CN102702301A - Novel process for extracting diosgenin - Google Patents
Novel process for extracting diosgenin Download PDFInfo
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- CN102702301A CN102702301A CN2012102074585A CN201210207458A CN102702301A CN 102702301 A CN102702301 A CN 102702301A CN 2012102074585 A CN2012102074585 A CN 2012102074585A CN 201210207458 A CN201210207458 A CN 201210207458A CN 102702301 A CN102702301 A CN 102702301A
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- saponin
- diosgenin
- rhodotorula glutinis
- fermentation
- starch
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Abstract
The invention provides an extraction process of diosgenin, and particularly discloses a process for extracting saponin in yam through microbial strengthened fermentation in combination with a dilute acid catalytic hydrolysis method. The process comprises the following steps of: cleaning and crushing the yam; performing the microbial strengthened fermentation to separate the saponin from starch and cellulose; then hydrolyzing with dilute acid under the action of a catalyst to obtain the diosgenin; performing soxhlet extraction on hydrolysate by using a solvent; and finally crystallizing and drying to obtain the finished product diosgenin. The process has the advantages of simple process, short process time, less acid consumption, less wastewater, reduced COD (Chemical Oxygen Demand) in the wastewater, extreme easiness in treatment and capability of effectively reducing the cost and the pollution.
Description
Technical field
The present invention relates to a kind of extraction process of diosgenin, specifically be meant a kind of microbial augmentation fermentation, extract the technology of saponin in the Chinese yam in conjunction with the method for diluted acid catalytic hydrolysis.
Background technology
Saponin prepares raw materials such as steroid hormone class medicine; Can only from plant, obtain at present through certain technology; Basis, optimal midbody are diosgenins wherein to prepare steroid hormone class medicine; Diosgenin is to be used as basic material, the steroid hormone class medicine in the whole world 67% with it as raw material production.In order to strengthen the international competitiveness of China, imperative with innovation to the improvement of backward production diosgenin technical matters.
Yellow ginger formal name used at school Rhizome of Peltate Yam; (in the following description popular name yellow ginger that adopts) more; It extensively plants one band and the Changjiang river middle and upper reaches area in China Qinling Mountains; The yellow ginger diosgenin that China produces accounts for more than 60% of whole international market share, and major ingredients content is starch (45% ~ 50%), Mierocrystalline cellulose (40% ~ 50%), dioscin (2% ~ 4%) in the block rhizome of yellow ginger, also contains a spot of yellow pigment, tannin etc.
Directly acid-hydrolysis method is traditional processing technology backwardness, old that from the block rhizome of yellow ginger, extracts diosgenin, and the history in more than 50 year has been arranged from beginning till now:
Yellow ginger → washing → pulverizing → acid hydrolysis → filtration washing → oven dry → gasoline extraction → condensing crystal → spinning → oven dry → diosgenin
The problem that this technology mainly exists is following: 1) the block rhizome of yellow ginger is by direct acid hydrolysis the time; Owing to exist a large amount of starch and Mierocrystalline cellulose that hydrolysis is had very big obstruction and interference effect; Cause hydrolysis not thorough; Saponin content is very low in the dry thing of the work in-process-hydrolysate of output, thereby the saponin yield is also very low; 2) the direct water hydrolysate of repetitive scrubbing after acid hydrolysis repeatedly, water content consumption is very big, and half-finished loss is very serious in the middle of the water washing process.Because directly rely on strong acid that saponin(e is hydrolyzed, the acid that expends is many, causes using big water gaging to clean work in-process again, cause waste water quality situation complicacy, quantity discharged very big, environmental pollution is serious.Handle saponin waste water by ordinary method, water outlet at all can not qualified discharge.One ton of saponin of every production will expend vitriol oil 50-100 ton, 1000 tons of sewage effluents, about 30 tons of COD total amount.
Prior art has used diverse ways to reduce the acid consumption and minimizing COD discharging of technology; Such as using physical method for separation starch and Mierocrystalline cellulose, Chinese patent (application number 03125387.3,200410060679.X; 200410060777.3) adopt physical sepn, sieve through grinding and revolve point-score and separate starch and Mierocrystalline cellulose, handle remaining saponin(e again; This technology can significantly reduce disposal of pollutants, but since saponin(e mainly to be present in the cell walls with polyhydroxy substance bonded form, the mechanical-physical method can't be avoided the situation of carrying secretly in the sepn process; The facility investment of this method simultaneously increases, and the physical process complicacy is loaded down with trivial details, for effective separating starch and Mierocrystalline cellulose; Need in technological process, add a large amount of water; Have the situation that water loss is big, sewage is many equally, in addition, this process method can not effectively be handled the situation of starch conversion in the dried yellow ginger.
Chinese patent (application number 03127944.9) has proposed to carry out pretreated method with UW; Shorten the reaction times, concentrated oven dry through strong acid treatment hydrolyzation system is later distilled simultaneously, extracted saponin with the method for supercritical extraction again; There is not sewage discharge; But this technology not only facility investment is big, and the technology cost is too high, and industrial value is very low.Use tensio-active agent and UW to combine the separating starch Mierocrystalline cellulose in the Chinese patent (publication number CN101705275), again through resin column purification saponin(e liquid, complex process, water consumption is big, and industrial value is very low.
Solvent-extraction process is a domestic method of extracting natural product; But because saponin content is low in the Chinese yam, combines comparatively closely with polyhydroxy substance in the Chinese yam, extract very complicacy; And yield is lower; Directly (" Wuhan University Of Science and Engineering's journal " the 06th phase in 2005 shows that Cheng Jun) yield is merely 63.7% of traditional technology to the report through the solvent extraction saponin.Adopt salt to destroy the binding substances of saponin(e and polyhydroxy substance in the Chinese patent (publication number CN101560239), improve extraction efficiency and separating effect, effectively reduce disposal of pollutants; But this technology has been used the high amounts of solvents extraction, has that filter residue is carried secretly, distill repeatedly etc. causes the excessive problem of solvent loss, simultaneously; Increased the recovery process that extracts solvent, complex equipments, power consumption is big; And when handling saponin(e, use traditional technology, and still excessive with the acid amount, the liquid waste disposal trouble.
Therefore, the farinose in the more effective processing Chinese yam, more effective extraction saponin becomes the emphasis of technology.Chinese patent (application number: 02138773.7,03134449.6,03134450; 200310111250.4,200410026364.3,200410013355.0,200610125197.7,200610124515.8) use enzyme that Chinese yam is handled; Farinose is changed into available substance dissolves in water; Isolate sedimentary saponin(e then, again saponin(e is handled.But there is following problem in technology: at first, the conditional request of enzymolysis is high, needs to add the water of several times of amounts of material, and the liquid waste disposal amount is big; Sacchariferous saponin(e slurry viscosity is big, separation difficulty; Cellulase hydrolysis is incomplete, has increased sour consumption and pollution in the follow-up acidolysis process.
In sum; The turmeric saponin industry can be developed rapidly; Produce huge economic benefit and social benefit; Can prevent the problem of environmental pollution that it is brought again in developing process rapidly, just must carry out omnibearing improvement turmeric saponin existing manufacturing technique and yellow ginger waste water treatment process.This technology not only can change the drawback of traditional processing technology; Improve the extraction yield of saponin; But also can reduce amount that produces waste water and the concentration that greatly reduces organic substance the waste water from the source; Alleviate wastewater treatment pressure, reduce treatment technology difficulty and processing cost, effluent quality all can reach emission standard.
Summary of the invention
The process for cleanly preparing that the purpose of this invention is to provide saponin in a kind of extraction yellow ginger of without sewage discharge.
The objective of the invention is to realize in the following manner:
A: Chinese yam is cleaned pulverizing; Add less water and become pasty state; Physical sepn is crossed starch and cellulosic saponin(e slurry or not separating starch and cellulosic mashed prod, add the rhodotorula glutinis of solid content 0.2-1.2%, 32 ℃-40 ℃ temperature bottom fermentations 12-48 hour;
B: tangible layering can appear in the mother liquor that ferments, and top liquid portion is separated, and the bottom aqueous precipitate partly gets into next procedure, and the upper clear supernate that contains rhodotorula glutinis in this step can be put into next fermenting step and use as Rhodotorula glutinis fungus;
C: behind the liquid portion above the mother liquor that ferments separates; The bottom aqueous precipitate is partly added 1.5-4.0% molysite or ferrous salt, also slowly adds concentration sour in the vitriol oil or hydrochloric acid to this suspension-s is 0.2N-1N; Pressurization 0.2-0.3MPa catalytic hydrolysis 2-3 hour filters, and washing obtains hydrolyzate; Waste filtrate after the filtration is in unslaked lime and continue fermentative processing, and COD reaches emission standard and reclaims and use;
D: extract carrying out Suo Shi with industrial naptha or sherwood oil equal solvent after the hydrolyzate drying, crystallization then, drying obtain diosgenin, extract the remaining Mierocrystalline cellulose in back and directly act as a fuel or other raw material.
Detail operations is following:
1) cadmium yellow ginger carries out thick, thin twice pulverizing, adds the water making beating;
2) isolate Mierocrystalline cellulose slag and starch through natural subsidence, also can not separate direct entering next step;
3) suspension liquid of collecting adds efficient rhodotorula glutinis fermentation 24-48 hour, removes supernatant (supernatant can be used as the yeast kind and puts into next fermenting step), gets sedimentary saponin(e mixed solution;
4) to add molysite or ferrous salt to concentration be 0.2N-0.5N and add the vitriol oil or concentrated hydrochloric acid to concentration is 0.2N-1N, pressurization 0.2-0.3MPa catalytic hydrolysis 2-3 hour;
5) the intact back of hydrolysis filter residue is neutralized to neutrality, then filtration, oven dry, lixiviate, concentrates, cooling, recrystallization, gets rid of filter, dries and obtain saponin;
6) acid filtrate neutralizes with lime, and more than the rhodotorula glutinis aeration degraded COD85% with screening, pigment is degraded more than 60%;
7) sedimentation of water outlet adding medicine, decolouring behind the aeration, the waste water reusable edible.
Benefit of the present invention is:
1) fermentation of the efficient rhodotorula glutinis of screening can significantly reduce water consumption, can degraded starch, Mierocrystalline cellulose etc., promote the concentration of saponin(e mixed solution, and reduce the usage quantity of acid, improve the saponin yield;
2) use catalyzer to quicken the saponin(e hydrolysis, reduce with the acid amount;
3) the effective organism in the degrading waste water of efficient rhodotorula glutinis reduces pollution.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Lift three embodiment below, the present invention is done further explanation, but the present invention be not only limited to these embodiment:
Embodiment 1
(1) takes by weighing a fresh Rhizome of Peltate Yam rhizome sample 100 grams that remove mud of cleaning;
(2) sample is pulverized, the water that adds 200 grams breaks into pulpous state;
(3) solidliquid mixture is filtered with double gauze, filter residue adds 100 gram water, continues to pulverize once with nine positive cooking machines, collects filtrating, and the filter residue single collection is pending;
(4) filtrating is poured in the separating funnel, standing demix, the upper strata is a supernatant liquid, and the centre is the suspension liquid layer, and lower floor's white is starch layer, and 350ml is in beaker altogether to pour out upper strata and middle layer, and it is pending to collect lower floor's starch.
(5) add Rhodotorula glutinis fungus 0.2 gram in the suspension liquid, standing for fermentation 24h, separation of supernatant part 250ml (rhodotorula glutinis bacterium liquid A), remaining saponin(e enriched mixture 100ml changes autoclave over to;
(6) vitriol oil adds slowly in the suspension liquid that to regulate sulfuric acid concentration be 0.2N, adds 4 gram ferrous sulfates, 125 ℃ of attemperation, and hydrolysis is 3 hours in autoclave.
(7) hydrolyzed solution filters to isolate filter residue, successively uses a small amount of lime aqueous solution, water to clean to pH value and is neutrality, and merging filtrate and washing lotion are about 120ml.
(8) filter residue is that hydrolyzate is 1.8 grams in 60 ℃ of oven for drying.
(9) filter residue carries out reflux cycle extraction 6h with the 250ml sherwood oil in apparatus,Soxhlet's.
(10) extracting solution is concentrated into the crystallization of 30ml postcooling, drying, is weighed as 0.67 gram.
Embodiment 2
(1) takes by weighing a fresh Rhizome of Peltate Yam rhizome sample 100 grams that remove mud of cleaning;
(2) sample is pulverized, added the rhodotorula glutinis bacterium liquid A furnishing pulpous state among the embodiment 1;
(3) standing for fermentation 48h, separation of supernatant part 200ml (rhodotorula glutinis bacterium liquid A), remaining saponin(e enriched mixture 100ml changes autoclave over to;
(4) vitriol oil adds slowly in the suspension liquid that to regulate sulfuric acid concentration be 0.5N, adds 1.5 gram sulphate of iron, 125 ℃ of attemperation, and hydrolysis is 3 hours in autoclave.
(5) hydrolyzed solution filters to isolate filter residue, successively uses a small amount of lime aqueous solution, water to clean to pH value and is neutrality, and merging filtrate and washing lotion are about 120ml.
(6) filter residue is that hydrolyzate is 5.3 grams in 60 ℃ of oven for drying.
(7) filter residue carries out reflux cycle extraction 6h with the 250ml sherwood oil in apparatus,Soxhlet's.
(8) extracting solution is concentrated into the crystallization of 30ml postcooling, drying, is weighed as 0.75 gram.
Embodiment 3
(1) takes by weighing a fresh Rhizome of Peltate Yam rhizome sample 100 grams that remove mud of cleaning;
(2) sample is pulverized, added rhodotorula glutinis bacterium 1.2 gram and 250 milliliters of furnishing pulpous states of water;
(3) standing for fermentation 48h, separation of supernatant part 250ml (rhodotorula glutinis bacterium liquid A), remaining saponin(e enriched mixture 100ml changes autoclave over to;
(4) concentrated hydrochloric acid adds slowly in the suspension liquid that to regulate concentration of hydrochloric acid be 1.0N, adds 1.5 gram iron chloride salt, 125 ℃ of attemperation, and hydrolysis is 3 hours in autoclave.
(5) hydrolyzed solution filters to isolate filter residue, successively uses a small amount of lime aqueous solution, water to clean to pH value and is neutrality, and merging filtrate and washing lotion are about 120ml.
(6) filter residue is that hydrolyzate is 5.2 grams in 60 ℃ of oven for drying.
(7) filter residue carries out reflux cycle extraction 6h with the 250ml sherwood oil in apparatus,Soxhlet's.
(8) extracting solution is concentrated into the crystallization of 30ml postcooling, drying, is weighed as 0.74 gram.
Claims (3)
1. diosgenin novel technology for extracting is characterized in that:
A: Chinese yam is cleaned pulverizing; Add less water and become pasty state; Physical sepn is crossed starch and cellulosic saponin(e slurry or not separating starch and cellulosic mashed prod, add the rhodotorula glutinis of solid content 0.2-1.2%, 32 ℃-40 ℃ temperature bottom fermentations 12-48 hour;
B: tangible layering can appear in the mother liquor that ferments, and top liquid portion is separated, and the bottom aqueous precipitate partly gets into next procedure, and the upper clear supernate that contains rhodotorula glutinis in this step can be put into next fermenting step and use as Rhodotorula glutinis fungus;
C: behind the liquid portion above the mother liquor that ferments separates; The bottom aqueous precipitate is partly added 1.5-4.0% molysite or ferrous salt, also slowly adds concentration sour in the vitriol oil or hydrochloric acid to this suspension-s is 0.2N-1N; Pressurization 0.2-0.3MPa catalytic hydrolysis 2-3 hour filters, and washing obtains hydrolyzate; Waste filtrate after the filtration is in unslaked lime and continue fermentative processing, and COD reaches emission standard and reclaims and use;
D: extract carrying out Suo Shi with industrial naptha or sherwood oil equal solvent after the hydrolyzate drying, crystallization then, drying obtain diosgenin, extract the remaining Mierocrystalline cellulose in back and directly act as a fuel or other raw material.
2. diosgenin novel technology for extracting according to claim 1 is characterized in that: described microbial augmentation fermentation is meant uses the rhodotorula glutinis forced fermentation to separate saponin(e.
3. diosgenin novel technology for extracting according to claim 1 is characterized in that: use catalyzer to combine diluted acid that saponin(e is hydrolyzed, catalyzer is molysite or ferrous salt, and concentration is 0.2N-0.5N.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102074585A CN102702301A (en) | 2012-06-22 | 2012-06-22 | Novel process for extracting diosgenin |
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| CN2012102074585A CN102702301A (en) | 2012-06-22 | 2012-06-22 | Novel process for extracting diosgenin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103114047A (en) * | 2013-02-03 | 2013-05-22 | 江南大学 | Strain for efficiently converting saponins in turmeric and applications thereof |
| CN105111274A (en) * | 2015-09-16 | 2015-12-02 | 张家界久瑞生物科技有限公司 | Method for extracting diosgenin saponin through yeast fermentation |
| CN105669824A (en) * | 2014-11-18 | 2016-06-15 | 陕西秦岭生物工程有限公司 | Method for extracting diosgenin by adopting wall-breaking method |
| CN110592142A (en) * | 2019-09-25 | 2019-12-20 | 山东萃茵生物科技有限公司 | Clean type yellow ginger fermentation process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394869A (en) * | 2002-07-22 | 2003-02-05 | 张万举 | dioscin and extraction method of diosgenin |
| CN1699399A (en) * | 2004-05-23 | 2005-11-23 | 张万举 | Process for preparing yam saponin |
| CN102061319A (en) * | 2010-11-09 | 2011-05-18 | 佛山市正合生物能源有限公司 | Method for preparing biological fatty oil from Dioscorea camposita |
| CN102321184A (en) * | 2011-08-08 | 2012-01-18 | 武汉纺织大学 | The application technology as the second resource of fresh Rhizome of Peltate Yam |
-
2012
- 2012-06-22 CN CN2012102074585A patent/CN102702301A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394869A (en) * | 2002-07-22 | 2003-02-05 | 张万举 | dioscin and extraction method of diosgenin |
| CN1699399A (en) * | 2004-05-23 | 2005-11-23 | 张万举 | Process for preparing yam saponin |
| CN102061319A (en) * | 2010-11-09 | 2011-05-18 | 佛山市正合生物能源有限公司 | Method for preparing biological fatty oil from Dioscorea camposita |
| CN102321184A (en) * | 2011-08-08 | 2012-01-18 | 武汉纺织大学 | The application technology as the second resource of fresh Rhizome of Peltate Yam |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103114047A (en) * | 2013-02-03 | 2013-05-22 | 江南大学 | Strain for efficiently converting saponins in turmeric and applications thereof |
| CN103114047B (en) * | 2013-02-03 | 2014-09-24 | 江南大学 | Strain for efficiently converting saponins in turmeric and applications thereof |
| CN105669824A (en) * | 2014-11-18 | 2016-06-15 | 陕西秦岭生物工程有限公司 | Method for extracting diosgenin by adopting wall-breaking method |
| CN105111274A (en) * | 2015-09-16 | 2015-12-02 | 张家界久瑞生物科技有限公司 | Method for extracting diosgenin saponin through yeast fermentation |
| CN110592142A (en) * | 2019-09-25 | 2019-12-20 | 山东萃茵生物科技有限公司 | Clean type yellow ginger fermentation process |
| CN110592142B (en) * | 2019-09-25 | 2021-07-23 | 山东萃茵生物科技有限公司 | Clean type yellow ginger fermentation process |
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Application publication date: 20121003 |