, obtains impure less Salvianic acidA elutriant.
The Salvianic acidA eluting liquid adsorbs impurity and metal ion after the strong acidic ion resin post, and this process Salvianic acidA is not adsorbed, and collects the post effluent liquid.
The above-mentioned method of extracting the purifying Salvianic acidA from the fresh red sage root is characterized in that wherein a kind of of the used sour optional hydrochloric acid of acid adjustment, sulfuric acid, phosphoric acid.
The above-mentioned method of extracting the purifying Salvianic acidA from the fresh red sage root is characterized in that the combination of strongly basic anion exchange resin and storng-acid cation exchange resin.
The above-mentioned method of from the fresh red sage root, extracting the purifying Salvianic acidA, it is characterized in that strongly basic anion exchange resin can select 717 for use, a kind of in 201 * semi-finals basic anion exchange resin, a kind of in optional 507,732 strong acidic ion resins of strong acidic ion resin.
The above-mentioned method of from the fresh red sage root, extracting the purifying Salvianic acidA, it is characterized in that segmentation absorption and stepwise elution: at first squeeze liquid by the saturated absorption of strongly basic anionic resin post, with the removal of impurities of 6～8 times of amount column volume deionized water wash-out strongly basic anion exchange resin posts, with 4～5 times of saturated lime solution wash-out Salvianic acidAs of amount, collect the Salvianic acidA eluting liquid after strong acid cation exchange resin column.
3) membrane sepn: above-mentioned post effluent liquid 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 Salvianic acidA molecular weight, earlier remove macromole impurity and colored component with the ultrafiltration membrane system of molecular weight cut-off 1000～3000, then follow-up the needs with gac the feed liquid processing of decolouring again; Hold back Salvianic acidA at normal temperatures with the nanofiltration membrane system again, play spissated purpose.
The above-mentioned method of extracting the purifying Salvianic acidA from the fresh red sage root is characterized in that ultrafiltration, nanofiltration that described Salvianic acidA separates in concentrating all carry out at normal temperatures.
The above-mentioned method of extracting the purifying Salvianic acidA from the fresh red sage root is characterized in that it is that 1000～3000 ultra-filtration membrane and molecular weight cut-off are 100 nanofiltration membrane that described ultra-filtration membrane uses molecular weight cut-off.
4) 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 red sage root Salvianic acidA in drying process.
2) squeezing is extracted, exchange resin adsorbs and membrane sepn all makes technological process maintain normal temperature, has therefore both ensured the stability of Salvianic acidA, has also saved a large amount of energy consumptions.
3) spraying drying speed is fast, the purity height, and especially effective to the thermo-sensitivity goods, solubility property is good, therefore can make granule, oral liquid etc. easily.
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 Danshensu 0.4%), pulverize 30 orders, add the immersion of 50L saturated limewater and in chamber filter press, be forced into the 80MPa squeezing in 1 hour, medicinal material is repeated to soak squeezing once, merge twice squeezing liquid.Regulate pH to 6 with hydrochloric acid, the 717 strongly basic anion exchange resin posts that add column volume 5L, with 30L deionized water flush away impurity, use 20L 1% saturated limewater eluant solution Salvianic acidA again, collect 732 strong acidic ion resins that eluting liquid adds volume 2.5L, collect lower column liquid, final lower column liquid is removed macromole impurity by the ultra-filtration membrane of molecular weight cut-off 1000 earlier, nanofiltration membrane with molecular weight cut-off 100 concentrates again, concentrated solution carries out spraying drying, finally obtains 209g content and be 80.1% Salvianic acidA finished product.
Embodiment 2:
Get the fresh red sage root of 60kg (content of Danshensu 0.35%), pulverize 80 orders, add the immersion of 90L saturated limewater and in chamber filter press, be forced into the 90MPa squeezing in 1.5 hours, residue is repeated to soak squeezing once, merge twice squeezing liquid.Regulate pH to 7 with sulfuric acid, the 507 strongly basic anion exchange resin posts that add column volume 5L with 40L deionized water flush away impurity, are used the saturated lime solution wash-out of 25L Salvianic acidA again, collect 201 * semi-finals acidic cationic resin that eluting liquid adds volume 2.5L, collect lower column liquid.Lower column liquid is earlier removed macromole impurity by the hollow fiber ultrafiltration membrane system of molecular weight cut-off 3000, and the nanofiltration membrane system with molecular weight cut-off 100 concentrates again, and concentrated solution carries out spraying drying, finally obtains 221g content and be 78% Salvianic acidA finished product.
Embodiment 3:
Get the fresh red sage root of 70kg (content of Danshensu 0.3%), pulverize 60 orders, add the immersion of 140L saturated limewater and in chamber filter press, be forced into the 100MPa squeezing in 1 hour, residue is repeated to soak squeezing once, merge twice squeezing liquid.Regulate pH to 7 with phosphoric acid, 201 * semi-finals basic anion exchange resin the post that adds column volume 5L with 35L deionized water flush away impurity, is used the saturated lime solution wash-out of 23L Salvianic acidA again, collect 732 strong acidic ion resins that eluting liquid adds volume 2.5L, collect lower column liquid.Lower column liquid is earlier removed macromole impurity by the ultrafiltration membrane system of molecular weight cut-off 2000, and the nanofiltration membrane system with molecular weight cut-off 100 concentrates again, and concentrated solution carries out spraying drying, finally obtains 230g content and be 76% Salvianic acidA finished product.
Claims (8)
1. method of extracting the purifying Salvianic acidA 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 saturated limewater and soak, cold pressing under pressurization 80～100MPa, residue is repeated to soak squeezing once, merge the pressed liquor that obtains for twice;
2) ion exchange resin absorption: pressed liquor acid adjustment pH to 6～7, filter, filtrate adds the strongly basic anion exchange resin post and carries out saturated absorption, use the deionized water removal of impurities during wash-out, use the saturated limewater eluant solution again, collect the Salvianic acidA eluting liquid, the Salvianic acidA eluting liquid adds the strong acidic ion resin post again, collects the post effluent liquid;
3) membrane sepn: above-mentioned post effluent liquid is held back macromolecular substance by ultrafiltration membrane system earlier, collects to see through liquid, concentrate with the nanofiltration membrane concentration systems, concentrated solution;
4) spraying drying: concentrated solution enters the spray-drying tower drying, promptly.
2. according to the described method of extracting the purifying Salvianic acidA from the fresh red sage root of claim 1, it is characterized in that fresh salvia miltiorrhiza raw material grinding particle size is 30～80 orders, adding the saturated limewater amount is 1～2: 1 than red sage root weight, soak time 1～2 hour.
3. according to the described method of from the fresh red sage root, extracting the purifying Salvianic acidA of claim 1, it is characterized in that wherein a kind of of the used sour optional hydrochloric acid of described acid adjustment, sulfuric acid, phosphoric acid.
4. according to the described method of from the fresh red sage root, extracting the purifying Salvianic acidA of claim 1, it is characterized in that described strongly basic anion exchange resin can select 717 for use, a kind of in 201 * semi-finals basic anion exchange resin, a kind of in optional 507,732 strong acidic ion resins of described strong acidic ion resin.
5. according to the described method of from the fresh red sage root, extracting the purifying Salvianic acidA of claim 1, it is characterized in that described ion exchange resin absorption is strongly basic anion exchange resin and storng-acid cation exchange resin combination coupling.
6. according to the described method of from the fresh red sage root, extracting the purifying Salvianic acidA of claim 1, it is characterized in that described ion exchange resin absorption is segmentation absorption and stepwise elution: at first squeeze liquid by the saturated absorption of strongly basic anionic resin post, with the removal of impurities of 6～8 times of amount column volume deionized water wash-out strongly basic anion exchange resin posts, with 4～5 times of saturated lime solution wash-out Salvianic acidAs of amount, collect the Salvianic acidA eluting liquid after strong acid cation exchange resin column.
7. according to the described method of from the fresh red sage root, extracting the purifying Salvianic acidA of claim 1, it is characterized in that described ultrafiltration, nanofiltration all carry out at normal temperatures.
8. according to the described method of extracting the purifying Salvianic acidA from the fresh red sage root of claim 1, it is characterized in that described ultra-filtration membrane is that molecular weight cut-off is 1000～3000 ultra-filtration membrane nanofiltration membrane, described nanofiltration membrane molecular weight cut-off is 100 nanofiltration membrane.
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| CN200910233835A CN101759555A (en) | 2009-10-22 | 2009-10-22 | Method for extracting and purifying salvianic acid A from fresh salvia miltiorrhiza |
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| CN200910233835A CN101759555A (en) | 2009-10-22 | 2009-10-22 | Method for extracting and purifying salvianic acid A from fresh salvia miltiorrhiza |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102429936A (en) * | 2010-09-29 | 2012-05-02 | 苏州瑞蓝博中药技术开发有限公司 | Method for purifying phenolic acid from ramie |
| CN106995369A (en) * | 2017-03-31 | 2017-08-01 | 吉林四长制药有限公司 | A kind of preparation method using danshensu as the red sage root extract of object |
| CN109966337A (en) * | 2019-03-28 | 2019-07-05 | 湖南华诚生物资源股份有限公司 | A method of extracting sennoside from folium sennae |
-
2009
- 2009-10-22 CN CN200910233835A patent/CN101759555A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102429936A (en) * | 2010-09-29 | 2012-05-02 | 苏州瑞蓝博中药技术开发有限公司 | Method for purifying phenolic acid from ramie |
| CN106995369A (en) * | 2017-03-31 | 2017-08-01 | 吉林四长制药有限公司 | A kind of preparation method using danshensu as the red sage root extract of object |
| CN106995369B (en) * | 2017-03-31 | 2019-06-14 | 吉林四长制药有限公司 | It is a kind of using danshensu as the preparation method of the red sage root extract of object |
| CN109966337A (en) * | 2019-03-28 | 2019-07-05 | 湖南华诚生物资源股份有限公司 | A method of extracting sennoside from folium sennae |
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Application publication date: 20100630 |