CN102304111B - Method for extracting and purifying salvianolic acid B with ion exchange fiber - Google Patents
Method for extracting and purifying salvianolic acid B with ion exchange fiber Download PDFInfo
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- CN102304111B CN102304111B CN 201110194765 CN201110194765A CN102304111B CN 102304111 B CN102304111 B CN 102304111B CN 201110194765 CN201110194765 CN 201110194765 CN 201110194765 A CN201110194765 A CN 201110194765A CN 102304111 B CN102304111 B CN 102304111B
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- exchange fiber
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Abstract
The invention discloses a method for extracting and purifying salvianolic acid B with ion exchange fiber. The method comprises the following specific operation steps of washing, drying and smashing a salvia miltiorrhiza medicinal material, and then decocting and leaching; adsorbing with an ion exchange fiber column under the conditions that the concentration of a salvianolic acid B raw liquid is 0.03-6.0 g.L<-1>, the temperature is 10-80 DEG C, the flow speed is 0.4-7.0 BV.h<-1> (BV: column volume) and the pH value is 7.0-13.0; eluting with an eluting agent at the elution temperature of 10-90 DEG C and the flow speed of 0.1-8.0 BV.h<-1>, wherein the eluting agent is prepared from water, alcohol or a mixture of water and alcohol and a 0.4-7.0 mol.L<-1> HCl pH regulator in a volume ratio of (1-10): 1; and collecting eluate, and recovering organic matters so as to obtain salvianolic acid B extractive powder. The method has the advantages of simple process, easily available production equipment, low operation cost, high economic efficiency and obvious energy-saving effect and is suitable for scale production, and the purity of the product is obviously improved.
Description
Technical field
The present invention relates to the method with ion-exchange fiber extraction, separation and purifying natural plants ' medicinal component, specifically, is the method for extracting the purifying salvianolic acid B with ion-exchange fiber.
Background technology
(Ion Exchange Fiber is a kind of fibrous ion exchange sorbing material IEF) to ion-exchange fiber, and it is made up of many fibre single threads, and fiber number is little, and its scope is between 20～300 μ m.Itself is reached by non diffusible ion and the movable ion of non diffusible ion opposite in sign is constituted.When the solution with the compound that can dissociate contacts, the movable ion of ion-exchange fiber namely with solution in the ion of same-sign exchange, so claim ion-exchange fiber.
Ion-exchange fiber is compared with the particulate state ion-exchanger, and it is big to have a specific surface, and diameter is little, and absorption, desorption rate are fast, and exchange capacity is big, regeneration easily, characteristics such as type of service is various.
Ion-exchange fiber mainly contains four classes: strong-acid cation exchange fibre, Subacidity cation exchange fiber, strongly basic anion ion exchange fibre, weakly basic anion exchange fibre.
As if the skeleton that represents the strong base anion fiber with R, when then fiber fully contacted with saponin(e solution, permutoid reaction took place, reaction process constantly consumes the cation exchange groups of strong base anion exchange fiber, causes the exchange capacity of fiber to weaken, even loses exchange capacity.In order to recover the exchange capacity of fiber, can make fiber recover exchange capacity with the layer of fibers of certain density NaOH solution by having lost efficacy.Therefore ion-exchange capacity is reversible.This reversibility can be used fiber repeatedly.
The red sage root has another name called red ginseng, Radix Salviae Miltiorrhizae, red etc.This product is the dry root and rhizome of dicotyledons Labiatae (Labiatae) the salvia red sage root (Salvia miltiorrhiza Bge.).Main product in Anhui, ground such as Henan, Shaanxi.Have promoting blood flow to regulate menstruation, stasis-dispelling and pain-killing, the cool blood carbuncle that disappears, the relieving restlessness that clears away heart-fire,
Effects such as nourishing blood to tranquillize the mind.Also have the energy coronary artery dilator, increase coronary flow, improve myocardial ischemia, infraction and heart function, regulate the rhythm of the heart, and can expand peripheral blood vessel, microcirculation improvement; Can improve body's hypoxia tolerance; Anticoagulation is arranged, promote fibrinolytic, suppress platelet aggregation, suppress thrombotic effect; The energy blood fat reducing suppresses coronary atherosclerosis and forms; Can suppress or alleviate hepatocellular degeneration, necrosis and inflammatory reaction, promote liver cell regeneration, and anti-fibrosis effect is arranged; Can shorten the decubation of red corpuscle and hemochrome, Reticulocyte is increased, can promote the reparation of tissue, accelerate the healing of fracture; Nervus centralis there is restraining effect; Antitumor action is arranged; Energy enhancing body immunologic function; The energy lowering blood glucose; Various bacteria such as tubercule bacillus there is restraining effect etc.
The red sage root mostly is the root of band rhizome, and the rhizome tubbiness has stem foot remnants, is descending to give birth to most elongated roots.Root is cylindrical, and crooked slightly, it is brick-red that the surface is, coarse, the most longitudinal furrows of tool or wrinkle have mark of fibrous root, the normal flakey of outside cork is peeled off, and cortex ftractures sometimes, long 8～22cm, diameter 5～12mm, the matter heavily fortified point is crisp, frangibility, the section injustice, loosening has the crack, the thirsty look or brick-red of skin zone palm fibre, and phloem is narrow.Form layers is obvious, light brown, xylem vessel's bundle lark or yellow-white, radial arrangement.Gas is little, mildly bitter flavor, puckery, and, look purplish red person sturdy with bar is good.
Red sage root mainly contains fat-soluble diterpenes composition and water miscible phenolic acid composition, also contains flavonoid, triterpenes, other compositions such as sterol.Water miscible phenol acid compound has: red sage root acid (sal-vianic acid) A, B, C.Red sage root acid B is exactly salvianolic acid B, is called for short salvianolic acid B.
Salvianolic acid B another name red sage root acid B, salvianolic acid second.Molecular formula C
36H
30O
16, molecular weight 718.62.
This product is pale brown look dried powder, and pure product are off-white powder; Mildly bitter flavor, puckery, tool draws moist.Water soluble, ethanol, methyl alcohol.Red sage root acid B is formed by the Salvianic acidA of 3 molecules and the coffic acid condensation of 1 molecule, has two carboxyls, and there is (K in the form of salt that can be different
+, Ca
2+, Na
+, NH
4+Etc. complex form).Be one of more salvianolic acid of research at present, organs such as the heart, brain, liver, kidney are all had the valuable pharmacological effect.A plurality of phenol cyano group in this compound structure, have than strong anti-oxidation, at present to the comparatively dark people of its research, think that salvianolic acid B is the strongest active composition in the salvia-soluble material, the red sage root can make aorta atheromatous plaque formation area obviously reduce serum total cholesterol, triglyceride level, all decreases to some degree.Modern pharmacology studies show that the pharmacologically active of salvianolic acid B mainly is to improve aspects such as blood system and systema cariovasculare functional, strengthening by means of tonics, adjusting immunity, therefore extracts salvianolic acid B exploitation treatment cardio-cerebrovascular diseases new drug and protective foods are had important academic significance and practical value.
At present, the common method that salvianolic acid B extracts is cold-maceration, also has some more traditional extracting method such as decoction alcohol precipitation method, percolations etc.
Along with the development of modern separation technology, the technology of some other fields also is applied in the extraction of salvianolic acid B, as ultrasonic wave/microwave extraction, macroporous adsorption resin technology, high-speed countercurrent chromatography and membrane separation technique etc.In the extraction and purification process of salvianolic acid B, most critical be this procedure of separation and purification.
Aforesaid method efficient is all lower, and the salvianolic acid B purity of separating is not high, poor repeatability, and production link is many, and high material consumption has caused the serious environmental pollution, the production cost height, the cycle is long.Make the bad monitoring of index in the sepn process.The scale operation of unfavorable salvianolic acid B.
Summary of the invention
Technical problem to be solved by this invention is at existing technical deficiency, and a kind of method of separation and purification salvianolic acid B is provided, and makes its product purity height, foreign matter content is few, operating procedure is simple and direct, production cost is low, is suitable for standard and large-scale production salvianolic acid B.
The present invention for the technical scheme that solves the problems of the technologies described above employing is:
(1) the dry root and rhizome of the red sage root is clean, dry, pulverizing back decocts lixiviate;
(2) vat liquor adsorbs with the ion-exchange fiber post;
(3) will be adsorbed on salvianolic acid B desorb (wash-out) on the ion-exchange fiber post;
(4) the elutriant drying obtains containing salvianolic acid B purified extract powder.
Wherein, the salvianolic acid B of step (1) leaching powder can add water, alcohol or its mixture by the starting material of the red sage root and decoct acquisition, and preferably water, methyl alcohol or its mixture decoct, and extraction temperature is 20～95 ℃; Preferably near the temperature of solution boiling point; The pH value is 6.0～12.0; Preferred pH value is 7.0～11.0; Extraction time is 1～5 hour; Preferred 2.0～4.0h; Lixiviate number of times 2～5 times; Preferred 3 times.Wherein, the ion-exchange fiber that uses of step (2) is strong basicity ion-exchange fiber or Weak-alkaline ion exchange fibre.Preferred strong basicity ion-exchange fiber, the type fiber is used for the separation and purification of salvianolic acid B, is to adopt first.The weight ratio of handled medicinal material and fiber is 2～30: 1, preferred 5～25: 1; Adorn post, the water of preferred 2～3 times of column volumes with the water wet method of 1～5 times of column volume earlier; Again with salvianolic acid B original liquid concentration 0.03～6.0gL
-1, preferred 0.06～3.0gL
-1Temperature is 10～80 ℃, preferred 40～70 ℃; Flow velocity 0.4～7.0BVh
-1, preferred 0.8～4.0BVh
-1The pH value is 7.0～13.0, and preferred pH value is 8.0～12.0 condition absorption.
Wherein, step (3) is that elder generation is with the water elution of 1～4 times of column volume, the water elution of preferred 2 times of column volumes; Again with the eluent wash-out of 2～10 times of column volumes, the eluent wash-out of 10～75% methanol aqueous solutions of preferred 4～8 times of column volumes and acid preparation; Eluting temperature is 10～90 ℃, and preferred temperature is 50～80 ℃; Flow velocity 0.1～8.0BVh
-1, preferable flow rate 0.3～6.0BVh
-1Eluent is that water, methyl alcohol or its mixture and concentration are 0.4～7.0molL
-1The agent of HCl pH regulator be 1～10: 1 formulated with volume ratio, preferred volume ratio 2～6.Collect elutriant.
Wherein, step (4) is that organism gets concentrated solution in the recovery elutriant, gets powder through vacuum decompression drying or lyophilize again.
The present invention is suitable for arbitrary extraction purifying that contains the raw-material salvianolic acid B of Potenlini.
Beneficial effect of the present invention is embodied in:
1. salvianolic acid B production method of the present invention has adopted the alkali ion exchange fiber as parting material, is to use first on salvianolic acid B is produced.
2. it is simple to produce equipment used, and the medicinal material proportion of fibers is lower, and extracting solution is directly gone up the fiber chromatography column without concentrating and any purification process, and technology is simple, and production process is lacked, and running cost is low, and efficient height, energy-saving effect are remarkable.
3. the inventive method has improved salvianolic acid B purity and yield, and quality product can be monitored, and solution can be recycled after distillation is reclaimed, and non-secondary pollution is applicable to large-scale production.
4. used fiber reusable edible.
Specific embodiments
Below further set forth the present invention with embodiment, but therefore do not limit the present invention in the specific embodiment scope.
Embodiment 1
Taking by weighing the 20g powder after will red sage root clean dry pulverizing, is 70% methanol aqueous solution 180mL with volume ratio, and transferring its pH value is 9, located to decoct 3.0 hours at 60 ℃, the decocting with 160mL boiled 3.0 hours again, merged decoction liquor and cooling, transferring the pH value of solution value is 11.0, with flow velocity 1.5BVh
-1, be that 1.0g, bed volume are that the strong basicity ion-exchange fiber post of 10mL adsorbs through weight.Again with flow velocity 3.0BVh
-1, the water elution of 3 times of column volumes, the back is with 80% methyl alcohol and hydrochloric acid (80% methyl alcohol: 3molL of 5 times of column volumes
-1The volume ratio of hydrochloric acid 4: 1) mixed solution wash-out reclaims methyl alcohol and gets the salvianolic acid B extract, and wherein content of danshinolic acid B is 61.28.22%, and yield is 3.85%.
Embodiment 2
Take by weighing the 200g powder after will red sage root clean dry pulverizing, be made into the aqueous solution 1800mL that volume ratio is 70% ethanol with distilled water and the ethanol of pH=7,60 ℃ of extractions 3.0 hours down, again with the mixed solution decoction of 1500mL 3.0 hours.The salvianolic acid B crude product yield that obtains is 10.28%, and purity is 23.55%.Be 11.0 in upper prop soup pH value, flow velocity 2.0BVh
-1, liquor strength is 0.2mgmL
-1Condition under, the strong basicity ion-exchange fiber post of crossing weight and be 12.0g, bed volume and be 120mL adsorbs.Be 750% methyl alcohol and 3molL with strippant
-1The mixed solution of hydrochloric acid (volume ratio 4: 1) 6BV, elution flow rate 3.0BVh
-1Carry out wash-out.Reclaim the salvianolic acid B extract that methyl alcohol gets purifying, wherein content of danshinolic acid B is 60.02%, and yield is 3.68%.
Claims (1)
1. the production method of a salvianolic acid B extract, comprise step: take by weighing the 20g powder after red sage root clean dry is pulverized, be 70% methanol aqueous solution 180mL with volume ratio, transferring its pH value is 9, located to decoct 3.0 hours at 60 ℃, the decocting with 160mL boiled 3.0 hours again, merged decoction liquor and cooling, transferring the pH value of solution value is 11.0, with flow velocity 1.5BVh
-1, be that 1.0g, bed volume are that the strong basicity ion-exchange fiber post of 10mL adsorbs through weight, again with flow velocity 3.0BVh
-1, the water elution of 3 times of column volumes, the back is with 80% methyl alcohol of 5 times of column volumes: 3molL
-14: 1 mixed solution wash-out of the volume ratio of hydrochloric acid reclaims methyl alcohol and gets the salvianolic acid B extract.
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| CN 201110194765 CN102304111B (en) | 2011-07-12 | 2011-07-12 | Method for extracting and purifying salvianolic acid B with ion exchange fiber |
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| CN 201110194765 CN102304111B (en) | 2011-07-12 | 2011-07-12 | Method for extracting and purifying salvianolic acid B with ion exchange fiber |
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| CN102304111B true CN102304111B (en) | 2013-08-14 |
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| CN1164582C (en) * | 2002-12-31 | 2004-09-01 | 南京虹桥医药技术研究所 | Process for preparing danshen salviandic acid |
| CN101613387A (en) * | 2008-06-26 | 2009-12-30 | 北京服装学院 | The method of extracting purified puerarin by utilizing ion-exchange fiber |
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