CN102631521B - Method for extracting dioscin by utilizing two-aqueous-phase system - Google Patents
Method for extracting dioscin by utilizing two-aqueous-phase system Download PDFInfo
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Abstract
The invention discloses a method for extracting dioscin by utilizing a two-aqueous-phase system. In the method disclosed by the invention, an ethanol/ammonium sulphate two-aqueous-phase system is taken as an extracting agent, an ultrasonic wave/SDS (sodium dodecyl sulphate) synergic auxiliary two-aqueous-phase system is adopted for extracting the dioscin, and then acid hydrolysis is carried out to produce diosgenin. By adopting the method disclosed by the invention, every gram of common yam dry powder can obtain more than 27.5mg of diosgenin, the purity reaches 85% or above, and single extraction recovery rate is more than 60%. Compared with the traditional acid hydrolysis method, the method disclosed by the invention has the advantages of rapid extraction, low acid consumption and less pollution; and the method disclosed by the invention has the advantages of low cost, easiness in operation and easiness in recovery of solvent in upper phase and lower phase compared with a common salt/polymer two-aqueous-phase system.
Description
Technical field
The present invention relates to a kind of extracting method of natural plant effective constituent, be specifically related to the method for the collaborative auxiliary aqueous two-phase extraction dioscin of a kind of ultrasonic wave/SDS.
Background technology
Rhizome of Peltate Yam (Dioscorea zingiberensis) has another name called yellow ginger, and the duration and degree of heating root contains multiple dioscin, yellow pigment, tannin, much starch and Mierocrystalline cellulose in its rhizome.Wherein, dioscin has pharmacological action widely and important biological activity, as antitumor, antimycotic, prevention and cure of cardiovascular disease, hypoglycemic, regulate immunity etc.In industrial production, dioscin is mainly for the production of diosgenin.Diosgenin, be commonly called as diosgenin, and chemical name is different volution-5-alkene-3 β-ol, belongs to the derivative of different spirostene alkane, is the important foundation raw material of numerous steroid hormone medicines such as synthetic contraceptive bian.
Utilize the method for the rhizome production diosgenin of Rhizome of Peltate Yam that the methods such as direct acid hydrolysis, pre-fermentation-acid hydrolysis, enzymolysis-acid hydrolysis, pre-separation Mierocrystalline cellulose-starch are arranged.Although can improve the saponin(e yield by pretreatment processs such as spontaneous fermentation, starch separation, enzymolysis, these methods all exist deficiency separately, for example the condition of spontaneous fermentation is difficult to control, and easily introduces miscellaneous bacteria, carrys out hidden danger to the medicine securing band; The starch partition method need be carried out sequence of operations, causes the saponin(e loss more; And the additional enzyme preparation improves production cost, thereby be difficult to practical application.At present mainly on industrial production adopt direct acid-hydrolysis method, but the shortcoming such as the method exists that sour consumption is large, seriously polluted, byproduct starch and Mierocrystalline cellulose can't reclaim.In recent years, people attempt exploration and at first in the rhizome of Rhizome of Peltate Yam, isolate dioscin, and then the method for producing diosgenin by acid hydrolysis, like this because Mierocrystalline cellulose, starch do not participate in hydrolysis, can greatly reduce sour consumption, the pollution of minimizing to environment, simultaneously also provide possibility for reclaiming the byproducts such as starch and Mierocrystalline cellulose, thereby provide new approaches for the environmental protection production of diosgenin.
The traditional technology that dioscin extracts is generally to adopt the method that cold soaking is put forward or laser heating refluxes, these methods not only extraction time long, extract not exclusively the shortcoming such as saponin(e loses larger, and the product yield is lower but also exist.Aqueous two-phase extraction is in recent years emerging a kind of high efficient separation technology.Traditional polymkeric substance-salt double-aqueous phase system is owing to existing extracting solution viscosity larger, and polymkeric substance is difficult for reclaiming, and production cost is high, and therefore the shortcomings such as subsequent disposal trouble are difficult to promote in actual suitability for industrialized production.
Summary of the invention
The objective of the invention is in order to overcome the existing above-mentioned deficiency of prior art, provide that a kind of operation steps is simple, the time is short, the rate of recovery is high, organic solvent consumption is few, environmental pollution is little, production cost is low and be easy to the diosgenin novel preparation method that industry is amplified.The present invention adopts the ethanol/ammonium sulfate double-aqueous phase system, in conjunction with supplementary meanss such as ultrasonic wave, SDS, at first from the Chinese yam rhizome, extracts total saponins, then is hydrolyzed with a small amount of acid, then adopts ethanol precipitation to extract diosgenin.The present invention is the new technology of the auxiliary aqueous two-phase extraction of a kind of ultrasonic wave/tensio-active agent, and this technology is enriched in pure phase by effective constituent, and the impurity such as foreign protein and polysaccharide are removed with the form of precipitation.
Its technical scheme is:
A kind of method of aqueous two-phase extraction dioscin comprises the following steps:
1) according to ammonium sulfate concentrations, be 15%～20% (w/w), alcohol concn is 29%～33% (w/v), and SDS concentration is 0.001～0.007mg/mL, sets up double-aqueous phase system;
2) by tapioca flour, by solid-liquid ratio, be that 0.05～0.1g/mL adds step 1) double-aqueous phase system in;
3) at ultrasonic power, be 200～300W, ultrasonic frequency is 20～80HZ, under the condition that temperature is 25～40 ℃, extracts 30～70min;
4) stratification, get upper strata alcohol phase, and ethanol is reclaimed in underpressure distillation, obtains the dioscin crude product.
Step 1) ammonium sulfate concentrations described in is 18% (w/w), and alcohol concn is 30% (w/v), and SDS concentration is 0.0045mg/mL.
Step 2) described is 0.058g/mL by tapioca flour by solid-liquid ratio.
Step 3) described ultrasonic power is 250W, and ultrasonic frequency is 75HZ, and extraction temperature is 37 ℃, and the time is 60min.
Further, to step 4) described in the dioscin crude product proceed following processing:
5) by solid-liquid ratio, be that 0.1～0.3g/mL is dissolved in the sulphuric acid soln of 1mol/L, boiling water bath backflow 3～4h, filter, and with 1% sodium bicarbonate washing filter residue, then is washed till neutrality with distilled water, then dry under 60～80 ℃, obtains the diosgenin crude product;
6) by step 5) the saponin dissolving crude product is in the dehydrated alcohol of 65～75 ℃, and solid-liquid ratio is 0.02～0.08g/mL, adds activated carbon powder to remove pigment, removes by filter gac;
7) ethanol is reclaimed in underpressure distillation, and then the cooling diosgenin of separating out, filter results saponin precipitation, and volatilize ethanol under 50～90 ℃, obtains the elaboration saponin.
Step 5) solid-liquid ratio described in is 0.2g/mL, and cracking 3h is dry under 80 ℃.
Step 6) in, the saponin dissolving crude product of gained is in the dehydrated alcohol of 70 ℃, and solid-liquid ratio is 0.05g/mL.
Step 7) in, under 60 ℃, volatilize ethanol.
Beneficial effect of the present invention:
Compared with prior art, technical scheme of the present invention has the following advantages:
1. the method for the invention adopts and adds a small amount of tensio-active agent and ultrasonic synergistic Assisted Ethanol/ammonium sulfate double-aqueous phase system to be extracted, with traditional direct acid hydrolysis process, compare, extraction time shortens greatly, the recyclable recycling of solvent and ammonium sulfate, the acid consumption greatly reduces, and has realized environmental protection production;
2. the present invention compares with traditional polymkeric substance-salt double-aqueous phase system, has overcome latter's polymer viscosity larger, is difficult for the remanufacture cost high, the shortcomings such as subsequent disposal trouble;
3. the present invention compares with simple ethanol/ammonium sulfate double-aqueous phase system, has reduced the use of organic solvent, and efficient, energy-conservation, pollute less, production cost is low;
4. the present invention and C0
2Relatively, less investment, be easy to promote, and the foreign matter content in product is low for the supercritical extraction system.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in more detail.
Embodiment 1 cleans the Chinese yam sample, removes the part of going rotten, addle, and cuts into slices, and is placed in 60 ℃ of baking ovens and dries to constant weight.The sample of oven dry is crushed to 200 orders with pulverizer, standby.
According to ammonium sulfate concentrations, be 17% (w/w), alcohol concn is 31% (w/v), and SDS concentration is 0.005mg/mL, sets up double-aqueous phase system;
20g Chinese yam powder is added in double-aqueous phase system by solid-liquid ratio 0.08g/mL, is 250W at ultrasonic power, and ultrasonic frequency is 75HZ, under the condition that temperature is 37 ℃, and extraction 60min.
Stratification, get upper strata alcohol phase, and heating recovery ethanol, obtain the dioscin crude product.
Embodiment 2 cleans the Chinese yam sample, removes the part of going rotten, addle, and cuts into slices, and is placed in 60 ℃ of baking ovens and dries to constant weight.The sample of oven dry is crushed to 200 orders with pulverizer, standby.
According to ammonium sulfate concentrations, be 15% (w/w), alcohol concn is 29% (w/v), and SDS concentration is 0.001mg/mL, sets up double-aqueous phase system;
20g Chinese yam powder is added in double-aqueous phase system by solid-liquid ratio 0.05g/mL, is 200W at ultrasonic power, and ultrasonic frequency is 30HZ, under the condition that temperature is 25 ℃, and extraction 30min.
Stratification, get upper strata alcohol phase, and heating recovery ethanol, obtain the dioscin crude product.
Embodiment 3 cleans the Chinese yam sample, removes the part of going rotten, addle, and cuts into slices, and is placed in 60 ℃ of baking ovens and dries to constant weight.The sample of oven dry is crushed to 200 orders with pulverizer, standby.
According to ammonium sulfate concentrations, be 20% (w/w), alcohol concn is 33% (w/v), and SDS concentration is 0.007mg/mL, sets up double-aqueous phase system;
20g Chinese yam powder is added in double-aqueous phase system by solid-liquid ratio 0.1g/mL, is 300W at ultrasonic power, and ultrasonic frequency is 80HZ, under the condition that temperature is 40 ℃, and extraction 70min.
Stratification, get upper strata alcohol phase, and heating recovery ethanol, obtain the dioscin crude product.
Embodiment 4 cleans the Rhizome of Peltate Yam rhizome, removes the part of going rotten, addle, and uses the size reduction machinery pulping, standby.
By Rhizome of Peltate Yam rhizome slurries, ammonium sulfate, 95% ethanol, SDS and water mix and blend, making ammonium sulfate concentrations is 17% (w/w), alcohol concn is 30% (w/v), and SDS concentration is 0.007mg/mL, and Chinese yam dry-matter ratio is that 0.08g/mL adds in double-aqueous phase system, at ultrasonic power, be 300W, ultrasonic frequency is 80HZ, under the condition that temperature is 40 ℃, and extraction 70min.
Stratification, get upper strata alcohol phase, and heating recovery ethanol, obtain the dioscin crude product.
Embodiment 5 prepares diosgenin by embodiment 1,2,3,4 gained dioscins according to following steps:
By the saponin(e crude product, by solid-liquid ratio, be that 0.2g/mL is dissolved in the sulphuric acid soln of 1mol/L, the boiling water bath reflux, cracking 3h, filter, and with 1% sodium bicarbonate washing filter residue, then is washed till neutrality with distilled water, then dry under 80 ℃, obtains the diosgenin crude product.
By the saponin dissolving crude product, in the dehydrated alcohol of 75 ℃, solid-liquid ratio is 0.05g/mL, adds activated carbon powder to remove pigment, removes by filter gac.
Ethanol is reclaimed in underpressure distillation, and then the cooling diosgenin of separating out, filter results saponin precipitation, and volatilize ethanol under 60 ℃, obtains the elaboration saponin.
The total saponins that utilizes the method for embodiment to prepare is produced saponin, and every 20 gram Chinese yam dry powder can obtain the above saponin of 550mg, and purity reaches more than 90%.Can obtain the above saponin of 650mg after extracting three times, the saponin rate of recovery of single extraction surpasses 75%.
The above; it is only preferably embodiment of the present invention; protection scope of the present invention is not limited to this; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses, the simple change of the technical scheme that can obtain apparently or equivalence are replaced and are all fallen within the scope of protection of the present invention.
Claims (7)
1. the method for an aqueous two-phase extraction dioscin, is characterized in that, comprises the following steps:
1) according to ammonium sulfate concentrations w/w, be 15%～20%, alcohol concn w/v is that 29%～33%, SDS concentration is 0.001～0.007mg/mL, sets up double-aqueous phase system;
2) by tapioca flour, by solid-liquid ratio, be that 0.05～0.1g/mL adds step 1) double-aqueous phase system in;
3) at ultrasonic power, be 200～300W, ultrasonic frequency is 20～80Hz, under the condition that temperature is 25～40 ℃, extracts 30～70min;
4) stratification, get upper strata alcohol phase, and heating recovery ethanol, obtain the dioscin crude product;
5) to step 4) described in the dioscin crude product proceed following processing: by solid-liquid ratio, be that 0.1～0.3g/mL is dissolved in the sulphuric acid soln of 1mol/L, the boiling water bath reflux, cracking 3～4h, filter, with 1% sodium bicarbonate washing filter residue, be washed till neutrality with distilled water again, then dry under 60～100 ℃, obtain the diosgenin crude product;
6) by step 5) the saponin dissolving crude product is in the dehydrated alcohol of 65～75 ℃, and solid-liquid ratio is 0.02～0.08g/mL, adds activated carbon powder to remove pigment, removes by filter gac;
7) ethanol is reclaimed in underpressure distillation, and then the cooling diosgenin of separating out, filter results saponin precipitation, and volatilize ethanol under 50～90 ℃, obtains the elaboration saponin.
2. the method for aqueous two-phase extraction dioscin according to claim 1, is characterized in that step 1) described in ammonium sulfate concentrations w/w be 18%, alcohol concn w/v is that 33%, SDS concentration is 0.0045mg/mL.
3. the method for aqueous two-phase extraction dioscin according to claim 1, is characterized in that step 2) described by tapioca flour, by solid-liquid ratio, be 0.058g/mL.
4. the method for aqueous two-phase extraction dioscin according to claim 1, is characterized in that step 3) described at ultrasonic power, be 250W, ultrasonic frequency is 75Hz, under the condition that temperature is 37 ℃, the extraction 60min.
5. the method for aqueous two-phase extraction dioscin according to claim 1, is characterized in that step 5) described in solid-liquid ratio be 0.2g/mL, cracking 3h, dry under 80 ℃.
6. the method for aqueous two-phase extraction dioscin according to claim 1, is characterized in that step 6) in the saponin dissolving crude product of gained in the dehydrated alcohol of 70 ℃, solid-liquid ratio is 0.05g/mL.
7. the method for aqueous two-phase extraction dioscin according to claim 1, is characterized in that step 7) in volatilize ethanol under 60 ℃.
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| CN102974125A (en) * | 2012-11-25 | 2013-03-20 | 竹溪创艺皂素有限公司 | Method for extracting saponin in yellow ginger by utilizing ultrasonic-assisted ethanol extraction |
| CN104435060B (en) * | 2014-11-05 | 2018-03-20 | 桂林三宝生物科技有限公司 | A kind of method that gynosaponin is extracted from gynostemma pentaphylla |
| CN106866835B (en) * | 2017-04-14 | 2019-03-01 | 张仕英 | A kind of ultrasonic technology extracts the preparation method of bletilla striata extract |
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| CN102366518A (en) * | 2011-10-17 | 2012-03-07 | 西北农林科技大学 | Method for ultrasonic assisted aqueous two-phase extraction of total dioscin |
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| CN102366518A (en) * | 2011-10-17 | 2012-03-07 | 西北农林科技大学 | Method for ultrasonic assisted aqueous two-phase extraction of total dioscin |
Non-Patent Citations (2)
| Title |
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| 刘琳，等.微波辅助双水相提取盾叶薯蓣中的皂苷成分.《过程工程学报》.2009,第9卷(第6期),摘要. * |
| 李祥,等.表面活性剂在盾叶薯蓣中萃取皂苷的应用研究.《中国酿造》.2012,第31卷(第2期),2.1表面活性剂的选择. * |
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