CN1188425C - Novel process for preparing diosgenin - Google Patents
Novel process for preparing diosgenin Download PDFInfo
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- CN1188425C CN1188425C CNB021539979A CN02153997A CN1188425C CN 1188425 C CN1188425 C CN 1188425C CN B021539979 A CNB021539979 A CN B021539979A CN 02153997 A CN02153997 A CN 02153997A CN 1188425 C CN1188425 C CN 1188425C
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Abstract
The present invention discloses a new method for preparing diosgenin in dioscorea nipponica or other dioscorea plants in industrial production, which comprises: firstly, total saponin in medicinal material is extracted by ethanol; then, the total saponin is degraded by acid, and calcium oxide or calcium hydroxide is added in hydrolyzate; the hydrolyzate is treated with flow back extraction by ethanol; after recrystallization, the diosgenin of which the purity is more than 94% is prepared. The present invention solves the problems of large acid use amount and serious environmental pollution existing in a previous method for preparing diosgenin. Especially, ethanol is used to replace 120# gasoline for extracting hydrolyzate, and the problem of using combustible and explosive gasoline is solved. The method has the characteristics of simplicity, advanced technology, high safety and high applicability, and is favorable for environmental protection.
Description
Technical field
The invention relates to a kind of novel method of from Chinese medicine Ningpo Yam Rhizome or other Dioscoreaceae plant, extracting preparation medicine material diosgenin, belong to the field of Chinese medicines.
Background technology
Ningpo Yam Rhizome is the dry rhizome of Dioscoreaceae plant Dioscorea nipponica Mak. Ningpo Yam Rhizome (Dioscorea nipponica Makino), is traditional Chinese medical science Chinese medicine commonly used, has activating blood and relaxing tendons, effects such as the Li Shui that helps digestion, wind-expelling pain-stopping.Contain abundant steroidal saponin in the Ningpo Yam Rhizome, obtain diosgenin (Diosgenin) after the total saponins hydrolysis.Diosgenin is the main precursor raw material of synthesizing steroid hormone, also has reducing blood-fat, preventing osteoporosis and the antitumor action of highly significant simultaneously.Abroad the demand to diosgenin increases year by year, is one of principal item of China's medicine foreign exchange earning.So it is significant to research and develop new preparation diosgenin technology.Except that Ningpo Yam Rhizome, other Dioscoreaceae plant also can be used as the raw material that extracts diosgenin, as Dioscorea panthaica Prain et Burkill, and Rhizome of Peltate Yam etc.Bibliographical information in the past, the general employing from medicinal material of the preparation of diosgenin begins just use sulphuric acid hydrolysis, uses 120# gasoline extraction hydrolyzate then, must diosgenin behind the recrystallization.Report is also arranged with the method for preparing diosgenin that has improved.This method is earlier the medicinal material water to be made homogenate, adds the degraded of an amount of saccharifying enzyme or amylase, and then uses acid hydrolysis, uses 120# gasoline extracting diosgenin after the hydrolyzate drying again.The yield of latter's method is better than the former, but has increased technologies such as grinding, add enzyme liberating.The above-mentioned method for preparing dioscin is still being used at present.The common drawback of previous methods is: crude drug is directly used sour heating hydrolysis, because the medicinal material volume is big, the amount that expends acid is bigger, cost height not only, and caused serious pollution to environment; All use 120# gasoline extracting hydrolysate in two kinds of technologies after the hydrolysis, the gasoline large usage quantity because gasoline is the explosion-proof solvent of one-level, needs the explosion-proof factory building of one-level in the production process, and use is absolutely unsafe.Except that above-mentioned two kinds of methods, also having a kind of method is to extract diosgenin with the method for carbon dioxide upercritical fluid extraction, existing patent.This method has solved the problem with gasoline extracting hydrolyzate, but also needs to do entrainment agent with adequate amount of ethanol.Present carbon dioxide upercritical fluid extraction equipment maximum be 90 liters only, is not suitable for industrialization and prepares in a large number, and cost is very high.
Summary of the invention
The object of the invention is to provide the novel preparation method of the diosgenin that a kind of suitable industrialization produces.
Diosgenin preparation method of the present invention can be selected from any in the following method.
Method one: with Chinese medicine Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, adds calcium oxide or the calcium hydroxide breast soaks, and places, and uses alcohol reflux again, and extracting liquid filtering reclaims ethanol, filter insolubles, drying under reduced pressure.Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, puts coldly, and suction filtration or centrifugal adds an amount of lime powder alcohol reflux hydrolyzate after the washing, and extracting solution adds decolorization and impurity removal by active carbon matter, diosgenin, recrystallization in the ethanol must the pure product of colourless needle crystal.
Described medicinal material at first must be used extraction using alcohol, and adds an amount of calcium oxide or calcium hydroxide.
Described hydrolyzate is used alcohol reflux after suction filtration, drying, and adds an amount of calcium oxide or calcium hydroxide, and extracting solution adds decolorization and impurity removal by active carbon matter.
The used acid of described acid hydrolysis is sulfuric acid or hydrochloric acid, and its concentration is 1mol/L-5mol/L.
Present method can also be: Ningpo Yam Rhizome 250-1000 weight part, adding 10-40 weight part calcium oxide breast soaks, placed 6-18 hour, with the alcohol reflux of 2-8 times of parts by volume (kg/L) 60-90% 2-4 time, each time is 2-4 hour, united extraction liquid, filter, reclaim ethanol, filter insolubles, with the insolubles drying under reduced pressure.Dry thing is used 2mol/L hydrochloric acid hydrolysis 3 hours, put cold, suction filtration or centrifugal adds 3-12 weight part lime powder after insolubles washes with water, with 85-95% 1-2 times of parts by volume of ethanol (kg/L) refluxing extraction hydrolyzate, extracting solution adds the gac 1-6 weight part decolouring removal of impurity, get diosgenin,, get the colourless needle crystal of diosgenin (Diosgenin) with 200-1000 parts by volume (kg/L) 85-95% ethyl alcohol recrystallization, yield is 1.2%, and content is 96.9%.
Method two:
With Chinese medicine Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, adds ordinary water and soaks, and discards soak solution, uses alcohol reflux, adds gac in extracting solution, and suction filtration reclaims ethanol, and suction filtration gets insolubles, drying.Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, and hydrolyzate suction filtration or centrifugal washes with water to neutrality, adds lime powder and stirring, drying, uses the alcohol reflux hydrolyzate, transfer pH value, use activated carbon decolorizing, suction filtration, reclaim ethanol, the dry diosgenin that gets gets the pure product of colourless needle crystal with ethyl alcohol recrystallization.
Present method also can be: with Chinese medicine Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, adds ordinary water and soaks, and discards soak solution, uses alcohol reflux, adds 1% gac in extracting solution, and suction filtration reclaims ethanol, and suction filtration gets insolubles, drying; Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, and hydrolyzate suction filtration or centrifugal washes with water to neutrality, adds an amount of lime powder and stirring, drying, uses the alcohol reflux hydrolyzate, transfer pH value, use activated carbon decolorizing, suction filtration reclaims ethanol, the dry diosgenin that gets is used ethyl alcohol recrystallization, gets colourless needle crystal.
Present method can also be: Ningpo Yam Rhizome 250-1000 weight part, add 8-12 times of parts by volume (kg/L) ordinary water soaking at room temperature 8-18 hour, discard immersion liquid,, use 4-8 times of parts by volume refluxing extraction of 70-90% ethanol 1-3 hour again with 4-10 times of parts by volume (kg/L) 85-95% alcohol reflux 2-4 hour, united extraction liquid, add 6-12 weight part gac in extracting solution, suction filtration reclaims ethanol, suction filtration gets insolubles, drying.Dry thing is used 1mol/L sulphuric acid hydrolysis 2-4 hour, the hydrolyzate suction filtration, wash with water to neutrality, add 20-60 weight part lime powder and stirring, drying, with 1-2 times of parts by volume of 85-95% ethanol (kg/L) refluxing extraction hydrolyzate, transfer pH value to 4-6, add medicinal carbon 1-3 weight part, decolouring, suction filtration reclaims ethanol, the dry diosgenin that gets, getting the colourless needle crystal of diosgenin (Diosgenin) yield with 85-95% ethanol 200-1000 parts by volume (kg/L) recrystallization is 1.4%, and content is 94.8%.
Method three:
With Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, adds 1% saccharifying enzyme or amylase, more than 24 hours, washes soak with ordinary water with the suitable quantity of water solution soaking again, uses alcohol reflux, reclaims ethanol extract, filters the insolubles drying.Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, and the suction filtration hydrolyzate washes with water to neutrality, drying adds calcium oxide or calcium hydroxide, stirs evenly, use alcohol reflux, suction filtration is transferred pH value, with activated carbon decolorizing, suction filtration reclaims ethanol, filter insolubles, the dry diosgenin crude product that gets is used ethyl alcohol recrystallization, gets the pure product of colourless needle crystal.
Present method also can be: with Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, adds 1% saccharifying enzyme or amylase, uses the suitable quantity of water solution soaking more than 24 hours, wash soak with ordinary water again, use alcohol reflux, reclaim ethanol extract, filter the insolubles drying; Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, and the suction filtration hydrolyzate washes with water to neutrality, drying, the calcium oxide or the calcium hydroxide of adding 2% stir evenly, with alcohol reflux 2-3 time, suction filtration, transfer pH value closely neutral, with the activated carbon decolorizing of 1-2%, suction filtration, reclaim ethanol, filter insolubles, the dry diosgenin crude product that gets is used ethyl alcohol recrystallization, gets colourless needle crystal.
Present method can also be: Ningpo Yam Rhizome 250-1000 weight part, the saccharifying enzyme that adds the 6-12 weight part, deionized water with 4-10 times of parts by volume (kg/L) soaked 12-36 hour, washed soak with ordinary water again, with 4-10 times of parts by volume (kg/L) 95% alcohol reflux 2-4 hour, the leaching extracting solution, use 4-10 times of parts by volume of 75-90% ethanol (kg/L) refluxing extraction 1-3 hour again, united extraction liquid reclaims ethanol extract, filter the insolubles drying.Dry thing is used 2mol/L hydrochloric acid hydrolysis 2-4 hour, and the suction filtration hydrolyzate washes with water to neutrality, drying, the calcium hydroxide of adding 10-30 weight part stirs evenly, with alcohol reflux 1-3 hour, suction filtration was transferred pH value 4-6, with 3-8 weight part activated carbon decolorizing, suction filtration, reclaim ethanol, filter insolubles, the dry diosgenin crude product that gets is with 85-95% ethanol 600-1000 parts by volume (kg/L) recrystallization, get the colourless needle crystal of diosgenin (Diosgenin), yield is 1.3%, and content is 96.3%.
Method four:
With Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, with the ethanolic soln refluxing extraction that contains calcium oxide or calcium hydroxide, filters, and transfers pH value, and decompression recycling ethanol filters dry leaching thing.With sulfuric acid or hydrochloric acid hydrolysis leaching thing, filtration or centrifugal washes with water to neutrality, and drying is used ethanol suction filtration hydrolyzate again, and suction filtration adds proper amount of active carbon, and agitation and filtration reclaims ethanol, and suction filtration is used ethyl alcohol recrystallization again, gets the pure product of colourless needle crystal.
Present method also can be: with Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, with the ethanolic soln refluxing extraction of the calcium oxide or the calcium hydroxide that contain 0.5-1.5%, filters, and transfers pH value to neutral, and decompression recycling ethanol filters dry leaching thing; With sulfuric acid or hydrochloric acid hydrolysis leaching thing, filtration or centrifugal washes with water to neutrality, and drying is used ethanol extracting hydrolyzate again, and suction filtration adds proper amount of active carbon, and agitation and filtration reclaims ethanol, and suction filtration is used ethyl alcohol recrystallization again, gets the pure product of colourless needle crystal;
Present method can also be: Ningpo Yam Rhizome 250-1000 weight part, add 40-80 weight part calcium hydroxide, with 4-10 times of parts by volume (kg/L) 80-95% ethanolic soln refluxing extraction 2-4 hour, the leaching extracting solution was used 4-10 times of parts by volume of 80-95% ethanol (kg/L) refluxing extraction 1-3 hour again, united extraction liquid, filter, transfer pH value, decompression recycling ethanol, filter dry leaching thing.With 2mol/L hydrochloric acid hydrolysis leaching thing, filter, wash with water to neutrality, drying uses 85-95% ethanol 600-1000 parts by volume (kg/L) to extract hydrolyzate, suction filtration again, filtrate adds 8-12 weight part gac, agitation and filtration reclaims ethanol, suction filtration, use 85-95% ethanol 600-1000 parts by volume (kg/L) recrystallization again, get the colourless needle crystal of diosgenin (Diosgenin), yield is 1.5%, and content is 96.3%.
Aforesaid method of the present invention all can be used for industrialization and prepare the monomer diosgenin in a large number, is the technology that a kind of cost is low, content is high, safe, low in the pollution of the environment; Diosgenin novel preparation method of the present invention is earlier medicinal material suitably to be handled the back with ethanol saponin(e to be extracted, suitably use acid hydrolysis behind the purifying, hydrolysate adds an amount of calcium oxide or calcium hydroxide, with ethanol extracting diosgenin, can get the pure product of diosgenin behind the recrystallization, content is more than 94%.Novel process has not only solved the problem (hydrolyzate can directly use ethanol extracting) of old technology with the 120# gasoline extraction, has solved the inflammable and explosive problem of 120# gasoline in preparation diosgenin process simultaneously.The consumption problems of too of acid when novel process has also solved acid hydrolysis, novel process per kilogram medicinal material hydrochloric acid content is 50ml, old technology per kilogram medicinal material hydrochloric acid content is 500ml, has reduced the pollution of acid to environment, has also reduced production cost simultaneously.
Diosgenin of the present invention is analyzed by high performance liquid chromatography and liquid-matter combined system.
1, high performance liquid phase (HPLC) analytical instrument: U.S. Agillent1100 type high performance liquid chromatograph (joining quaternary pump, diode array detector, automatic sampler, column oven, software is the multiple several automated processing systems of Agillent1100 type), condition: chromatographic column is Zorbax C
18(4.6cm * 150cm), sample size is 5ul to the reverse phase silica gel post, and moving phase is methyl alcohol: water=80: 20, flow velocity are 1.0ml/min, and the detection wavelength is 215nm.Analytical results: the diosgenin retention time is 15.385min, and is consistent with standard substance, and external standard method quantitatively is more than 94%.
2, liquid-matter coupling (LC/MSD) analytical instrument: U.S. Agillent liquid-matter combined instrument (joining quaternary pump, compensating unit pump, diode array detector, automatic sampler, column oven, software is Agillent1100 type several data treatment system).Condition: chromatographic column is ZOBAX EXTEND C
18Post, moving phase are acetonitrile: water (PH is 3.5)=80: 20.Flow velocity is 0.9ml/min, and the post post-compensation is urged ionization reagent ammonia soln (0.1ml/min), and the mass spectrum condition is negative ion mode (NEG) electron spray(ES) (API-ESI) scanning.It is in full accord to analyze compound and the standard substance diosgenin of having determined the present invention's extraction through liquid-matter coupling.
Aforesaid method of the present invention can be used for industrialization and prepare the monomer diosgenin in a large number, is the technology that a kind of cost is low, content is high, safe, low in the pollution of the environment.Before finishing, the present invention do not have report about this technology.
Embodiment 1
Ningpo Yam Rhizome 1kg adds 40g calcium oxide breast and soaks, and places 12 hours, and with the alcohol reflux twice of 6000ml80%, each time is 3 hours, and united extraction liquid filters, recovery ethanol, filter insolubles, with the insolubles drying under reduced pressure.Dry thing is used 2mol/L hydrochloric acid hydrolysis 3 hours, put cold, suction filtration or centrifugal, add the 10g lime powder after insolubles washes with water with 95% ethanol 1000ml refluxing extraction hydrolyzate, extracting solution adds the gac 5g decolouring removal of impurity, diosgenin, use the 800ml95% ethyl alcohol recrystallization, get the about 12g of the colourless needle crystal of diosgenin (Diosgenin), yield is 1.2%, and content is 96.9%.
Embodiment 2
Ningpo Yam Rhizome 1kg adds 10000ml ordinary water soaking at room temperature 12 hours, discards immersion liquid, uses 8000ml95% alcohol reflux 3 hours, use 80% ethanol 6000ml refluxing extraction 2 hours again, united extraction liquid adds 10g gac, suction filtration in extracting solution, reclaim ethanol, suction filtration gets insolubles, drying.Dry thing is used 1mol/L sulphuric acid hydrolysis 3 hours, the hydrolyzate suction filtration washes with water to neutrality, adds 40g lime powder and stirring, drying, with 95% ethanol 1000ml refluxing extraction hydrolyzate, transfer pH value to 5, add medicinal carbon 2g decolouring, suction filtration reclaims ethanol, the dry diosgenin that gets, get the about 14g of the colourless needle crystal of diosgenin (Diosgenin) with 95% ethanol 800ml recrystallization, yield is 1.4%, and content is 94.8%.
Embodiment 3
Ningpo Yam Rhizome 1kg, the saccharifying enzyme that adds 10g, deionized water with 8000ml soaked 24 hours, washed soak with ordinary water again, used 8000ml95% alcohol reflux 3 hours, the leaching extracting solution, use 85% ethanol 6000ml refluxing extraction 2 hours again, merge extracted twice liquid, reclaim ethanol extract, filter the insolubles drying.Dry thing is used 2mol/L hydrochloric acid hydrolysis 3 hours, and the suction filtration hydrolyzate washes with water to neutrality, drying, the calcium hydroxide of adding 20g stirs evenly, with alcohol reflux 2 hours, suction filtration, transfer pH value closely neutral, use the 5g activated carbon decolorizing, suction filtration reclaims ethanol, filter insolubles, the dry diosgenin crude product that gets is with 95% ethanol 800ml recrystallization, get the about 13g of the colourless needle crystal of diosgenin (Diosgenin) with 95% ethanol 800ml recrystallization, yield is 1.3%, and content is 96.3%.
Embodiment 4
Ningpo Yam Rhizome 1kg adds 60g calcium hydroxide, uses 8000ml85% ethanolic soln refluxing extraction 3 hours, the leaching extracting solution, use 85% ethanol 6000ml refluxing extraction 2 hours again, merge extracted twice liquid, filter, transfer pH value to neutral, decompression recycling ethanol filters dry leaching thing.With 2mol/L hydrochloric acid hydrolysis leaching thing, filter, wash with water to neutrality, drying is extracted hydrolyzate, suction filtration with 95% ethanol 1000ml again, filtrate adds the 10g gac, agitation and filtration reclaims ethanol, suction filtration, use 95% ethanol 800ml recrystallization again, get the about 15g of the colourless needle crystal of diosgenin (Diosgenin), yield is 1.5%, and content is 96.3%.
Claims (18)
1, a kind of preparation method of diosgenin is characterized in that this method is:
With Chinese medicine Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, adds calcium oxide or the calcium hydroxide breast soaks, and places, and uses alcohol reflux again, and extracting liquid filtering reclaims ethanol, filter insolubles, drying under reduced pressure; Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, puts coldly, and suction filtration or centrifugal adds an amount of lime powder alcohol reflux hydrolyzate after the washing, and extracting solution adds decolorization and impurity removal by active carbon matter, diosgenin, recrystallization in the ethanol must the pure product of colourless needle crystal.
2,, it is characterized in that medicinal material at first must use extraction using alcohol, and add an amount of calcium oxide or calcium hydroxide according to right 1 described method.
3, method according to claim 1 is characterized in that hydrolyzate uses alcohol reflux through suction filtration, after dry, and adds an amount of calcium oxide or calcium hydroxide that extracting solution adds decolorization and impurity removal by active carbon matter.
4, method according to claim 1 is characterized in that the used acid of acid hydrolysis is sulfuric acid or hydrochloric acid, and its concentration is 1mol/L-5mol/L.
5, the preparation method of a kind of diosgenin as claimed in claim 1 is characterized in that this method is:
Ningpo Yam Rhizome 250-1000 weight part adds 10-40 weight part calcium oxide breast and soaks, and places 6-18 hour, with the alcohol reflux of 2-8 times of parts by volume 60-80% 2-4 time, each time is 2-4 hour, and united extraction liquid filters, reclaim ethanol, filter insolubles, with the insolubles drying under reduced pressure; Dry thing is used 2mol/L hydrochloric acid hydrolysis 3 hours, put cold, suction filtration or centrifugal, after washing with water, insolubles adds 3-12 weight part lime powder, with 1-2 times of parts by volume refluxing extraction of 85-95% ethanol hydrolyzate, extracting solution adds the gac 1-6 weight part decolouring removal of impurity, gets diosgenin, with 200-1000 parts by volume 85-95% ethyl alcohol recrystallization, get the colourless needle crystal of diosgenin.
6, the preparation method of a kind of diosgenin as claimed in claim 5 is characterized in that this method is:
Ningpo Yam Rhizome 1000 weight parts add 40 weight part calcium oxide breasts and soak, and place 12 hours, with twice of the alcohol reflux of 6000 parts by volume 80%, each time is 3 hours, and united extraction liquid filters, reclaim ethanol, filter insolubles, with the insolubles drying under reduced pressure; Dry thing is used 2mol/L hydrochloric acid hydrolysis 3 hours, put cold, suction filtration or centrifugal, after washing with water, insolubles adds 10 weight part lime powders with 95% ethanol, 1000 parts by volume refluxing extraction hydrolyzates, extracting solution adds the gac 5 weight parts decolouring removal of impurity, get diosgenin, use the 800ml95% ethyl alcohol recrystallization, get the colourless needle crystal of diosgenin.
7, a kind of preparation method of diosgenin is characterized in that this method is:
With Chinese medicine Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, adds ordinary water and soaks, and discards soak solution, uses alcohol reflux, adds gac in extracting solution, and suction filtration reclaims ethanol, and suction filtration gets insolubles, drying; Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, and hydrolyzate suction filtration or centrifugal washes with water to neutrality, adds lime powder and stirring, drying, uses the alcohol reflux hydrolyzate, transfer pH value, use activated carbon decolorizing, suction filtration, reclaim ethanol, the dry diosgenin that gets gets the pure product of colourless needle crystal with ethyl alcohol recrystallization.
8, the preparation method of a kind of diosgenin as claimed in claim 7 is characterized in that this method is:
With Chinese medicine Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, adds ordinary water and soaks, and discards soak solution, uses alcohol reflux, adds 1% gac in extracting solution, and suction filtration reclaims ethanol, and suction filtration gets insolubles, drying; Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, and hydrolyzate suction filtration or centrifugal washes with water to neutrality, adds an amount of lime powder and stirring, drying, uses the alcohol reflux hydrolyzate, transfer pH value, use activated carbon decolorizing, suction filtration reclaims ethanol, the dry diosgenin that gets is used ethyl alcohol recrystallization, gets colourless needle crystal.
9, the preparation method of a kind of diosgenin as claimed in claim 7 is characterized in that this method is:
Present method can also be: Ningpo Yam Rhizome 250-1000 weight part, add 8-12 times of parts by volume ordinary water soaking at room temperature 8-18 hour, discard immersion liquid,, use 4-8 times of parts by volume refluxing extraction of 70-90% ethanol 1-3 hour again with 4-10 times of parts by volume 85-95% alcohol reflux 2-4 hour, united extraction liquid, add 6-12 weight part gac in extracting solution, suction filtration reclaims ethanol, suction filtration gets insolubles, drying; Dry thing is used 1mol/L sulphuric acid hydrolysis 2-4 hour, the hydrolyzate suction filtration washes with water to neutrality, adds 20-60 weight part lime powder and stirring, drying, with 1-2 times of parts by volume refluxing extraction of 85-95% ethanol hydrolyzate, transfer pH value to 4-6, add medicinal carbon 1-3 weight part, decolouring, suction filtration, reclaim ethanol, the dry diosgenin that gets gets the colourless needle crystal of diosgenin with 85-95% ethanol 200-1000 parts by volume recrystallization.
10, the preparation method of a kind of diosgenin as claimed in claim 9 is characterized in that this method is:
Ningpo Yam Rhizome 1kg adds 10000ml ordinary water soaking at room temperature 12 hours, discards immersion liquid, uses 8000ml95% alcohol reflux 3 hours, use 80% ethanol 6000ml refluxing extraction 2 hours again, united extraction liquid adds 10g gac, suction filtration in extracting solution, reclaim ethanol, suction filtration gets insolubles, drying; Dry thing is used 1mol/L sulphuric acid hydrolysis 3 hours, the hydrolyzate suction filtration, wash with water to neutrality, add 40g lime powder and stirring, drying, with 95% ethanol 1000ml refluxing extraction hydrolyzate, transfer pH value to 5, add medicinal carbon 2g decolouring, suction filtration, reclaim ethanol, the dry diosgenin that gets gets the colourless needle crystal of diosgenin with 95% ethanol 800ml recrystallization.
11, a kind of preparation method of diosgenin, it is characterized in that this method is: with Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, add 1% saccharifying enzyme or amylase, with the suitable quantity of water solution soaking more than 24 hours, wash soak with ordinary water again, use alcohol reflux, reclaim ethanol extract, filter the insolubles drying; Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, and the suction filtration hydrolyzate washes with water to neutrality, drying adds calcium oxide or calcium hydroxide, stirs evenly, use alcohol reflux, suction filtration is transferred pH value, with activated carbon decolorizing, suction filtration reclaims ethanol, filter insolubles, the dry diosgenin crude product that gets is used ethyl alcohol recrystallization, gets the pure product of colourless needle crystal.
12, the preparation method of a kind of diosgenin as claimed in claim 11 is characterized in that this method is:
With Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, adds 1% saccharifying enzyme or amylase, more than 24 hours, washes soak with ordinary water with the suitable quantity of water solution soaking again, uses alcohol reflux, reclaims ethanol extract, filters the insolubles drying; Dry thing is with sulfuric acid or hydrochloric acid hydrolysis, and the suction filtration hydrolyzate washes with water to neutrality, drying, the calcium oxide or the calcium hydroxide of adding 2% stir evenly, with alcohol reflux 2-3 time, suction filtration, transfer pH value closely neutral, with the activated carbon decolorizing of 1-2%, suction filtration, reclaim ethanol, filter insolubles, the dry diosgenin crude product that gets is used ethyl alcohol recrystallization, gets colourless needle crystal.
13, a kind of preparation method of diosgenin, it is characterized in that this method is: Ningpo Yam Rhizome 250-1000 weight part, add the saccharifying enzyme of 6-12 weight part, soaked 12-36 hour with the deionized water of 4-10 times of parts by volume, wash soak with ordinary water again, with 4-10 times of parts by volume 95% alcohol reflux 2-4 hour, the leaching extracting solution was used 4-10 times of parts by volume refluxing extraction of 75-90% ethanol 1-3 hour again, united extraction liquid, reclaim ethanol extract, filter the insolubles drying; Dry thing is used 2mol/L hydrochloric acid hydrolysis 2-4 hour, and the suction filtration hydrolyzate washes with water to neutrality, drying, the calcium hydroxide of adding 10-30 weight part stirs evenly, with alcohol reflux 1-3 hour, suction filtration was transferred pH value 4-6, with 3-8 weight part activated carbon decolorizing, suction filtration, reclaim ethanol, filter insolubles, the dry diosgenin crude product that gets with 85-95% ethanol 600-1000 parts by volume recrystallization, gets the colourless needle crystal of diosgenin.
14, the preparation method of a kind of diosgenin as claimed in claim 13 is characterized in that this method is:
Ningpo Yam Rhizome 1kg, the saccharifying enzyme that adds 10g, deionized water with 8000ml soaked 24 hours, washed soak with ordinary water again, used 8000ml95% alcohol reflux 3 hours, the leaching extracting solution, use 85% ethanol 6000ml refluxing extraction 2 hours again, merge extracted twice liquid, reclaim ethanol extract, filter the insolubles drying; Dry thing is used 2mol/L hydrochloric acid hydrolysis 3 hours, and the suction filtration hydrolyzate washes with water to neutrality, drying, the calcium hydroxide of adding 20g stirs evenly, with alcohol reflux 2 hours, suction filtration, transfer pH value closely neutral, use the 5g activated carbon decolorizing, suction filtration reclaims ethanol, filter insolubles, the dry diosgenin crude product that gets with 95% ethanol 800ml recrystallization, gets the colourless needle crystal of diosgenin with 95% ethanol 800ml recrystallization.
15, a kind of preparation method of diosgenin is characterized in that this method is: with Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, with the ethanolic soln refluxing extraction that contains calcium oxide or calcium hydroxide, filter, transfer pH value, decompression recycling ethanol, filter dry leaching thing; With sulfuric acid or hydrochloric acid hydrolysis leaching thing, filtration or centrifugal washes with water to neutrality, and drying is used ethanol suction filtration hydrolyzate again, and suction filtration adds proper amount of active carbon, and agitation and filtration reclaims ethanol, and suction filtration is used ethyl alcohol recrystallization again, gets the pure product of colourless needle crystal.
16, the preparation method of a kind of diosgenin as claimed in claim 15, it is characterized in that this method is: with Ningpo Yam Rhizome or other Dioscoreaceae plant is raw material, ethanolic soln refluxing extraction with calcium oxide that contains 0.5-1.5% or calcium hydroxide, filter, transfer pH value to neutral, decompression recycling ethanol filters dry leaching thing; With sulfuric acid or hydrochloric acid hydrolysis leaching thing, filtration or centrifugal washes with water to neutrality, and drying is used ethanol extracting hydrolyzate again, and suction filtration adds proper amount of active carbon, and agitation and filtration reclaims ethanol, and suction filtration is used ethyl alcohol recrystallization again, gets the pure product of colourless needle crystal;
17, the preparation method of a kind of diosgenin as claimed in claim 15 is characterized in that this method is:
Ningpo Yam Rhizome 250-1000 weight part, add 40-80 weight part calcium hydroxide, with 4-10 times of parts by volume 80-95% ethanolic soln refluxing extraction 2-4 hour, the leaching extracting solution was used 4-10 times of parts by volume refluxing extraction of 80-95% ethanol 1-3 hour again, united extraction liquid, filter, transfer pH value, decompression recycling ethanol, filter dry leaching thing; With 2mol/L hydrochloric acid hydrolysis leaching thing, filter, wash to neutrality drying with water, extract hydrolyzate with 85-95% ethanol 600-1000 parts by volume again, suction filtration, filtrate add 8-12 weight part gac, agitation and filtration, reclaim ethanol, suction filtration is used 85-95% ethanol 600-1000 parts by volume recrystallization again, gets the colourless needle crystal of diosgenin.
18, the preparation method of a kind of diosgenin as claimed in claim 17 is characterized in that this method is:
Ningpo Yam Rhizome 1kg adds 60g calcium hydroxide, uses 8000ml85% ethanolic soln refluxing extraction 3 hours, the leaching extracting solution, use 85% ethanol 6000ml refluxing extraction 2 hours again, merge extracted twice liquid, filter, transfer pH value to neutral, decompression recycling ethanol filters dry leaching thing; With 2mol/L hydrochloric acid hydrolysis leaching thing, filter, wash to neutrality drying with water, extract hydrolyzate with 95% ethanol 1000ml again, suction filtration, filtrate adds 10g gac, agitation and filtration, reclaim ethanol, suction filtration is used 95% ethanol 800ml recrystallization again, gets the colourless needle crystal of diosgenin.
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| CNB021539979A CN1188425C (en) | 2002-12-09 | 2002-12-09 | Novel process for preparing diosgenin |
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| CNB021539979A CN1188425C (en) | 2002-12-09 | 2002-12-09 | Novel process for preparing diosgenin |
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| CN1418888A CN1418888A (en) | 2003-05-21 |
| CN1188425C true CN1188425C (en) | 2005-02-09 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100451097C (en) * | 2006-12-07 | 2009-01-14 | 云南省微生物研究所 | Aspergillus niger |
| CN100572553C (en) * | 2006-09-14 | 2009-12-23 | 中国科学院武汉植物园 | Method with preparing dioscin with dioscin penicillium notatum |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460419C (en) * | 2005-12-08 | 2009-02-11 | 王喜军 | New cleanproduction process for extracting saponin from dioscorea zingiberensis |
| CN100451029C (en) * | 2006-01-18 | 2009-01-14 | 中南大学 | Technique for extracting yam saponin, amylocellulose, and yellow pigment by separating yam |
| CN102020693B (en) * | 2009-09-18 | 2014-04-23 | 张万举 | Clean production method of yam saponin |
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2002
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100572553C (en) * | 2006-09-14 | 2009-12-23 | 中国科学院武汉植物园 | Method with preparing dioscin with dioscin penicillium notatum |
| CN100451097C (en) * | 2006-12-07 | 2009-01-14 | 云南省微生物研究所 | Aspergillus niger |
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| Publication number | Publication date |
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| CN1418888A (en) | 2003-05-21 |
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