CN100451029C - Technique for extracting yam saponin, amylocellulose, and yellow pigment by separating yam - Google Patents
Technique for extracting yam saponin, amylocellulose, and yellow pigment by separating yam Download PDFInfo
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- CN100451029C CN100451029C CNB2006100311580A CN200610031158A CN100451029C CN 100451029 C CN100451029 C CN 100451029C CN B2006100311580 A CNB2006100311580 A CN B2006100311580A CN 200610031158 A CN200610031158 A CN 200610031158A CN 100451029 C CN100451029 C CN 100451029C
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Abstract
This invention discloses a process for separating and extracting dioscin, amylocellulose and yellow pigment from yam. The method comprises: (1) pulverizing yam or pulping, extracting with industrial alcohol solvent for 1-8 h, filtering the extract, cooling to obtain crude yellow pigment, separating and purifying with macroporous adsorption resin to obtain yellow pigment; (2) hydrolyzing the residue in sulfuric acid solution under pressure, or naturally fermenting at 25-50 deg.C and then hydrolyzing in sulfuric acid solution under pressure, washing the residue with cold water, or neutralizing with alkaline compound, drying, milling, heating in gasoline or petroleum ether, filtering, concentrating the crude extract, and crystallizing to obtain white dioscin crystal. The method utilizes fresh or dried yam as the raw material, and recovers the effective components in it. The pulverized yam is extracted with industrial alcohol solvent to obtain dioscin, which is then acid-hydrolyzed, thus reducing aicd consumption and wastewater discharge. Besides, energy and reagent consumption needed for drying and decolorization is also reduced.
Description
[technical field]
The present invention relates to a kind of from Chinese yam the technology of separation and Extraction diosgenin, farinose, yellow pigment.
[background technology]
Traditional suitability for industrialized production diosgenin is to be starting material with the exsiccant Chinese yam, adopts fermentation-acid hydrolysis in advance-gasoline to extract diosgenin from Rhizome of Peltate Yam.This process spent water discharging is serious, and decoloration process is loaded down with trivial details, and the diosgenin foreign matter content of gained is higher.To the extraction or the production of diosgenin in the Chinese yam, also there is the big problem of sour consumption, and for from Chinese yam, extracting starch, Mierocrystalline cellulose, yellow pigment, diosgenin simultaneously, realize that filtering decolouring after raw-material integrated application and the alcohol extracting does not see that as yet report is arranged.
[summary of the invention]
Serious and measure big problem in order to overcome sewage discharge in traditional diosgenin production process with acid, the present invention adopt Chinese yam not with pigment broken-technology of ethanol-extracted-filtration decolouring-acid hydrolysis-gasoline refluxing extraction.At in the diosgenin production process saponin acid hydrolysis being become sapogenin and use the problem of a large amount of acid solutions, and the R base of considering saponin is a glycosyl, the characteristics of possess hydrophilic property, the present invention proposes do not add water and directly pulverize Chinese yam after, extract through the industrial alcohols kind solvent earlier, with the saponin solid filtering after the alcohol extracting, carry out acid hydrolysis again.The present invention includes following concrete steps:
(1) dried stem tuber Chinese yam is not added water directly be crushed to the 50-500 order maybe will be with hollander with bright stem tuber Chinese yam polishing pulping, with industrial alcohol compound heating extraction 1-8 hour;
(2) with the extracting solution filtered while hot of industrial alcohols compounds, filter residue is starch, cellulosic mixture, can be used as fermentative production alcohol with raw material or feed with raw material or agricultural fertilizer;
(3) with extracting solution cooling, the filtration of industrial alcohols compounds, filter residue is stand-by.Reclaim methyl alcohol or ethanol in the filtrate, obtain the yellow pigment crude extract, the yellow pigment crude extract can further get yellow pigment with the macroporous adsorbent resin separation and purification;
(4) filter residue distillation is further reclaimed the industrial alcohols compounds after, filter residue with sulphuric acid soln under the condition of pressurization hydrolysis 2-4 hour or in 25-50 ℃ spontaneous fermentation after 48 hours with sulphuric acid soln under the condition of pressurization hydrolysis 2-4 hour;
(5) through the cooling of acid-hydrolyzed solution, filter, filter residue with cold wash to neutral or with NaOH, CaO or NaHCO
3Be neutralized to the pH value between 7-9 Deng basic cpd;
(6) filter residue is dried to constant weight between 80-90 ℃, and grinds;
(7) grind the back filter residue and heated 2-8 hour with gasoline or sherwood oil, filtered while hot gets filtrate;
(8) filtrate is reclaimed gasoline or sherwood oil, and the product of will slightly carrying concentrate and crystallization;
(9) add cold gasoline or sherwood oil in crystallization, the residue pigment in the product is slightly carried in dissolving, promptly gets the diosgenin of white crystals, and with crystallizing and drying to constant weight.Cold gasoline or sherwood oil recycle as feed intake next time.
The present invention serves as to produce starting material with bright stem tuber Chinese yam or dried stem tuber Chinese yam, has enlarged raw-material range of application, effectively reduces the dry required energy consumption of Chinese yam.Filtration after the alcohol extracting reduces pigment and brings next road production process into, reduced the energy consumption and the material consumption of decolouring, has also reduced the required space of sour water discharging, fermentation and the disposal of pollutants of fermented liquid, reduced follow-up extraction or produce in the gasoline consumption.
[embodiment]
Embodiment 1 with a certain amount of Rhizome of Peltate Yam (bright stem tuber) do not add water with hollander with Rhizome of Peltate Yam (bright stem tuber) polishing pulping, take by weighing Rhizome of Peltate Yam slurry 100 grams, be placed on and add 200 ml methanol in the apparatus,Soxhlet's, speed is to reflux once in 4 minutes, refluxed 6 hours, alcohol insoluble solids is starch, cellulosic mixture in the apparatus,Soxhlet's, can be used as fermentative production alcohol with raw material or feed with raw material or agricultural fertilizer; Phegma is fully cooled off, use filter paper filtering, reclaim the methyl alcohol in the filtrate, obtain the yellow pigment crude extract, the yellow pigment crude extract can further get yellow pigment with the macroporous adsorbent resin separation and purification; Filter residue is placed 40 ℃ of spontaneous fermentations 48 hours, add 100 milliliter 12.8% sulphuric acid soln hydrolysis 6 hours, be cooled to room temperature, filter, filter residue is extremely neutral with cold water flush, in 80 ℃ of loft drier, dry to constant weight, add 200 milliliters of No. 120 gasoline and in apparatus,Soxhlet's, refluxed 6 hours, concentrate and reclaim gasoline, get the solid crystal thing, the solid crystal thing is placed on the filter paper filters, and with cold gasoline flush away pigment.The solid crystal thing is dried to constant weight under 80-90 ℃ of condition, get the white diosgenin powder of 0.85 gram.
Embodiment 2 with a certain amount of Rhizome of Peltate Yam (bright stem tuber) do not add water with hollander with Rhizome of Peltate Yam (bright stem tuber) polishing pulping, take by weighing Rhizome of Peltate Yam slurry 100 grams, add 50 ml methanol, heated 1 hour, and used the filter paper filtered while hot, alcohol insoluble solids is starch, cellulosic mixture, add 50 ml methanol again, heated 1 hour, and used the filter paper filtered while hot, it is stand-by to merge twice filtrate; Filter residue as fermentative production alcohol with raw material or feed with raw material or agricultural fertilizer; Twice filtrate after the merging is fully cooled off, and obtains a large amount of dioscins, filters, and reclaims the methyl alcohol in filtrate and the filter residue, and filtrate obtains the yellow pigment crude extract after reclaiming methyl alcohol, and the yellow pigment crude extract can further get yellow pigment with the macroporous adsorbent resin separation and purification; Add 100 milliliter 12.8% sulphuric acid soln hydrolysis 6 hours in the filter residue, be cooled to room temperature, filter filter residue NaHCO
3Be neutralized to the pH value between 7-9 Deng basic cpd, in 80 ℃ of loft drier, dry, add 200 milliliters of sherwood oils and in apparatus,Soxhlet's, refluxed 6 hours, concentrate and reclaim gasoline, the solid crystal thing, the solid crystal thing is placed on the filter paper filters, and with cold gasoline flush away pigment.The solid crystal thing is dried to constant weight under 80-90 ℃ of condition, get the white diosgenin powder of 0.82 gram.
Or else embodiment 3 adds a certain amount of Rhizome of Peltate Yam (dried stem tuber) with pulverizer under the condition of water and directly is crushed to the 50-500 order, take by weighing Rhizome of Peltate Yam slurry 100 grams, be placed on and add 200 milliliters of ethanol in the apparatus,Soxhlet's, speed is to reflux once in 5 minutes, refluxed 6 hours, alcohol insoluble solids is starch, cellulosic mixture in the apparatus,Soxhlet's, can be used as fermentative production alcohol with raw material or feed with raw material or agricultural fertilizer; Phegma is fully cooled off, use filter paper filtering, reclaim the ethanol in the filtrate, obtain the yellow pigment crude extract, the yellow pigment crude extract can further get yellow pigment with the macroporous adsorbent resin separation and purification; In filter residue, add 100 milliliter 12.8% sulphuric acid soln hydrolysis 6 hours, be cooled to room temperature, filter, filter residue is neutralized to the pH value between 7-9 with basic cpds such as NaOH, dries to constant weight in 80 ℃ of loft drier, adds 200 milliliters of No. 120 gasoline and refluxes in apparatus,Soxhlet's 6 hours, concentrate and reclaim gasoline, the solid crystal thing, the solid crystal thing is placed on the filter paper filters, and with cold gasoline flush away pigment.The solid crystal thing is dried to constant weight under 80-90 ℃ of condition, get the white diosgenin powder of 2.45 grams.
Embodiment 4 with a certain amount of Rhizome of Peltate Yam (bright stem tuber) do not add water with hollander with Rhizome of Peltate Yam (bright stem tuber) polishing pulping, take by weighing Rhizome of Peltate Yam slurry 100 grams, add 50 milliliters of ethanol, heated 1 hour, and used the filter paper filtered while hot, alcohol insoluble solids is starch, cellulosic mixture, add 50 milliliters of ethanol again, heated 1 hour, and used the filter paper filtered while hot, it is stand-by to merge twice filtrate; Filter residue as fermentative production alcohol with raw material or feed with raw material or agricultural fertilizer; Twice filtrate after the merging is fully cooled off, and obtains a large amount of dioscins, filters, and reclaims the ethanol in filtrate and the filter residue, obtains the yellow pigment crude extract behind the filtrate recycling ethanol, and the yellow pigment crude extract can further get yellow pigment with the macroporous adsorbent resin separation and purification; The sulphuric acid soln that adds 100 milliliter 12.8% in the filter residue soaked 12 hours, and pressurized hydrolysis in pressure kettle (101.3-142.7kPa) 2 hours is cooled to room temperature, filtered filter residue Na
2CO
3Or basic cpd such as CaO is neutralized to the pH value between 7-9, dries in 80 ℃ of loft drier, adds 300 milliliters of sherwood oils to reflux in apparatus,Soxhlet's 6 hours, concentrate and reclaim gasoline, the solid crystal thing, the solid crystal thing is placed on the filter paper filters, and with cold gasoline flush away pigment.The solid crystal thing is dried to constant weight under 80-90 ℃ of condition, get the white diosgenin powder of 0.79 gram.
Chinese yam of the present invention is meant Rhizome of Peltate Yam, imperial Chinese yam, Chinese yam classes such as powder back of the body Chinese yam, hollyhock Chinese yam, Xiao Hua Chinese yam.
Claims (4)
1. the technology of a separation and Extraction diosgenin from Chinese yam, farinose mixture and yellow pigment is characterized in that comprising the following steps:
(1) dried stem tuber Chinese yam directly is crushed to the 50-500 order or with hollander with bright stem tuber Chinese yam polishing pulping, with industrial alcoholic solvent heating extraction 1-8 hour;
(2) with the extracting solution filtered while hot of industrial alcohols kind solvent, filter residue is starch, cellulosic mixture, as fermentative production alcohol with raw material or feed with raw material or agricultural fertilizer;
(3) with extracting solution cooling, the filtration of industrial alcohols kind solvent, filter residue is stand-by, reclaims the industrial alcohols kind solvent in the filtrate, obtains the yellow pigment crude extract, and the yellow pigment crude extract gets yellow pigment with the macroporous adsorbent resin separation and purification;
(4) filter residue distillation is further reclaimed the industrial alcohols kind solvent after, filter residue with sulphuric acid soln under the condition of pressurization hydrolysis 2-4 hour or in 25-50 ℃ spontaneous fermentation after 48 hours with sulphuric acid soln under the condition of pressurization hydrolysis 2-4 hour;
(5) through acid-hydrolyzed solution cooling, filtration, filter residue is extremely neutral with cold wash; Filter residue is dried to constant weight between 80-90 ℃, and grinds;
(6) grind the back filter residue and heated 2-8 hour, filter, get filtrate with gasoline or sherwood oil;
(7) filtrate is reclaimed gasoline or sherwood oil, and the product of will slightly carrying concentrate and crystallization;
(8) add cold gasoline or petroleum ether in crystallization, the residue pigment in the product is slightly carried in dissolving, the diosgenin crystallization that promptly get white crystals, and with crystallizing and drying to constant weight, cold gasoline or sherwood oil conduct feed intake next time and recycle.
2. according to claim 1 a kind of from Chinese yam the technology of separation and Extraction diosgenin, farinose mixture and yellow pigment, it is characterized in that: described Chinese yam is fresh Chinese yam or dried stem tuber Chinese yam.
3. according to claim 1 a kind of from Chinese yam the technology of separation and Extraction diosgenin, farinose mixture and yellow pigment, it is characterized in that: described Chinese yam is Rhizome of Peltate Yam, Dioscorea nipponica Mak. Ningpo Yam Rhizome, the powder back of the body Chinese yam, hollyhock Chinese yam or Xiao Hua Chinese yam.
4. according to claim 1 a kind of from Chinese yam the technology of separation and Extraction diosgenin, farinose mixture and yellow pigment, it is characterized in that the described cold water flush of step (5) is with NaOH, CaO, Na
2CO
3Or NaHCO
3The basic cpd neutralization method replaces, up to the pH value between 7-9.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100311580A CN100451029C (en) | 2006-01-18 | 2006-01-18 | Technique for extracting yam saponin, amylocellulose, and yellow pigment by separating yam |
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| CNB2006100311580A CN100451029C (en) | 2006-01-18 | 2006-01-18 | Technique for extracting yam saponin, amylocellulose, and yellow pigment by separating yam |
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| CN100451029C true CN100451029C (en) | 2009-01-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805777B (en) * | 2010-02-24 | 2012-04-25 | 中国科学院过程工程研究所 | Steam explosion primary refining poly-generation method of dioscorea raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101402669B (en) * | 2008-11-19 | 2013-03-20 | 湖南科源生物制品有限公司 | Environment friendly method for producing diosgenin |
| CN101885750B (en) * | 2010-03-08 | 2012-08-22 | 李绍通 | Method for circularly processing and utilizing rhizome in dioscorea |
| CN101816372B (en) * | 2010-05-17 | 2015-04-22 | 湘西自治州奥瑞克医药化工有限责任公司 | Clean production method of coproduced biologic protein feed of diosgenin |
| CN102464898B (en) * | 2010-11-13 | 2014-04-09 | 陕西理工学院 | Method for recovering yellow ginger pigment from yellow ginger hydrolysate saponin extraction waste liquid |
| CN102321184B (en) * | 2011-08-08 | 2014-04-09 | 武汉纺织大学 | Resource utilization technology of fresh peltate yam |
| CN103087144A (en) * | 2013-01-24 | 2013-05-08 | 湖北民族学院 | Diosgenin production method |
| CN103319564A (en) * | 2013-06-24 | 2013-09-25 | 向华 | Method for producing diosgenin, yellow pigment and acidic starch by using yellow ginger |
| CN103583184A (en) * | 2013-10-17 | 2014-02-19 | 固镇县玉鹏蔬菜开发有限责任公司 | Method for artificially cultivating dioscorea nipponica in forests |
| CN107814828B (en) * | 2017-11-19 | 2020-07-21 | 十堰赟天生物科技发展有限公司 | Unconventional extraction technology of hydrolysate |
| CN108559305B (en) * | 2018-05-31 | 2021-02-19 | 北京市农林科学院 | Fresh-cut Chinese yam yellow pigment with antioxidant activity and preparation method thereof |
| CN109438546A (en) * | 2018-10-23 | 2019-03-08 | 王吟箫 | A kind of technique that saponin is extracted from plants |
| CN109825107A (en) * | 2019-04-03 | 2019-05-31 | 王国锋 | The technique of pigment and saponin is extracted in a kind of yellow ginger |
| CN109851656A (en) * | 2019-04-03 | 2019-06-07 | 山东洲星生物技术有限公司 | The technique of pigment and saponin is extracted in a kind of yellow ginger saponin(e |
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| CN1243834A (en) * | 1999-06-27 | 2000-02-09 | 中国科学院昆明植物研究所 | Process for preparing yam saponin |
| CN1418888A (en) * | 2002-12-09 | 2003-05-21 | 吉林天药科技股份有限公司 | Novel process for preparing diosgenin |
| CN1699399A (en) * | 2004-05-23 | 2005-11-23 | 张万举 | Process for preparing yam saponin |
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Patent Citations (3)
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| CN1243834A (en) * | 1999-06-27 | 2000-02-09 | 中国科学院昆明植物研究所 | Process for preparing yam saponin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101805777B (en) * | 2010-02-24 | 2012-04-25 | 中国科学院过程工程研究所 | Steam explosion primary refining poly-generation method of dioscorea raw material |
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