CN101838338B - Method for extracting and separating panax japonicus saponin and polysaccharide - Google Patents
Method for extracting and separating panax japonicus saponin and polysaccharide Download PDFInfo
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- CN101838338B CN101838338B CN2010101308651A CN201010130865A CN101838338B CN 101838338 B CN101838338 B CN 101838338B CN 2010101308651 A CN2010101308651 A CN 2010101308651A CN 201010130865 A CN201010130865 A CN 201010130865A CN 101838338 B CN101838338 B CN 101838338B
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Abstract
The invention relates to a method for extracting and separating panax japonicus saponin and polysaccharide from the panax japonicus, which comprises the following steps of: extracting the panax japonicus; adjusting a pH value; performing foam separation; and purifying panax japonicus polysaccharide. The method has the advantages of high separating efficiency, high purity, large extraction volume, low energy consumption, simple device, low cost, no introduction of an organic solvent pollutant, no damage to the structure of the panax japonicus saponin and the like. A surfactant is not necessary to add in the foam extraction process, so the problems of recovery of the surfactant and the pollution caused by the recovery are solved.
Description
[technical field]
The invention belongs to the Chinese medicinal materials processing technique field, more specifically, the present invention relates to a kind of method from rhizome of Japanese Ginseng extraction separation Rhizoma Panacis Japonici saponin and polysaccharide.
[background technology]
Rhizoma Panacis Japonici saponin is that a class can produce a large amount of lasting foamy complicated molecules through jolting in the aqueous solution, and its molecular weight is big, polarity is bigger, and is water-soluble strong, separates, refining certain degree of difficulty arranged.The extraction separation inefficiency of traditional method, loss of effective components is serious, and may cause environmental pollution etc.In the new separation technology, the utilization of technology such as supercritical liq extraction, ultrasound assisted extraction technique, macroporous adsorbent resin separation when having improved the separating effect of Rhizoma Panacis Japonici saponin, also exists defective separately.For example, the facility investment of supercritical liquid extraction technique and ultrasound assisted extraction technique is excessive, and a small amount of extraction separation of pharmaceutically active ingredient or efficient part lacks the pilot scale and the industrial large-scale production research of its production in only limiting at present; There are shortcomings such as adsorption selectivity is poor, technical difficulty is big, resin regeneration difficulty in the macroporous adsorbent resin technology.The present invention is based on and contains Rhizoma Panacis Japonici saponin class Chinese medicine and can carry out the technology that modernization that isolating principle develops separates Rhizoma Panacis Japonici saponin by bubbling.Rare Chinese medicinal materials rhizome of Japanese Ginseng contains a large amount of saponin components, utilizes the surface-active difference of other compositions such as its saponin component and polysaccharide, is separating medium with the bubble, and saponin component in the rhizome of Japanese Ginseng is carried out extraction separation.Extract the compositions such as polyose that still contain and have physiologically active in the debris,, further its polyose composition is extracted, makes with extra care for promoting the comprehensive development and utilization of rhizome of Japanese Ginseng herb resource.Advantages such as the present invention compares with traditional method, has the separation efficiency height, and purity is good, does not bring organic solvent into and pollutes, and does not destroy advantages such as saponin(e structure, compares with other new separation technologies, and it is little that foam separation has energy consumption again, and equipment is simple, and is with low cost.And because saponin component is natural surface active ingredient, therefore in foam extraction process, need not add tensio-active agent in addition, do not exist the screening and the consumption of tensio-active agent to investigate problem like this, do not have the recovery of tensio-active agent and the pollution problem that is brought thereof yet.
[summary of the invention]
[technical problem that will solve]
The purpose of this invention is to provide a kind of foam separation method of from the Chinese medicinal materials rhizome of Japanese Ginseng, extracting Rhizoma Panacis Japonici saponin and polysaccharide.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to the extraction and separation method of a kind of Rhizoma Panacis Japonici saponin and polysaccharide.
This method comprises the steps:
The extraction of A, rhizome of Japanese Ginseng:
Taking by weighing 30-50 weight part rhizome of Japanese Ginseng powder, is that 10-20 adds water according to the weight ratio of rhizome of Japanese Ginseng powder and water, extracts 2-4 time under little condition of boiling, and each 1-3h filters, and these filtrates merging obtain described rhizome of Japanese Ginseng extracting solution;
B, pH regulator
The pH regulator that uses the rhizome of Japanese Ginseng extracting solution that mineral acid or alkali obtains step (A) is to 4.5-5.0;
C, foam separation:
The rhizome of Japanese Ginseng extracting solution that step (B) is obtained is added in the foam separating tower, bubbling air or rare gas element at the bottom of the described tower, the throughput ratio of described rhizome of Japanese Ginseng extracting solution and described rare gas element is 4-8: 3-6, separates the foam solution and the debris that contains Rhizoma Panacis Japonici polysaccharides that obtain being rich in Rhizoma Panacis Japonici saponin;
The concentration ratio of described Rhizoma Panacis Japonici saponin is more than 5.5, and the purity ratio is more than 2.1, and the rate of recovery is more than 90%;
The purifying of D, Rhizoma Panacis Japonici polysaccharides
In described debris, add 50-90 volume % aqueous ethanolic solution, make in the described concentrated extracting solution final alcohol concn reach 48-70 volume %, at room temperature carrying out alcohol precipitation spends the night, carry out filtering separation then, through washing and drying under reduced pressure, obtain the Rhizoma Panacis Japonici polysaccharides extract of 60%-90% mass percent concentration.
A preferred embodiment of the invention, the granularity of described rhizome of Japanese Ginseng powder are the 20-40 orders.
According to another kind of preferred implementation of the present invention, described mineral acid is selected from hydrochloric acid, sulfuric acid or nitric acid, and described mineral alkali is selected from sodium hydroxide, potassium hydroxide or yellow soda ash.
According to another kind of preferred implementation of the present invention, described bubbled gas is air or rare gas element, and wherein, rare gas element is selected from nitrogen, argon gas or nitrogen-ar mixture.
According to another kind of preferred implementation of the present invention, the Rhizoma Panacis Japonici saponin mass concentration in the resultant rhizome of Japanese Ginseng extracting solution of step (B) is 0.14-0.25mg/mL.
According to another kind of preferred implementation of the present invention, the throughput ratio of described rhizome of Japanese Ginseng extracting solution and described air or rare gas element is 6: 4.
The present invention relates to a kind of foam separation device that is used for Rhizoma Panacis Japonici saponin and polysaccharide extraction separation, it is characterized in that what described device was made up of producer gas generator (1), the wetting bottle of gas (2), control valve (3), gas meter (4), gas distributor (5), foam separating tower (6), demister (7), broken foam liquid receiving flask (8) and raffinate receiving flask (9).
According to another kind of preferred implementation of the present invention, described gas wetting bottled have distilled water or tap water.
According to another kind of preferred implementation of the present invention, the aperture of gas distributor is 0.2-0.5mm.
Below the present invention will be described in more detail.
The present invention relates to the extraction and separation method of a kind of Rhizoma Panacis Japonici saponin and polysaccharide.
This method comprises the steps:
The extraction of A, rhizome of Japanese Ginseng:
Taking by weighing 30-50 weight part rhizome of Japanese Ginseng powder, is that 10-20 adds water according to the weight ratio of rhizome of Japanese Ginseng powder and water, extracts 2-4 time under little condition of boiling, and each 1-3h filters, and these filtrates merging obtain described rhizome of Japanese Ginseng extracting solution.
A large amount of research work show, the main active ingredient of rhizome of Japanese Ginseng is Rhizoma Panacis Japonici saponin (chikusetsusaponin), ginsenoside (ginsenoside), Rhizoma Panacis Japonici polysaccharides (tochhibanan) and volatilization wet goods, also contain multiple water-soluble amino acids, comprising 8 kinds of essential amino acids.Adopt method of the present invention mainly extract with separate rhizome of Japanese Ginseng in Rhizoma Panacis Japonici saponin and panax japonicus polysaccharide.
Described rhizome of Japanese Ginseng for example can be the rhizome of Japanese Ginseng Chinese medicinal materials of selling on the present China market, for example be selected from the rhizome of Japanese Ginseng of Xuanen County, Enshi, Hubei Province Chinese toon wood battalion rhizome of Japanese Ginseng planting base plantation, it is an Araliaceae rhizome of Japanese Ginseng Panaxjaponicus C.A.Mey. rhizome, for pharmacopeia is recorded kind.
Then, rhizome of Japanese Ginseng medicinal material rhizome is removed silt, use and clean at normally used in the art ultrasonic cleaner, the KQ-250B type ultrasonic cleaner that for example uses Kunshan Ultrasonic Instruments Co., Ltd. to produce cleans.Rhizome of Japanese Ginseng after the cleaning cuts into medicine materical crude slice, re-uses at normally used in the art vacuum drying oven to carry out drying, and the vacuum drying oven that for example German MMM company produces carries out drying.Then, use normally used pulverizer in medicinal material processing is pulverized the exsiccant rhizome of Japanese Ginseng, and the rhizome of Japanese Ginseng of pulverizing is sieved with standard sieve again, collects 20-40 purpose rhizome of Japanese Ginseng powder.
Take by weighing 30-50 weight part rhizome of Japanese Ginseng powder, weight ratio according to rhizome of Japanese Ginseng powder and water is that 10-20 adds water, its mixture uses and carries out heating and refluxing extraction at normally used in the art extractor under little condition of boiling, and for example uses Shanghai grand emerging mechanical device industry manufacturing company electronic thermostatic stainless steel water bath of producing and the SXT-06 type apparatus,Soxhlet's that the big vast discipline plant and instrument in Shanghai company limited provides to carry out heating and refluxing extraction.
Repeat to extract 2-4 time each 1-3h like this.After each the extraction, the filter method and the equipment that use those skilled in the art to know filter, and the merging of these filtrates obtains described rhizome of Japanese Ginseng extracting solution.
B, pH regulator
The pH regulator that uses the rhizome of Japanese Ginseng extracting solution that mineral acid or alkali obtains step (A) is to 4.5-5.0.4.6-4.9 preferably.
In the present invention, mineral acid or alkali should be appreciated that it is except that regulating its pH, should not produce the mineral acid or the alkali of any influence to its extracting solution.Generally all use the mineral acid or the alkali aqueous solution of intermediate concentration when using mineral acid or alkali to carry out the pH regulator of rhizome of Japanese Ginseng extracting solution.
Described mineral acid is selected from hydrochloric acid, sulfuric acid or nitric acid.Preferably, described mineral acid is selected from hydrochloric acid or sulfuric acid.
Described mineral alkali is selected from sodium hydroxide, potassium hydroxide or yellow soda ash.Preferably, described mineral alkali is selected from sodium hydroxide or yellow soda ash.
C, foam separation:
The rhizome of Japanese Ginseng extracting solution that step (B) is obtained is added in the foam separating tower, bubbling air or rare gas element at the bottom of the described tower, the throughput ratio of described rhizome of Japanese Ginseng extracting solution and described air or rare gas element is 4-8: 3-6, separates the foam and the debris that contains Rhizoma Panacis Japonici polysaccharides that obtain being rich in Rhizoma Panacis Japonici saponin.
In the present invention, use foam separation device of the present invention (seeing accompanying drawing 1) to carry out foam separation.Described foam separating tower is the normally used foam separating tower in the chemical technology field.
The gas distributor aperture of described foam separating tower is 0.2-0.5mm.
Described rare gas element is selected from nitrogen, argon gas or nitrogen-ar mixture.Preferably, described rare gas element is selected from nitrogen or argon gas.More preferably, described rare gas element is a nitrogen.
Preferably, the throughput ratio of described rhizome of Japanese Ginseng extracting solution and described bubbled gas is 6: 4.
Then, measure amount, calculate recovery rate, concentration ratio and the purity ratio of Rhizoma Panacis Japonici saponin and solid substance in rhizome of Japanese Ginseng extracting solution, the foam solution respectively, to filter out the best foam separation processing condition of Rhizoma Panacis Japonici saponin.Wherein,
The total mass of Rhizoma Panacis Japonici saponin * 100% in Rhizoma Panacis Japonici saponin total mass/extracting solution in the rate of recovery=foam solution;
Rhizoma Panacis Japonici saponin purity (%) in the purity of Rhizoma Panacis Japonici saponin (%)/extracting solution in the purity ratio=foam solution;
Saponin(e quality/extracting solution in purity=extracting solution concentrates quality * 100% that obtains solid substance; Rhizoma Panacis Japonici saponin mass concentration in the mass concentration/extracting solution of Rhizoma Panacis Japonici saponin in concentration ratio=foam solution;
The mensuration of solid substance: pipette 25 or 50mL (volume V) determinand, (quality is M to place the constant weight furnace pot
1), in water-bath, evaporate into driedly, place 105 ℃ of baking ovens to dry again to constant weight, claim that (quality is M to its quality
2), according to formula (M
2-M
1)/V calculates solid quality concentration.
The measuring method of Rhizoma Panacis Japonici saponin is as follows:
The preparation of need testing solution:
Pipette rhizome of Japanese Ginseng extracting solution, separating obtained foam solution 10mL respectively, use is with water saturated n-butanol extraction 4 times, each 10mL, merge butanol extraction liquid, use then with the saturated water 20mL of propyl carbinol and wash, divides the butanol extraction liquid merging that obtains after dried up, evaporate into dried, the pure dissolve with methanol of its residue transfers in the 25mL volumetric flask, and adds to scale.
The preparation of reference substance solution:
Precision takes by weighing ginsenoside Re's (the Chengdu HPLC of Bioisystech Co., Ltd of Cisco＞98%) reference substance 10.4mg, puts in the 10mL volumetric flask, adds methyl alcohol to scale, shakes up, promptly.
The drafting of typical curve:
Accurate reference substance solution 100,120,180,200, the 240 μ L that draw put in the 10mL tool plug test tube, volatilize solvent after, add 5% Vanillin-glacial acetic acid solution 0.2mL respectively, perchloric acid 0.8mL, jump a queue, shake up, in 60 ℃ of heating in water bath 15min, take out, put and cool off 3min in the ice-water bath, add glacial acetic acid 5mL respectively, shake up, after leaving standstill 8min, survey absorbance at the 552nm place.With the working sample quality absorbancy is returned, get typical curve: A=0.0025X-0.0418, R
2=0.9993.
Need testing solution is measured:
Precision pipettes need testing solution 0.5mL or 1mL puts in the 10mL tool plug test tube, volatilizes solvent, is measuring the absorbancy of measuring need testing solution under the identical condition of absorbancy with reference substance solution, and is calculating mass concentration according to above-mentioned typical curve.
The purifying of D, Rhizoma Panacis Japonici polysaccharides
In the resulting debris of step (C) foam separation, add 70-100 weight % aqueous ethanolic solution, make in the described concentrated extracting solution final alcohol concn reach 40-70 weight %, at room temperature carrying out alcohol precipitation spends the night, carry out filtering separation then, through washing and drying under reduced pressure, obtain the Rhizoma Panacis Japonici polysaccharides extract of 60%-90% mass percent concentration.
On meaning of the present invention, alcohol precipitation utilizes the polyose composition can not be dissolved in ethanol exactly and impurity is dissolved in the alcoholic acid characteristic, and after adding ethanol, impurity component changes and is dissolved in the ethanol that the polyose composition is then precipitated to come out.The purpose of alcohol precipitation is to keep medicine polyose composition in order to remove impurity, thereby the alcohol precipitation operation should be crucial.
Preferably, add 95 volume % aqueous ethanolic solutions (industrial spirit) in the concentrated extracting solution that obtains, make that final alcohol concn reaches 60 volume % in the described concentrated extracting solution, at room temperature carry out alcohol precipitation and spend the night.
In the present invention, the polysaccharide content in the described Rhizoma Panacis Japonici polysaccharides solution is to adopt in the phenolsulfuric acid colorimetry that adopts usually in the art to measure.
The invention still further relates to a kind of foam separation device that is used for Rhizoma Panacis Japonici saponin and polysaccharide extraction separation.Described tripping device is made up of producer gas generator 1, the wetting bottle 2 of gas, control valve 3, gas meter 4, gas distributor 5, foam separating tower 6, demister 7, broken foam liquid receiving flask 8 and raffinate receiving flask 9.
Above-mentioned rhizome of Japanese Ginseng extracting solution is added in the foam separating tower 6, the gas that is produced by producer gas generator 1 is by the wetting bottle 2 of the gas that distilled water or tap water are housed, again by control valve 3 and gas meter 4 controls and detected gas flow, treat that gas flow is stable after the gas distributor 5 at 6 ends of foam separating tower enters foam separating tower 6, this gas and rhizome of Japanese Ginseng extracting solution thorough mixing in foam separating tower 6, form a large amount of foams, these foams rise by demister 7, enter brokenly foam liquid receiving flask 8 behind the froth breaking, the raffinate that obtains behind the foam separation enters raffinate receiving flask 9, carries out the mensuration of Rhizoma Panacis Japonici saponin then.
Various piece all is a normally used unit in the technology of the present invention field in the foam separation device of the present invention.
Described producer gas generator also can normally used high-pressure air source, for example gas cylinder or the air compressor of knowing usually people in the art.
Debubbling method of the present invention is that foam is placed natural froth breaking of air or adding organic solvent froth breaking.
The aperture of described gas distributor is 0.2-0.5mm.
[beneficial effect]
Compare with traditional method, method of the present invention has the separation efficiency height, and good product purity is not also introduced the organic solvent pollutent, does not destroy advantages such as Rhizoma Panacis Japonici saponin structure, and the while has advantages such as extracted amount is big, and energy consumption is little, and equipment is simple, and is with low cost again.And because the Rhizoma Panacis Japonici saponin constituents is natural surface active ingredient, therefore in foam extraction process, do not need to add in addition tensio-active agent, do not exist the screening and the consumption of tensio-active agent to investigate problem like this, do not have the recovery of tensio-active agent and the pollution problem that is brought thereof yet.
[description of drawings]
Fig. 1: rhizome of Japanese Ginseng extracting solution foam separation process flow sheet
1-producer gas generator, the wetting bottle of 2-gas, 3-control valve, 4-gas meter, 5-gas distributor, 6-foam separating tower, 7-demister, the broken foam liquid receiving flask of 8-, 9-raffinate receiving flask.
Fig. 2: gas velocity is to the influence of foam separation
Fig. 3: the Rhizoma Panacis Japonici saponin mass concentration is to the influence of foam separation in the extracting solution
Fig. 4: inlet amount is to the influence of foam separation
Fig. 5: pH value is to the influence of foam separation
[embodiment]
The extraction and separation method of Rhizoma Panacis Japonici saponin of the present invention and polysaccharide
This method steps is as follows:
The extraction of A, rhizome of Japanese Ginseng:
Taking by weighing 40 weight parts, 25 order rhizome of Japanese Ginseng powder, is 15 to add water according to the weight ratio of rhizome of Japanese Ginseng powder and water, extracts 3 times under little condition of boiling, and each 2h filters, and the merging of these filtrates obtains described rhizome of Japanese Ginseng extracting solution;
B, pH regulator
Use 1molL
-1Aqueous hydrochloric acid and 1molL
-1The pH regulator to 4.8 of the rhizome of Japanese Ginseng extracting solution that aqueous sodium hydroxide solution obtains step (A);
C, foam separation:
Use foam separation device of the present invention to carry out, the rhizome of Japanese Ginseng extracting solution that step (B) is obtained is added in the foam separating tower 6, by the air of gas cylinder 1 or nitrogen gas by the wetting bottle 2 of the gas that distilled water is housed, the throughput ratio of described rhizome of Japanese Ginseng extracting solution and described gas is 6: 4, again by control valve 3 and gas meter 4 controls and detected gas flow, treat that gas flow is stabilized in 400mL/min after the gas distributor 5 at 6 ends of foam separating tower enters foam separating tower 6, this gas and rhizome of Japanese Ginseng extracting solution thorough mixing in foam separating tower 6, form a large amount of foams, these foams rise by demister 7, enter brokenly foam liquid receiving flask 8 behind the froth breaking, the raffinate that obtains behind the foam separation enters raffinate receiving flask 9, and the method that adopts the present invention to describe is then carried out the mensuration of Rhizoma Panacis Japonici saponin.
Rhizoma Panacis Japonici saponin content in the broken foam liquid is 0.95mg/ml;
Rhizoma Panacis Japonici saponin content in the raffinate is 0.01mg/ml.
The purifying of D, Rhizoma Panacis Japonici polysaccharides
In described debris, add 95 volume % aqueous ethanolic solutions (industrial spirit), make in the described concentrated extracting solution final alcohol concn reach 60 volume %, at room temperature carrying out alcohol precipitation spends the night, carry out filtering separation then, through washing and drying under reduced pressure, obtain the Rhizoma Panacis Japonici polysaccharides extract of 82.13% mass percent concentration again.
Experimental example 1: gas flow rate is to the influence of foam separation
The Rhizoma Panacis Japonici saponin mass concentration be 0.17mg/mL, pH value be 4.88 with inlet amount be under the situation of 600mL, studied of the influence of gas with various flow velocity to foam separation, it the results are shown in Figure 2.Can see that by Fig. 2 along with the increase of gas flow rate, concentration ratio and purity are than on a declining curve.Because gas velocity is accelerated, bubble residence time in separating device is short, and the surfactant adsorption time shortens, and the liquid between the foam do not have time enough to be back in the stoste, liquid content is increased, so concentration ratio decline.Gas speed is accelerated, and is unfavorable for foam selective absorption Rhizoma Panacis Japonici saponin, and the impurity that carries increases, and purity is than also descending.High gas flow rate helps producing more bubble, thereby more Rhizoma Panacis Japonici saponin is adsorbed onto on the liquid-gas interface, makes lather volume bigger, and isolating Rhizoma Panacis Japonici saponin total amount increases, and the rate of recovery is improved.
Experimental example 2: the Rhizoma Panacis Japonici saponin mass concentration of extracting solution is to the influence of foam separation
At gas flow rate is that 400mL/min, inlet amount are that 600ml, pH are under 4.88 the condition, extracting solution is diluted 6,9,12,15,18,24 times successively, studied that the Rhizoma Panacis Japonici saponin mass concentration is to the influence of separating effect in different extracting solutions, it the results are shown in Figure 3.As seen from Figure 3, along with the Rhizoma Panacis Japonici saponin mass concentration reduces, concentration ratio and purity are than in rising trend.Because mass concentration is lower, foam is unstable, the coalescence that easily breaks, and it is few to carry liquid measure secretly, and concentration ratio is higher.When mass concentration was low, other material competitive adsorption effects were also lower, and the impurity that foam is taken out of is few, and Rhizoma Panacis Japonici saponin purity is higher.When reducing because of mass concentration, froth stability descends, and the Rhizoma Panacis Japonici saponin that is adsorbed onto liquid-gas interface reduces, and the rate of recovery reduces.Comprehensive every index, selecting the feeding liquid mass concentration is 0.17mg/mL.
Experimental example 3: the influence of inlet amount
At gas flow rate is that 400mL/min, extracting solution Rhizoma Panacis Japonici saponin mass concentration are that 0.17mg/mL and pH are under 4.88 the condition, has studied the influence of different feeds amount to separating effect, and it the results are shown in Figure 4.As seen from Figure 4, concentration ratio is along with the increase of inlet amount, and raising earlier afterwards descends.This is that the residence time of bubble in liquid layer has with regard to long more, is beneficial to the absorption mass transfer because inlet amount is big more, but can shorten foam layer height simultaneously, and cause the foam drain time to reduce, liquid holdup increases, influenced concentration ratio, concentration ratio can reach an optimum value under certain inlet amount.With the increase of inlet amount, purity is more little than changing, and the rate of recovery is on a declining curve.Comprehensive every index, the selection inlet amount is 600ml.
Experimental example 4: the influence of pH value
At gas flow rate is that the Rhizoma Panacis Japonici saponin mass concentration is that 0.17mg/mL and inlet amount are under the situation of 600ml in 400mL/min, the extracting solution, has studied the influence of different pH values to separating effect, and it the results are shown in Figure 5.As seen from Figure 5, the original pH value of feeding liquid is 4.88, with saturated sodium hydroxide solution feeding liquid is transferred to neutrality after, can not produce foam, may be that acid Rhizoma Panacis Japonici saponin generates sodium salt, surfactivity reduces greatly.When the increase of feeding liquid acidity, the soup whipability strengthens, and lather volume increases, and the rate of recovery increases, but concentration ratio reduces.
Experimental example 5: the proof test of optimal separation condition
Using the rhizome of Japanese Ginseng extracting solution of Rhizoma Panacis Japonici saponin mass concentration as 0.17mg/mL, is that 600mL, pH value are under 4.88 the condition for 400mL/min, inlet amount in gas speed, carries out 3 foam separation and tests, and the results are shown in Table 1.
Table 1 proof test result
At gas flow rate is that 400mL/min, extracting solution Rhizoma Panacis Japonici saponin mass concentration are that 0.17mg/mL, inlet amount are that 600ml, pH value are under 4.88 the condition, the Rhizoma Panacis Japonici saponin concentration ratio is 5.6, the purity ratio is 2.2, the rate of recovery is 91.9%, this shows, adopt method of the present invention can realize the good separation of Rhizoma Panacis Japonici saponin and Rhizoma Panacis Japonici polysaccharides.
Experimental example 6: the proof test of polysaccharide purification technology
Get the foam separation raffinate that embodiment 1 obtains, concentrate and be settled to the test solution that every 1ml is equivalent to the 0.2g crude drug, prepare 6 parts altogether, add 95 volume % aqueous ethanolic solutions then respectively, reaching the ethanol ultimate density is 60 volume %, alcohol precipitation spends the night, after filtration, washing and drying under reduced pressure obtain dry Rhizoma Panacis Japonici polysaccharides extract.Adopt the phenolsulfuric acid colorimetry to measure, obtaining Rhizoma Panacis Japonici polysaccharides content is 82.13% mass percent concentration, RSD (relative standard deviation)=0.60%, and the result of this experimental example shows that this extraction and purification process stablizes feasible.
Claims (1)
1. the extraction and separation method of Rhizoma Panacis Japonici saponin and Rhizoma Panacis Japonici polysaccharides is characterized in that this method comprises the steps:
The extraction of A, rhizome of Japanese Ginseng
Taking by weighing an amount of rhizome of Japanese Ginseng medicinal material coarse powder, is that 10-20 adds water according to medicinal material and the weight ratio of extracting solvent, extracts 2-4 time under little condition of boiling, and each 1-3h filters, and the merging of these filtrates obtains described rhizome of Japanese Ginseng extracting solution;
B, pH regulator
The pH regulator that uses the rhizome of Japanese Ginseng extracting solution that mineral acid or alkali obtains step (A) is to 4.5-5.0;
C, foam separation
The rhizome of Japanese Ginseng extracting solution that step (B) is obtained is added in the foam separating tower, bubbling air or rare gas element at the bottom of the described tower, the throughput ratio of described rhizome of Japanese Ginseng extracting solution and described air or rare gas element is 4-8:3-6, separates the foam solution and the debris that contains Rhizoma Panacis Japonici polysaccharides that obtain being rich in Rhizoma Panacis Japonici saponin;
The concentration ratio of described Rhizoma Panacis Japonici saponin is more than 5.5, and the purity ratio is more than 2.1, and the rate of recovery is 90 above %;
The purifying of D, Rhizoma Panacis Japonici polysaccharides
In described debris, add 70-100 volume % aqueous ethanolic solution, make in the described concentrated extracting solution final alcohol concn reach 40-70 volume %, at room temperature carrying out alcohol precipitation spends the night, carry out filtering separation then, through washing and drying under reduced pressure, obtain the Rhizoma Panacis Japonici polysaccharides extract of 60%-90% mass percent concentration.
2, method according to claim 1, the granularity that it is characterized in that described rhizome of Japanese Ginseng powder are the 20-40 orders.
3, method according to claim 1 is characterized in that described mineral acid is selected from hydrochloric acid, sulfuric acid or nitric acid, and described mineral alkali is selected from sodium hydroxide, potassium hydroxide or yellow soda ash.
4, method according to claim 1 is characterized in that in described air or the rare gas element, rare gas element is selected from nitrogen, argon gas or nitrogen-ar mixture.
5, method according to claim 1 is characterized in that the total Rhizoma Panacis Japonici saponin mass concentration in the resultant rhizome of Japanese Ginseng extracting solution of step (B) is 0.14-0.25mg/ml.
6, method according to claim 1, the throughput ratio that it is characterized in that described rhizome of Japanese Ginseng extracting solution and described air or rare gas element is 6:4.
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| CN102134268B (en) * | 2011-01-14 | 2012-12-19 | 陕西中医学院 | Method for preparing panax japonicus saponin IVa and application of panax japonicus saponin IVa in preparing a medicament for protecting liver and lowering transaminase |
| CN102276752B (en) * | 2011-09-13 | 2013-06-05 | 陕西理工学院 | Device and method for extracting polysaccharides from agaric polysaccharide extracting solution by foam fractionation |
| CN103611157B (en) * | 2013-12-05 | 2015-02-11 | 三峡大学 | Panax japonicus saponin as well as preparation method and application thereof |
| CN103613680B (en) * | 2013-12-05 | 2016-06-01 | 三峡大学 | Alcohol-precipitated panax japonicus polysaccharide, preparation method and application thereof |
| CN109970286B (en) * | 2019-04-29 | 2020-06-09 | 南京瑞轩环保科技有限公司 | Treatment method of garlic processing wastewater |
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| CN1789220A (en) * | 2005-11-15 | 2006-06-21 | 江西汇仁药业有限公司 | Method for separating Chinese medicinal active substances |
| CN101249121A (en) * | 2008-03-24 | 2008-08-27 | 三峡大学 | Panax japonicus total saponins preparation and its applications in medicament for curing myocardial ischemia |
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| CN1789220A (en) * | 2005-11-15 | 2006-06-21 | 江西汇仁药业有限公司 | Method for separating Chinese medicinal active substances |
| CN101249121A (en) * | 2008-03-24 | 2008-08-27 | 三峡大学 | Panax japonicus total saponins preparation and its applications in medicament for curing myocardial ischemia |
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