CN102205039B - Method for extracting purified saponin with ion exchange fiber - Google Patents
Method for extracting purified saponin with ion exchange fiber Download PDFInfo
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Abstract
The invention discloses a method for extracting purified saponin with an ion exchange fiber. The method comprises the following specific steps of: cleaning saponin-containing raw materials such as leaves, stems, roots, fruits and the like, drying, grinding, decocting and soaking; adsorbing with an ion exchange fiber column under the conditions that the concentration of a saponin stock solution is0.05-5.0 g.L<-1>, the temperature is 15-80 DEG C, the flow rate is 0.1-6.0 BV.h<-1> (BV refers to column volume) and the pH value is 5.0-11.0; eluting with an eluting agent at the eluting temperature10-90 DEG C and the flow rate 0.1-12.0 BV.h<-1>, wherein the eluting agent is prepared from water, ethanol or a mixture of the water and the alcohol and an HCl pH regulating agent with the concentration 0.1-6.0 mol.L<-1> in the ratio (1-9):1; and collecting an eluent and recycling organic matters to obtain saponin extract powder. The method has the advantages of simple process, readily-available operating equipment, low running cost, high running efficiency, remarkable energy saving effect and remarkable increase in product purity, and is suitable for mass production.
Description
Technical field
The present invention relates to the method with ion-exchange fibre extraction, separation and purifying natural plants ' medicinal component, specifically, is the method with extracting purified saponin with ion exchange fiber.
Background technology
Ion-exchange fibre (Ion Exchange Fiber, IEF) is a kind of fibrous ion exchange adsorption material, and it is comprised of many fibre single threads, and diameter is little, and its scope is between 20～300 μ m.Itself is reached by fixed ion and the movable ion of fixed ion opposite in sign is consisted of.When the solution with the chemical compound that can dissociate contacts, the movable ion of ion-exchange fibre namely with solution in the ion of same-sign exchange, therefore claim ion-exchange fibre.Compare with the graininess ion-exchanger, ion-exchange fibre has the characteristics such as specific surface is large, and diameter is little, and Adsorption and desorption speed is fast, and exchange capacity is large, easily regenerates, and type of service is various.
Ion-exchange fibre mainly contains four classes: strong-acid cation exchange fibre, Subacidity cation exchange fiber, strongly basic anion ion exchange fibre, weakly basic anion exchange fibre.
If represent the skeleton of strong alkali anion fiber with R, when then fiber fully contacted with saponin solution, exchange reaction occured, course of reaction constantly consumes the cation exchange groups of strong alkali 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 with the fibrous layer of certain density NaOH solution by having lost efficacy, make fiber recover exchange capacity.Therefore ion-exchange capacity is reversible.This reversibility makes the fiber can Reusability.
" saponin " word is by English name Saponin free translation, and English name then comes from Latin Sapo, means soap.Saponin is the chemical compound of complicated structure in the glycoside.They extensively are present in the plant, and are of a great variety, form complicated.Very active to the research of saponin in the world, entered a new climax eighties.
Saponin is made of sapogenin and sugar.The sugar that forms saponin common are glucose, galactose, rhamnose, arabinose, xylose, glucuronic acid and galacturonic acid etc.
Aglycon is that the saponin of spirostane class (C-27 steroidal compounds) is called steroidal saponin, mainly is present in Dioscoreaceae, Liliaceae and Scrophulariaceae etc., is neutral; Aglycon is that the saponin of triterpenes is called triterpene saponin (C-30 carbon atom forms), mainly is present in Araliaceae, pulse family, Polygalaceae and Cucurbitaceae etc., and its kind analogy steroidal saponin is many, distributes also more extensive.Most of triterpene saponin is acid, and it is neutral that minority is.
Saponin mostly is white or milky amorphous powder, and minority is crystal, and bitter in the mouth and pungent has zest to mucosa.The general water soluble of saponin, methanol and Diluted Alcohol are soluble in hot water, hot methanol and hot ethanol.
Saponin connects the difference of sugar chain number according to aglycon, can be divided into monodesmosidic saponin, bisdesmoside and three sugar chain saponin.On the sugar chain of some saponin, also be connected with other groups by ester bond.
Most saponin can reduce the surface tension of liquid (water), have the character of spuming and emulsifying agent effect, can be used as cleaning agent, also have the effect of haemolysis and malicious fish.The many Chinese medicine of saponin component such as effects that Radix Polygalae, Radix Platycodonis etc. have expelling phlegm for arresting cough of containing are arranged; Some saponin also has the antibiotic valuable biological activity such as active or analgesic, calm, anticancer.Indivedual saponin have special physiologically active, can promote the biosynthesis of DNA and protein such as the ginsenoside, improve the immunocompetence of body.Glycyrrhizic acid has the effect that promotes adrenocortical hormone, and the effect of cough-relieving and treatment gastric ulcer is arranged.
At present, the extracting method of saponin has a variety of.The method that Chinese Pharmacopoeia is used is cold-maceration, but comparatively time-consuming; Also having some more traditional extracting method such as decoction alcohol precipitation method, percolation all is the main method of extracting at present saponin.Along with the development of modern science and technology, the technology of some other fields also is applied in the extraction of saponin, is optimized extraction process etc. such as ultrasound wave/microwave extraction, macroporous adsorption resin technology, tank group countercurrent extraction technology and utilization neural network model.In the extraction and purification process of polysaccharide, most critical be this operation of separation and purification.
But these method efficient are all lower, and the saponin purity of separating is not high, poor repeatability, and production link is many, and parting material consumption is large, has caused serious environmental pollution and material consumption, and production cost is high, and the cycle is long.So that the bad monitoring of the index in the separation process.The large-scale production of unfavorable saponins compound.
Summary of the invention
Technical problem to be solved by this invention is for existing technical deficiency, a kind of method of separation and purification saponins compound is provided, make that its product purity is high, impurity content is few, operating procedure is simple and direct, production cost is low, be suitable for standardization and produce saponins compound.
The present invention for the technical scheme that solves the problems of the technologies described above employing is:
(1) will contain the raw material of saponin such as Radix Ginseng, Radix Polygalae, Radix Platycodonis, Radix Glycyrrhizae, the Rhizoma Anemarrhenae and Radix Bupleuri etc. clean, dry, decoct lixiviate after pulverizing;
(2) lixiviating solution adsorbs with the ion-exchange fibre post;
(3) will be adsorbed on saponin desorbing (eluting) on the ion-exchange fibre post;
(4) the eluent drying obtains containing saponin purified extract powder.
Wherein, the saponin of step (1) leaching powder can add by the raw material that contains saponin water, alcohol, ether, acetone, chloroform or its mixture and decoct acquisition, and preferred water, alcohol or its mixture decoct, and extraction temperature is 35～90 ℃; Preferably near the temperature of solution boiling point; PH value is 4.0～9.0; Preferred pH value is 6.0～8.0; Extraction time is 1～6 hour; Preferred 2.5h; Extracting times 2～6 times; Preferred 3 times.
Wherein, the ion-exchange fibre that uses of step (2) is strong basicity ion-exchange fibre or Weak-alkaline ion exchange fibre.Preferred strong basicity ion-exchange fibre, the type fiber is used for the separation and purification of saponin, is to adopt first.The weight ratio of handled medical material and fiber is 2～30: 1, preferred 5～25: 1; Water wet method with 1～4 times of column volume fills post, the water of preferred 2～3 times of column volumes first; Again with saponin original liquid concentration 0.05～5.0gL
-1, preferred 0.08～4.0gL
-1Temperature is 15～85 ℃, preferred 50～80 ℃; Flow velocity 0.1～6.0BVh
-1, preferred 0.8～5.0BVh
-1PH value is 5.0～11.0, and preferred pH value is 6.5～10.5 condition absorption.
Wherein, step (3) is that elder generation is with the water elution of 1～3 times of column volume, the water elution of preferred 2 times of column volumes; Again with the eluant eluting of 3～15 times of column volumes, the eluant eluting of 15～75% ethanol waters of preferred 5～8 times of column volumes and acid preparation; Eluting temperature is 10～90 ℃, and preferred temperature is 50～80 ℃; Flow velocity 0.1～12.0BVh
-1, preferable flow rate 0.4～8.0BVh
-1Eluant is that water, ethanol or its mixture and concentration are 0.1～6.0molL
-1The HCl pH adjusting agent take volume ratio as 1～9: 1 is formulated, preferred volume ratio 3～5.Collect eluent.
Wherein, step (4) is that Organic substance gets concentrated solution in the recovery eluent, gets powder through vacuum decompression drying or lyophilization again.
The present invention is suitable for arbitrary extraction purification that contains the raw-material saponin of saponin.
Beneficial effect of the present invention is embodied in:
1. saponin production method of the present invention has adopted the alkali ion exchange fiber as parting material, is to use first on saponin is produced.
2. used production equipment is easy to get, and the medical material proportion of fibers is low, and extracting solution is directly gone up the fiber chromatographic column without concentrated and any purification process, and technique is simple, and production process is short, and operating cost is low, and efficient is high, energy-saving effect is remarkable.
3. the inventive method has improved product purity and yield, and target level of product quality is controlled, and solution can be recycled behind Distillation recovery, and non-secondary pollution is applicable to large-scale production.
4. used fiber is renewable recycling.
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
With taking by weighing the 20g powder after the pulverizing of Radix Notoginseng clean dry, be 70% ethanol water 180mL with volume ratio, transferring its pH value is 7, located to decoct 2.5 hours at 65 ℃, the decocting with 140mL boiled 2.5 hours again, merged decoction liquor and cooling, transferring pH is 10.0, with flow velocity 1.5BVh
-1, be that 1.0g, bed volume are that the strong basicity ion-exchange fibre post of 10mL adsorbs through weight.Again with flow velocity 5.0BVh
-1, the water elution of 3 times of column volumes is afterwards with 60% ethanol and hydrochloric acid (60% ethanol: 3molL of 5 times of column volumes
-1The volume ratio of hydrochloric acid 4: 1) mixed liquor eluting, Recycled ethanol gets saponin extract, and wherein saponin content is 62.01%, and yield is 7.47%.
Embodiment 2
Take by weighing the 200g powder after will the Radix Notoginseng clean dry pulverizing, be made into the aqueous solution 2000mL that volume ratio is 70% ethanol with distilled water and the ethanol of pH=7,70 ℃ of lower extractions 3 hours, again with the mixed liquor decoction of 1600mL 2 hours.The saponin crude product yield that obtains is 25.60%, and purity is 8.02%.Be 9.5 at upper prop medicinal liquid pH value, flow velocity 2.0BVh
-1, liquor strength is 0.4mgmL
-1Condition under, the strong basicity ion-exchange fibre post of crossing weight and be 12.0g, bed volume and be 120mL adsorbs.Be 50% ethanol and 3molL with strippant
-1The mixed liquor of second hydrochloric acid acid (volume ratio 4: 1) 7BV, elution flow rate 4.0BVh
-1Carry out eluting.Recycled ethanol gets the saponin extract of purification, and wherein saponin content is 60.21%, and yield is 7.12%.
Embodiment 3
Taking by weighing Radix Glycyrrhizae powder 20g, is 65% ethanol water 180mL with volume ratio, and transferring its pH value is 6.8, locates to decoct 3.0 hours at 70 ℃, and the decocting with 150mL boiled 2.5 hours again, merges decoction liquor and cooling, and transferring pH is 10.5, with flow velocity 1.5BVh
-1, be that 1.0g, bed volume are that the strong basicity ion-exchange fibre post of 10mL adsorbs through weight.Again with flow velocity 4.0BVh
-1, with the water elution of 3 times of column volumes, again with 65% ethanol (65% ethanol: 3molL of 5 times of column volumes
-1The volume ratio of hydrochloric acid 4: 1) eluting, Recycled ethanol gets saponin extract, and wherein saponin content is that 52.21% yield is 6.37%.
Embodiment 4
Take by weighing the 200g powder after will the Radix Glycyrrhizae clean dry pulverizing, be made into the aqueous solution 2000mL that volume ratio is 75% ethanol with distilled water and the ethanol of pH=7,70 ℃ of lower extractions 3 hours, again with the mixed liquor decoction of 1800mL 2.5 hours.Merge decoction liquor, concentrated.Be 9.5 at upper prop medicinal liquid pH value, flow velocity 2.0BVh
-1, liquor strength is 0.41mgmL
-1Condition under, the strong basicity ion-exchange fibre post of crossing weight and be 14.0g, bed volume and be 140mL adsorbs.Be 55% ethanol and 3molL with strippant
-1The mixed liquor of hydrochloric acid (volume ratio 4: 1) 8BV, elution flow rate 4.0BVh
-1Carry out eluting.Recycled ethanol gets the saponin extract of purification, and wherein saponin content is 49.32%, and yield is 6.27%.
Claims (2)
1. the production method of a Radix Notoginseng or glycyrrhizin extract comprises step:
(1) will contain the raw material Radix Notoginseng of saponin or Radix Glycyrrhizae clean, dry, decoct lixiviate after pulverizing;
(2) lixiviating solution adsorbs with the ion-exchange fibre post;
(3) will be adsorbed on saponin eluting on the ion-exchange fibre post;
(4) the eluent drying obtains containing saponin purified extract powder;
Wherein, the extraction solvent that step (1) is used is formulated as water, alcohol or its mixture and soda acid pH value regulator, and the weight ratio of digestion agent and raw material is 10～30: 1; Extraction temperature is 35～90 ℃; PH value is 4.0～9.0; Extraction time is 1～6 hour; Extracting times 2～6 times;
Step (2) is that elder generation is with the water wet method dress post of 1～4 times of column volume, again with leaching liquid original liquid concentration or concentrated concentration 0.05～5.0gL
-1, 15～85 ℃ of temperature, flow velocity 0.1～6.0BVh
-1, the condition of pH value 5.0～11.0 is adsorbed;
Step (3) is first water elution with 1～3 column volume, with the eluant eluting of 3～15 times of column volumes, collects eluent again, and eluting temperature is 10～90 ℃; Flow velocity is 0.1～12.0BVh
-1Used eluant is that water, ethanol or its mixture and concentration are 0.1～6.0molL
-1The HCl pH adjusting agent take volume ratio as 1～9: 1 is formulated;
Step (4) is that Organic substance gets concentrated solution in the recovery eluent, obtains powder through vacuum decompression drying or lyophilization again.
2. according to production method claimed in claim 1, wherein the weight of step (2) use fiber and the ratio of medical material weight are 1: 2～30, and used fiber is the strong basicity ion-exchange fibre of domestic or import; PH adjusting agent is inorganic base, mineral acid, organic acid, organic base.
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