CN103965283A - Separation method of high-purity diosgenin - Google Patents
Separation method of high-purity diosgenin Download PDFInfo
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Abstract
The invention discloses a separation method of high-purity diosgenin and belongs to the technical field of pharmaceutical raw material production. The method is characterized by comprising the steps as follows: adopting the ultrasonic assisted sodium lauryl sulfate extraction technology and utilizing the solubilization action of sodium lauryl sulfate to extract dioscin from dioscorea zingiberensis; adopting the flocculation technology to separate the dioscin from the extracting solution to obtain crude dioscin; obtaining crude diosgenin through hydrolyzation, filtration, water scrubbing, drying, reflux extraction and cooling crystallization of the crude dioscin; obtaining precision processed diosgenin through batch splitting precision processing of the crude diosgenin in warm water. The separation method has the benefits that the precision processing of the method overcomes the deficiency of difficulty in diosgenin separation and purification, and the degree of purity of the precision processed diosgenin is above 98.5%.
Description
Technical field
The invention belongs to medicine material production technical field, be specifically related to a kind of separation method of high purity diosgenin.
Background technology
Around pollution problem and the Cost Problems of producing diosgenin, people have carried out a large amount of research work, have obtained some achievements.Before 2003, China generally adopts pre-fermentation-acidolysis process to produce diosgenin, and this technique is compared with classical acid direct hydrolysis technique, and the productive rate of diosgenin increases, but basic suitable with traditional technology by acid amount, therefore pollute with traditional technology basic identical.In research process, it is found that and cause the acid of diosgenin production process greatly, COD value in waste water, the root that BOD value is high are: the dioscin in Rhizome of Peltate Yam is in being hydrolyzed to diosgenin, and the starch in Rhizome of Peltate Yam, Mierocrystalline cellulose are hydrolyzed to carbohydrate (monose, disaccharides, trisaccharide and polysaccharide).In order to reduce sour consumption, Li Xiang etc. are analyzing on the basis of the distributions such as starch in Rhizome of Peltate Yam, Mierocrystalline cellulose, xylogen, dioscin and character, adopt wet grinding mill sizing process, starch, Mierocrystalline cellulose, xylogen, dioscin are separated, reduce to a certain extent sour consumption, reduce COD value, BOD value, colourity of waste water etc., reclaimed the starch in Rhizome of Peltate Yam, Mierocrystalline cellulose.2003 under the support of national environmental protection project, Environmental Protection Agency of Shaanxi Province is the suitability for industrialized production for diosgenin by this technology, build up to be separated into main diosgenin cleaner production model enterprise-adret Jinchuan Feng Xing chemical industry limited liability company in Shangluo Prefecture, from running condition, the consumption of this technology acid, coal, gasoline is respectively 10%～15%, 25%～50% and 30%～35% of traditional technology, wastewater discharge is 90% of traditional technology, the COD value of waste water, BOD value are traditional technology 10%, 20%～25% starch in recyclable Rhizome of Peltate Yam.But because this operational path is longer, facility investment is large, and cost is high, and because the starch reclaiming contains silt etc., limit the application of reclaiming starch.
In order to reduce the production cost of diosgenin, Linli Qiu etc. are on the basis of traditional alcohol extraction technology, ultrasonic technology is introduced in the research of dioscin extraction, save widely the extraction time of dioscin, improve the extraction efficiency of dioscin, increased the yield of diosgenin.But because ethanol loss in extraction process is larger, poor stability etc. have restricted applying of this technology.Liu Shuxing etc. are the research for dioscin extraction by tensio-active agent, found that, in the situation that diosgenin yield is constant, tensio-active agent add the remarkable volume fraction that reduces ethanol.
Process for producing diosgenin taking Surfactant SDS as extraction agent, taking flocculation technique as core has reduced the consumption of acid in diosgenin production process effectively, has reduced pollution, has reduced cost.But often exist diosgenin crystal by the phenomenon of lauryl alcohol (oily matter) parcel, this phenomenon causes diosgenin separation difficulty, and the diosgenin product obtaining often purity is not high.
Summary of the invention
In order to overcome the defect of above-mentioned prior art existence, the object of the present invention is to provide a kind of separation method of high purity diosgenin, the method is simple to operate, environmental friendliness, can effectively solve the problem of diosgenin separation and purification difficulty.
The present invention is achieved through the following technical solutions:
A separation method for high purity diosgenin, comprises roughing out and precision processing two steps, and described roughing out concrete operation step is:
1) Rhizome of Peltate Yam of pulverizing is immersed in sodium dodecyl sulfate solution, after lixiviate 2～4h, ultrasonic extraction, then centrifugal, obtain dioscin extraction liquid and filter residue;
2) filter residue is continued use sodium dodecyl sulfate solution ultrasonic extraction, then centrifugal, the dioscin extraction liquid merging that the centrifugal extraction liquid obtaining and step 1) are obtained, obtains the total extraction liquid of dioscin;
3) press the total extraction liquid of dioscin: the flocculating agent A aqueous solution=100:(4～10) volume ratio, be 0.8%～1.2% flocculating agent A aqueous solution to adding massfraction in the total extraction liquid of dioscin, after Micelle formation, stop stirring, leave standstill after 5～20min, filter, obtain filter residue 1 and filtrate 1, then to add massfraction to filtrate 1 be 2%～6% the flocculating agent B aqueous solution, at 40～50 DEG C, leave standstill after 1～3h, centrifugal, obtain filtrate 2 and filter residue 2, merge filter residue 1 and filter residue 2, obtain dioscin crude product;
Wherein, described flocculating agent A, in massfraction, comprises 95%～100% chitosan, 0%～5% xanthan gum; Described flocculating agent B, in massfraction, comprises 55～60% bar-shaped wilkinite, 40～45% bentonite clarifying agent;
4) in the ratio of every g dioscin crude product interpolation 2.5～3mL sulfuric acid, dioscin crude product is joined in the sulfuric acid that concentration is 1.3～1.8mol/L, at 105～108 DEG C, after hydrolysis 4～6h, will be cooling hydrolyzed solution and neutralization after filter, it is dry after neutral that washing filter residue to effluent liquid is, then by dry filter residue after refluxing extraction, cooling, crystallization, obtain diosgenin crude product;
Described precision processing concrete operation step is:
(1) be in the water of 60～90 DEG C to splashing into temperature in diosgenin crude product, stir, then centrifugal, reject upper water and oily matter, obtain diosgenin;
(2) by after diosgenin repeating step (1) operation of purifying 2～4 times, the diosgenin with moisture is dried, obtains high purity diosgenin.
The usage ratio that in precision processing operation, diosgenin crude product and the temperature splashing into are the water of 60～90 DEG C is 1g:(5～10) mL.
In precision processing operation, described centrifugal of step (1) is under the condition of 2500～3000r/min, centrifugal 5～10min.
Dry in precision processing operation is to carry out at 60～70 DEG C.
Step 1) in roughing out operation is according to 1g:(8～10) ratio of mL, immerses the Rhizome of Peltate Yam after pulverizing in sodium dodecyl sulfate solution.
Ultrasonic extraction described in roughing out operation is to be under 25.8KHz in ultrasonic frequency, extraction 25～30min.
Centrifugal described in roughing out operation is under the condition of 2000～4000r/min, centrifugal 8～15min.
The concentration of the sodium dodecyl sulfate solution described in roughing out operation is 25.8 × 10
-3mol/L.
Neutralization in roughing out operation described in step 4) is under agitation condition, and adding massfraction is 18%～22% Na
2cO
3solution; Described drying temperature is 50～60 DEG C.
Refluxing extraction in roughing out operation described in step 4) is specially: by after dry filter residue filter paper parcel, be placed in apparatus,Soxhlet's, add the sherwood oil of container 4/5 volume, with the speed refluxing extraction 4～6h of 4～6 per second.
Compared with prior art, the present invention has following useful technique effect:
The present invention adopts ultrasonic wave to assist sodium lauryl sulphate abstraction technique, utilize the solublization of sodium lauryl sulphate, first dioscin is extracted from Rhizome of Peltate Yam, adopt again flocculation technique that dioscin is separated from extraction liquid, obtain dioscin crude product, dioscin crude product through hydrolysis, filter, washing, dry, refluxing extraction and crystallisation by cooling, obtain diosgenin crude product.Then carry out precision processing to adding in warm water in diosgenin crude product, obtain the diosgenin after precision processing.
Advantage of the present invention is mainly reflected in:
1, the present invention, taking Surfactant SDS as extraction agent, has avoided the use (organic solvent of the prior art, as alcohol extraction dioscin) of organic solvent, has reduced cost, has reduced pollution, has increased the security of operating process;
2, the present invention substitutes traditional hot beneficiation technologies with flocculation technique, prevent in dioscin enrichment (concentrating) process, (sodium lauryl sulphate, dioscin are tensio-active agent to cause the loss of dioscin because bubbling, therefore very easily bubble in the time of vacuum concentration), reduce the energy consumption in dioscin enrichment process, ensure the cleaner production of diosgenin under low cost, proved that through test of many times flocculence occupies very large advantage than traditional hot concentration method on cost;
3, the present invention adopts homemade flocculating agent A and flocculating agent B, there is good flocculating effect, flocculating agent A composition comprises chitosan and xanthan gum, in chitosan molecule, contain a certain amount of amido, for cationic flocculant, in extraction liquid, with the dioscin micelle generation static neutralizing effect of electronegative property, impel the flocculation of dioscin micelle; Xanthan gum adds in dioscin extraction liquid, can form and surpass in conjunction with banded spiral interpolymer, forms the reticulated structure of fragile similar glue; In the time that the concentration of xanthan gum is higher, this reticulated structure can be supported the form of solid particulate in extraction liquid, drop and bubble, demonstrates very strong stable emulsifying effect and higher suspension ability.In the time that the concentration of xanthan gum is lower, this reticulated structure can be caught the flocs unit that dioscin micelle in extraction liquid and chitosan form, and accelerates the flocculation of dioscin;
Flocculating agent B comprises bar-shaped wilkinite finings and bentonite clarifying agent, wilkinite is a kind of material of vesicular structure, there is very strong adsorption, on the one hand, can do not adsorbed the dioscin of (flocculation) by chitosan (xanthan gum) by sorption extraction liquid, on the other hand, because wilkinite proportion is larger, can accelerate the flocculation of dioscin.Bar-shaped wilkinite and bentonite clarifying agent are to distinguish to some extent in nature, and bar-shaped wilkinite specific surface area is large, and high adsorption capacity, in dioscin flocculation process, can adsorb not by the dioscin of chitosan, xanthan gum flocculation.Bentonite clarifying agent specific surface area is relatively little, adsorptive power relatively a little less than, but density is relatively large, mixes use with bar-shaped wilkinite, can accelerate the separation of dioscin in extraction liquid.
4,, compared with traditional technology, while having reduced dioscin hydrolysis, the consumption of acid, has reduced COD value in waste water, BOD value, ammonia nitrogen, solid content, thereby has saved cost for wastewater treatment.
5, precision processing of the present invention operates to have overcome and adopts the diosgenin clean preparation method gained diosgenin taking Surfactant SDS as extraction agent, taking flocculation technique as core to be wrapped up by lauryl alcohol (oily matter), the shortcoming of diosgenin separation and purification difficulty, the purity of the diosgenin after precision processing can reach more than 98.5%.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Lauryl alcohol is white or colourless oil liquid, tool flowery odour, 24 DEG C of fusing points, boiling point 255-259 DEG C, relative density 0.8201g/cm
3(24 DEG C), 126.7 DEG C of flash-points, water insoluble, glycerine, is dissolved in propylene glycol, ethanol, benzene, chloroform, ether.
Diosgenin is white or micro-yellow crystalline powder, 195 DEG C of fusing points, 527.1 DEG C of boiling points, relative density 1.13g/cm
3(25 DEG C), 272.6 DEG C of flash-points, water insoluble, be soluble in the organic solvents such as gasoline, ethanol, chloroform.
Can be found out by above-mentioned character, lauryl alcohol is very similar to the chemical property of diosgenin, adopts chemical method separating difficulty larger.The boiling point of lauryl alcohol and diosgenin differs greatly, and lauryl alcohol is 255-259 DEG C, and diosgenin is 527.1 DEG C, can adopt distillation under vacuum to be separated, but vacuum distillation equipment investment is large, certainly will cause the production cost of diosgenin to rise.Fusing point, the Relatively density contrast of lauryl alcohol and diosgenin are also larger, and the fusing point of lauryl alcohol is 24 DEG C, and relative density is 0.8201g/cm
3(24 DEG C), and the fusing point of diosgenin is 195 DEG C, relative density is 1.13g/cm
3(25 DEG C).If wrap up the oily matter of the lauryl alcohol of diosgenin by hot-water cure, because lauryl alcohol fusing point is low, relative density is little, therefore be suspended on the water surface, diosgenin fusing point is high, and relative density is large, water insoluble again, therefore in underwater, can simply, effectively separate the oily matter of diosgenin crystal and lauryl alcohol by the inventive method.
Embodiment 1
A flocculation extracting method for diosgenin, comprises roughing out and precision processing step:
Roughing out:
1) first getting 100g granularity is 80 object Rhizome of Peltate Yam, and adding 1000mL concentration is 25.8 × 10
-3in the sodium dodecyl sulfate solution of mol/L, at soaking at room temperature 2h, be then under 25.8KHz in ultrasonic frequency, ultrasonic extraction 30min, centrifugation, obtains dioscin extraction liquid 1 and Rhizome of Peltate Yam filter residue; By the solid-liquid ratio of Rhizome of Peltate Yam filter residue: sodium lauryl sulphate=1g:8mL, Rhizome of Peltate Yam filter residue is joined in dodecyl sulphate solution, under identical ultrasound condition, ultrasonic extraction, centrifugation, obtains extraction liquid 2 and filter residue; And then by the solid-liquid ratio of filter residue: sodium lauryl sulphate=1g:5mL, filter residue is added in sodium lauryl sulphate, ultrasonic extraction under the same terms, then centrifugal collection extraction liquid 3, then merges extraction liquid 1, extraction liquid 2 and extraction liquid 3 to obtain the total extraction liquid of dioscin.
2) be the ratio of 0.8% the self-control flocculating agent A aqueous solution according to adding 5mL massfraction in 100mL extraction liquid, dropwise add the flocculating agent A aqueous solution to rapid stirring limit, limit in the total extraction liquid of dioscin, after Micelle formation, stop stirring, leave standstill after 10min, the most of sinking of micelle, few part floating, middle layer clarification bright (now the ζ of system approximates 0), filter, obtain filter residue 1 and filtrate, give again that to add while stirring massfraction in filtrate be 5% the self-control flocculating agent B aqueous solution through immersion treatment, after gel group is completed into, stop stirring, at 40 DEG C, leave standstill 1h, centrifugation 10min under 3000rpm, obtain filter residue 2, merge filter residue 1 and filter residue 2, obtain dioscin crude product,
Wherein, described flocculating agent A, in massfraction, comprises 95% chitosan, 5% xanthan gum; Described flocculating agent B, in massfraction, comprises 60% bar-shaped wilkinite finings (the special finings of grape wine), 40% fruit juice clarifier (bentonite clarifying agent).
3) according to the ratio of dioscin crude product: sulfuric acid=1g:2.5mL, give the sulfuric acid that adds 1.5mol/L in dioscin crude product, at 108 DEG C, be hydrolyzed 4h, cooling hydrolyzed solution, to room temperature, under stirring state, slowly adds 20% Na
2cO
3solution neutralization, filters, water repeatedly lotion filter residue to without SO
4 2-, at 50 DEG C, dry filter residue is to constant weight.
4) with filter paper, the filter residue of dry gained is wrapped, be placed in the soxhlet's extractor of 100mL, add the sherwood oil of about 80mL, with the speed backflow 4h of 4/s, after recovery part sherwood oil, crystallisation by cooling, obtains diosgenin crude product;
Precision processing:
(1) getting 1g diosgenin crude product, is the hot water of 90 DEG C to dropwise adding 10mL temperature in diosgenin crude product, after having oily matter to occur on the water surface, and centrifugal 10min under 3000r/min, reject upper water and oily matter, obtain diosgenin;
(2) operation 2 times of repeating step (1), obtains the diosgenin with moisture, then at 60 DEG C, is dried to constant weight, obtains the Powdered diosgenin of white, and purity is 98.9%.
Embodiment 2
A flocculation extracting method for diosgenin, comprises the following steps:
Roughing out:
1) first getting 100g granularity is 80 object Rhizome of Peltate Yam, and adding 800mL concentration is 25.8 × 10
-3in the sodium dodecyl sulfate solution of mol/L, at room temperature soaking 3h, is under 25.8KHz in ultrasonic frequency, ultrasonic extraction 30min, and centrifugation, obtains dioscin extraction liquid 1 and Rhizome of Peltate Yam filter residue; By the solid-liquid ratio of Rhizome of Peltate Yam filter residue: sodium lauryl sulphate=1g:10mL, Rhizome of Peltate Yam filter residue is joined in dodecyl sulphate solution, under identical ultrasound condition, ultrasonic extraction, centrifugation, obtains extraction liquid 2 and filter residue; And then by the solid-liquid ratio of filter residue: sodium lauryl sulphate=1g:7mL, filter residue is added in sodium lauryl sulphate, ultrasonic extraction under the same terms, then centrifugal collection extraction liquid 3, then merges extraction liquid 1, extraction liquid 2 and extraction liquid 3 to obtain the total extraction liquid of dioscin
2) be the ratio of 1% self-control flocculating agent A according to adding 4mL massfraction in 100mL extraction liquid, dropwise add the flocculating agent A aqueous solution to rapid stirring limit, limit in the total extraction liquid of dioscin, after Micelle formation, stop stirring, leave standstill after 20min, the most of sinking of micelle, few part floating, middle layer clarification bright (now the ζ of system approximates 0), filter, obtain filter residue 1 and filtrate, give again that to add while stirring massfraction in filtrate be 4% the flocculating agent B aqueous solution, at 40 DEG C, leave standstill after 3h, centrifugation under 3000rpm/10min, obtain filtrate and filter residue 2, merge filter residue 1 and filter residue 2, obtain dioscin crude product,
Wherein, described flocculating agent A, in massfraction, comprises 97% chitosan, 3% xanthan gum; Described flocculating agent B, in massfraction, comprises 55% bar-shaped wilkinite finings (the special finings of grape wine), 45% fruit juice clarifier (bentonite clarifying agent).
3) according to the ratio of dioscin crude product: sulfuric acid=1g:3mL, give the sulfuric acid that adds 1.3mol/L in dioscin crude product, at 105 DEG C, be hydrolyzed 4h, cooling hydrolyzed solution, to room temperature, under stirring state, slowly adds 18% Na
2cO
3solution neutralization, filters, water repeatedly lotion filter residue to without SO
4 2-, at 55 DEG C, dry filter residue is to constant weight.
4) with filter paper, the filter residue of dry gained is wrapped, be placed in the soxhlet's extractor of 100mL, add the sherwood oil of about 80mL, with the speed backflow 5h of 5/s, after recovery part sherwood oil, crystallisation by cooling, obtains diosgenin crude product;
Precision processing
(1) getting 1g diosgenin crude product, is the hot water of 70 DEG C to dropwise adding 8mL temperature in diosgenin crude product, after having oily matter to occur on the water surface, and centrifugal 8min under 3000r/min, reject upper water and oily matter, obtain diosgenin;
(2) operation 3 times of repeating step (1), obtains the diosgenin with moisture, then at 70 DEG C, is dried to constant weight, obtains the Powdered diosgenin of white, and purity is 99.3%.
Embodiment 3
A flocculation extracting method for diosgenin, comprises the following steps:
Roughing out:
1) first getting 100g granularity is 100 object Rhizome of Peltate Yam, and adding 900mL concentration is 25.8 × 10
-3in the sodium dodecyl sulfate solution of mol/L, at room temperature soaking 4h, is under 25.8KHz in ultrasonic frequency, ultrasonic extraction 30min, and centrifugation obtains dioscin extraction liquid 1 and Rhizome of Peltate Yam filter residue; By the solid-liquid ratio of Rhizome of Peltate Yam filter residue: sodium lauryl sulphate=1g:9mL, Rhizome of Peltate Yam filter residue is joined in dodecyl sulphate solution, under identical ultrasound condition, ultrasonic extraction, centrifugation, obtains extraction liquid 2 and filter residue; And then by the solid-liquid ratio of filter residue: sodium lauryl sulphate=1g:6mL, filter residue is added in sodium lauryl sulphate, ultrasonic extraction under the same terms, then centrifugal collection extraction liquid 3, then merges extraction liquid 1, extraction liquid 2 and extraction liquid 3 to obtain the total extraction liquid of dioscin.
2) be the ratio of 1.2% the self-control flocculating agent A aqueous solution according to adding 6mL massfraction in 100mL extraction liquid, dropwise add the flocculating agent A aqueous solution to rapid stirring limit, limit in the total extraction liquid of dioscin, after Micelle formation, stop stirring, leave standstill after 15min, the most of sinking of micelle, few part floating, middle layer clarification bright (now the ζ of system approximates 0), filter, obtain filter residue 1 and filtrate, give again that to add while stirring massfraction in filtrate be 5% the self-control flocculating agent B aqueous solution through immersion treatment, at 50 DEG C, leave standstill after 1h, centrifugation under 3000rpm/10min, obtain filtrate and filter residue 2, merge filter residue 1 and filter residue 2, obtain dioscin crude product
Wherein, described flocculating agent A is chitosan; Described flocculating agent B, in massfraction, comprises 58% bar-shaped wilkinite finings (the special finings of grape wine), 42% fruit juice clarifier (bentonite clarifying agent).
3) according to the ratio of dioscin crude product: sulfuric acid=1g:2.8mL, give the sulfuric acid that adds 1.8mol/L in dioscin crude product, at 108 DEG C, be hydrolyzed 6h, cooling hydrolyzed solution, to room temperature, under stirring state, slowly adds 22% Na
2cO
3solution neutralization, filters, water repeatedly lotion filter residue to without SO
4 2-, at 60 DEG C, dry filter residue is to constant weight.
4) with filter paper, the filter residue of dry gained is wrapped, be placed in the soxhlet's extractor of 100mL, add the sherwood oil of about 80mL, with the speed backflow 4h of 6/s, after recovery part sherwood oil, crystallisation by cooling, obtains diosgenin crude product;
Precision processing:
(1) getting 1g diosgenin crude product, is the hot water of 80 DEG C to dropwise adding 5mL temperature in diosgenin crude product, after having oily matter to occur on the water surface, and centrifugal 5min under 3000r/min, reject upper water and oily matter, obtain diosgenin;
(2) operation 2 times of repeating step (1), obtains the diosgenin with moisture, then at 60 DEG C, is dried to constant weight, obtains the Powdered diosgenin of white, and purity is 99.1%.
Embodiment 4
A flocculation extracting method for diosgenin, comprises the following steps:
Roughing out:
1) first getting 100g granularity is 80～100 object Rhizome of Peltate Yam, and adding 1000mL concentration is 25.8 × 10
-3in the sodium dodecyl sulfate solution of mol/L, soaking at room temperature 3h, is under 25.8KHz in ultrasonic frequency, ultrasonic extraction 30min, and centrifugation obtains dioscin extraction liquid 1 and Rhizome of Peltate Yam filter residue; By the solid-liquid ratio of Rhizome of Peltate Yam filter residue: sodium lauryl sulphate=1g:8mL, Rhizome of Peltate Yam filter residue is joined in dodecyl sulphate solution, under identical ultrasound condition, ultrasonic extraction, centrifugation, obtains extraction liquid 2 and filter residue; And then by the solid-liquid ratio of filter residue: sodium lauryl sulphate=1g:5mL, filter residue is added in sodium lauryl sulphate, ultrasonic extraction under the same terms, then centrifugal collection extraction liquid 3, then merges extraction liquid 1,2,3 to obtain the total extraction liquid of dioscin.
2) be the ratio of 1% the self-control flocculating agent A aqueous solution according to adding 10mL massfraction in 100mL extraction liquid, dropwise add the flocculating agent A aqueous solution to rapid stirring limit, limit in the total extraction liquid of dioscin, after Micelle formation, stop stirring, leave standstill after 5min, the most of sinking of micelle, few part floating, middle layer clarification bright (now the ζ of system approximates 0), filter, obtain filter residue 1 and filtrate, give again that to add while stirring massfraction in filtrate be 4% the flocculating agent B aqueous solution through immersion treatment, at 45 DEG C, leave standstill after 2h, centrifugation under 3000rpm/10min, obtain filtrate and filter residue 2, merge and filter residue 2, obtain dioscin crude product,
Wherein, described flocculating agent A, in massfraction, comprises 96% chitosan, 4% xanthan gum; Described flocculating agent B, in massfraction, comprises 60% bar-shaped wilkinite finings (the special finings of grape wine), 40% fruit juice clarifier (bentonite clarifying agent).
3) according to the ratio of dioscin crude product: sulfuric acid=1g:2.8mL, give the sulfuric acid that adds 1.5mol/L in dioscin crude product, at 107 DEG C, be hydrolyzed 6h, cooling hydrolyzed solution, to room temperature, under stirring state, slowly adds 20% Na
2cO
3solution neutralization, filters, water repeatedly lotion filter residue to without SO
4 2-, at 55 DEG C, dry filter residue is to constant weight.
4) with filter paper, the filter residue of dry gained is wrapped, be placed in the soxhlet's extractor of 100mL, add the sherwood oil of about 80mL, with the speed backflow 4h of 5/s, after recovery part sherwood oil, crystallisation by cooling, obtains diosgenin crude product;
Precision processing:
(1) getting 1g diosgenin crude product, is the hot water of 60 DEG C to dropwise adding 10mL temperature in diosgenin crude product, after having oily matter to occur on the water surface, and centrifugal 8min under 2500r/min, reject upper water and oily matter, obtain diosgenin;
(2) operation 4 times of repeating step (1), obtains the diosgenin with moisture, then at 70 DEG C, is dried to constant weight, obtains the Powdered diosgenin of white, and purity is 98.5%.
In sum, the diosgenin production method of the present invention taking sodium lauryl sulphate as extraction agent, taking flocculation technique as core reduced the consumption of acid in diosgenin production process effectively, reduced pollution, reduced cost.Meanwhile, precision processing operation efficiently solves the phenomenon that diosgenin crystal is wrapped up by lauryl alcohol, and the present invention can be separated diosgenin, lauryl alcohol, simple, separates and obtains highly purified diosgenin.
Claims (10)
1. a separation method for high purity diosgenin, is characterized in that, comprises roughing out and precision processing two steps, and described roughing out concrete operation step is:
1) Rhizome of Peltate Yam of pulverizing is immersed in sodium dodecyl sulfate solution, after lixiviate 2～4h, ultrasonic extraction, then centrifugal, obtain dioscin extraction liquid and filter residue;
2) filter residue is continued use sodium dodecyl sulfate solution ultrasonic extraction, then centrifugal, the dioscin extraction liquid merging that the centrifugal extraction liquid obtaining and step 1) are obtained, obtains the total extraction liquid of dioscin;
3) press 100:(4～10) volume ratio, be 0.8%～1.2% flocculating agent A aqueous solution to adding massfraction in the total extraction liquid of dioscin, after Micelle formation, stop stirring, leave standstill after 5～20min, filter, obtain filter residue 1 and filtrate 1, then to add massfraction to filtrate 1 be 2%～6% the flocculating agent B aqueous solution, at 40～50 DEG C, leave standstill after 1～3h, centrifugal, obtain filtrate 2 and filter residue 2, merge filter residue 1 and filter residue 2, obtain dioscin crude product;
Wherein, described flocculating agent A, in massfraction, comprises 95%～100% chitosan, 0%～5% xanthan gum; Described flocculating agent B, in massfraction, comprises 55～60% bar-shaped wilkinite, 40～45% bentonite clarifying agent;
4) in the ratio of every g dioscin crude product interpolation 2.5～3mL sulfuric acid, dioscin crude product is joined in the sulfuric acid that concentration is 1.3～1.8mol/L, at 105～108 DEG C, after hydrolysis 4～6h, will be cooling hydrolyzed solution and neutralization after filter, it is dry after neutral that washing filter residue to effluent liquid is, then by dry filter residue after refluxing extraction, cooling, crystallization, obtain diosgenin crude product;
Described precision processing concrete operation step is:
(1) be in the water of 60～90 DEG C to splashing into temperature in diosgenin crude product, stir, then centrifugal, reject upper water and oily matter, obtain diosgenin;
(2) by after diosgenin repeating step (1) operation of purifying 2～4 times, the diosgenin with moisture is dried, obtains high purity diosgenin.
2. the separation method of a kind of high purity diosgenin according to claim 1, is characterized in that, the usage ratio that in precision processing operation, diosgenin crude product and the temperature splashing into are the water of 60～90 DEG C is 1g:(5～10) mL.
3. the separation method of a kind of high purity diosgenin according to claim 1, is characterized in that, in precision processing operation, described centrifugal of step (1) is under the condition of 2500～3000r/min, centrifugal 5～10min.
4. the separation method of a kind of high purity diosgenin according to claim 1, is characterized in that, dry in precision processing operation is to carry out at 60～70 DEG C.
5. according to the separation method of a kind of high purity diosgenin described in any one in claim 1～4, it is characterized in that, step 1) in roughing out operation is according to 1g:(8～10) ratio of mL, immerses the Rhizome of Peltate Yam after pulverizing in sodium dodecyl sulfate solution.
6. according to the separation method of a kind of high purity diosgenin described in any one in claim 1～4, it is characterized in that, the ultrasonic extraction described in roughing out operation is to be under 25.8KHz in ultrasonic frequency, extraction 25～30min.
7. according to the separation method of a kind of high purity diosgenin described in any one in claim 1～4, it is characterized in that, centrifugal described in roughing out operation is under the condition of 2000～4000r/min, centrifugal 8～15min.
8. according to the separation method of a kind of high purity diosgenin described in any one in claim 1～4, it is characterized in that, the concentration of the sodium dodecyl sulfate solution described in roughing out operation is 25.8 × 10
-3mol/L.
9. according to the separation method of a kind of high purity diosgenin described in any one in claim 1～4, it is characterized in that, the neutralization in roughing out operation described in step 4) is under agitation condition, and adding massfraction is 18%～22% Na
2cO
3solution; Described drying temperature is 50～60 DEG C.
10. according to the separation method of a kind of high purity diosgenin described in any one in claim 1～4, it is characterized in that, refluxing extraction in roughing out operation described in step 4) is specially: by after dry filter residue filter paper parcel, be placed in apparatus,Soxhlet's, add the sherwood oil of container 4/5 volume, with the speed refluxing extraction 4～6h of 4～6 per second.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774240A (en) * | 2015-04-30 | 2015-07-15 | 陕西科技大学 | Method for extracting diosgenin through dioscin hydrolysis |
| CN105534946A (en) * | 2016-01-11 | 2016-05-04 | 陕西科技大学 | Preparation method of traditional Chinese medicine capsules |
| CN107827949A (en) * | 2017-11-07 | 2018-03-23 | 西南民族大学 | A kind of diosgenin antitumor derivative and its synthetic method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591373A (en) * | 2008-05-28 | 2009-12-02 | 河南大学 | A kind of extracting method of dioscin |
| CN101705275A (en) * | 2009-10-30 | 2010-05-12 | 陕西科技大学 | Process for producing diosgenin and method for processing peltate yam after extracting same |
-
2014
- 2014-04-11 CN CN201410145370.4A patent/CN103965283B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591373A (en) * | 2008-05-28 | 2009-12-02 | 河南大学 | A kind of extracting method of dioscin |
| CN101705275A (en) * | 2009-10-30 | 2010-05-12 | 陕西科技大学 | Process for producing diosgenin and method for processing peltate yam after extracting same |
Non-Patent Citations (1)
| Title |
|---|
| 兀浩: "表面活性剂提取薯蓣皂苷及薯蓣皂苷元水解工艺的研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ集》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774240A (en) * | 2015-04-30 | 2015-07-15 | 陕西科技大学 | Method for extracting diosgenin through dioscin hydrolysis |
| CN105534946A (en) * | 2016-01-11 | 2016-05-04 | 陕西科技大学 | Preparation method of traditional Chinese medicine capsules |
| CN107827949A (en) * | 2017-11-07 | 2018-03-23 | 西南民族大学 | A kind of diosgenin antitumor derivative and its synthetic method |
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