CN101947250A - Novel energy-saving process for extracting and purifying panax notoginseng saponins - Google Patents
Novel energy-saving process for extracting and purifying panax notoginseng saponins Download PDFInfo
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- CN101947250A CN101947250A CN2010102653733A CN201010265373A CN101947250A CN 101947250 A CN101947250 A CN 101947250A CN 2010102653733 A CN2010102653733 A CN 2010102653733A CN 201010265373 A CN201010265373 A CN 201010265373A CN 101947250 A CN101947250 A CN 101947250A
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- radix notoginseng
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Abstract
The invention discloses a novel energy-saving process for extracting and purifying panax notoginseng saponins, comprising: crushing raw materials, extracting solvent, cooling and clarifying extraction liquid, concentrating, chromatographically separating and purifying, decoloring, concentrating, evaporating, etc.; the steps are specifically as follows: pre-processing the pseudo-ginseng raw materials and then feeding into an extracting tank, adding 5-10 times of about 70% of ethanol solution, heating to 75 DEG. C, refluxing and extracting for about 3h; collecting the extraction liquid, cooling and clarifying, performing film concentration and recovering ethanol, stopping concentrating till amount of the permeated ethanol solution is 90% of that of the extraction liquid, evaporating the concentrated solution till to ethanol-free, transferring into a chromatographic column, absorbing the solution by the column, separating and purifying, eluting with 70% of ethanol solution, decoloring the eluent and then leading the eluent into a film concentrator to concentrate, directly feeding the concentrated solution into an evaporator to evaporate and recover the residual ethanol, finally preparing fine extract of the panax notoginseng saponins; through the film concentration process, concentration quantity of thermal evaporation is effectively reduced by 90%, comprehensive energy-saving rate reaches above 80%, absolute recovery rate of the solvent reaches above 90%, and solvent consumption is effectively reduced; thus, the process is evident in energy saving and consumption reducing.
Description
Technical field
The invention belongs to technical field of plant extraction, be specifically related to traditional Radix Notoginseng active ingredient is extracted the improvement of purification technique, more specifically relate to a kind of Radix Notoginseng total arasaponins and extract the purification new energy-saving process.
Background technology
The prior art extraction process that the Radix Notoginseng active ingredient is extracted needs the evaporation and concentration of twice ethanol extract at least, it once is the crude extract evaporation and concentration, it once is the evaporation and concentration of chromatographic column ethanol elution, this twice evaporation not only expends a large amount of steam, and each ethanol concentrates and all can lose about 20% because of alcoholic acid evaporation.Because energy prices go up and the cost of alcohol solvent improves, it is more and more higher that the energy consumption of prior art solvent enrichment process and solvent loss account for the ratio of extracting totle drilling cost, make many pharmacy corporation urgent needss change a social system, to adapt to the energy-saving and cost-reducing economic requirement and the environmental requirement of reduction of discharging to traditional handicraft.Based on this, the inventor is through concentrating on studies, and developed a kind of Radix Notoginseng total glucosides and extracted and concentrate new energy-saving process based on membrane technology, evidence, energy-saving and cost-reducing, emission reduction effect is remarkable.
Summary of the invention
The object of the present invention is to provide a kind of technological process easy, before traditional evaporation technology, increase membrance concentration and process matched therewith, make evaporation capacity reduce 90%, reduce alcoholic acid loss, effectively lower the new energy-saving process that the Radix Notoginseng total arasaponins that extracts the purification cost extracts purification.
The object of the present invention is achieved like this: comprise that raw material pulverizing, solvent extraction, extracting solution cooling clarification, extracting solution membrance concentration, chromatography are purified, decolorizing column is decoloured, the eluent membrance concentration, evaporator evaporation specifically comprises following operation:
A, the Radix Notoginseng raw material cleaned, dries, pulverizes after, send in the extraction pot, add 5-10 and doubly measure 70% left and right sides alcoholic solution, be heated to about 75 ℃ and extracted about 3 hours;
B, will cool off clarifying extracting solution and import film condensing device and concentrate and reclaim ethanol, reaching 90% o'clock of extracting liquid measure to the alcoholic solution amount that sees through stops to concentrate, the ethanol that reclaims goes back to storage tank to be continued to use as extracting with solvent, concentrated solution or directly send into evaporator evaporation and reclaim and obtain the Radix Notoginseng total arasaponins crude extract behind the residue ethanol and send into the C operation and carry out separation and purification;
C, change layer over to and wash post and carry out upper prop and separate to purify from the concentrated solution of slightly carrying of B operation, the alcoholic solution with about 70% carries out eluting as eluent, and the collection eluent is sent into the decolorizing column processing of decolouring earlier;
D, eluent is imported film condensing device concentrate, the alcoholic solution that sees through changes storage tank over to be continued to use with ethanol as eluting, stop to concentrate when isolating alcoholic solution amount reaches eluting liquid measure 90%, concentrated solution is directly sent into and is obtained the smart extracted extract of Radix Notoginseng total arasaponins after evaporator evaporation reclaims residue ethanol.
The present invention has increased membrance concentration and the process matched therewith pre-concentration before as vaporizer before the vaporizer of traditional handicraft, effectively reduce thermal evaporation and concentrate amount 90%, the synthesis energy saving rate reaches more than 80%, the solvent absolute recovery reaches more than 90%, significantly reduced the consumption of solvent, energy conservation and consumption reduction effects of the present invention is remarkable.
Description of drawings:
Accompanying drawing is a process flow diagram of the present invention.
The specific embodiment:
The present invention is further illustrated below in conjunction with accompanying drawing, but never in any form the present invention is limited, and any conversion based on training centre of the present invention is done all falls into protection scope of the present invention.
As shown in drawings, the present invention includes raw material pulverizing, solvent extraction, extracting solution cooling clarification, eluent membrance concentration, chromatography purification, decolorizing column decolouring, eluent membrance concentration, evaporator evaporation specifically comprises following operation:
A, the Radix Notoginseng raw material cleaned, dries, pulverizes after, send in the extraction pot, add 5-10 and doubly measure 70% alcoholic solution, be heated to 75 ℃ of left and right sides reflux, extract, about 3 hours;
B, will cool off clarifying extracting solution and import film condensing device and concentrate and reclaim ethanol, reaching 90% o'clock of extracting liquid measure to isolating alcoholic solution amount stops to concentrate, the ethanol that reclaims goes back to storage tank to be continued to use as extracting, concentrated solution or directly send into evaporator evaporation and reclaim and obtain the Radix Notoginseng total arasaponins crude extract behind the residue ethanol and send into the C operation and carry out separation and purification;
C, change layer over to and wash post and carry out upper prop and separate to purify from the concentrated solution of slightly carrying of B operation, the alcoholic solution with about 70% carries out eluting as eluent, collects eluent, enters decolorizing column and decolours;
D, the eluent after will decolouring import film condensing device and concentrate, reaching 90% o'clock of eluting liquid measure to isolating alcoholic solution amount stops to concentrate, isolating alcoholic solution changes storage tank over to be continued to use as eluting, and concentrated solution is directly sent into and obtained the smart extracted extract of Radix Notoginseng total arasaponins after evaporator evaporation reclaims residue ethanol and moisture content.
Adding 5-10 doubly measures the alcoholic solution about 75% in the described A operation, is heated to about 75 ℃ and extracts about 3 hours.
Cooling in described B operation clarification operation is finished by heat exchanger and microporous filter clarification or centrifugal clarification device.
In the described C operation, the alcoholic solution with about 75% carries out eluting as eluent, collects eluent, sends into the decolorizing column processing of decolouring earlier.
Described clarification operation is finished by centrifuge or microporous filter.
Described chromatographic column is a macroporous adsorptive resins, as D101 or HDD-400 resin chromatographic column.
Described decoloration process is the alumina adsorption post.
Operation principle of the present invention and work process:
In the Radix Notoginseng alcohol extraction process, the temperature of isolated extracting solution is about 75 ℃ from extraction pot, in order to adapt to the arts demand of membrance concentration, enter film condensing device after the cooling clarification, the alcoholic solution that membrance separation goes out is sent into ethanol storage tank and is continued to use as extracting, and concentrated solution (account for extract liquid measure 10%) is sent into evaporator evaporation and obtained crude extract or directly send into purification procedures and carry out separation and purification.
Crude extract is sent into chromatographic column and is carried out chromatography, carries out eluting with alcoholic solution, collects eluent, enters the decolorizing column decolouring.Because eluent series normal temperature state, need not cool off and directly to concentrate eluent, be about to eluent after the decolouring and enter the membrane concentrator group after by microfiltration, isolating alcoholic solution is recycled to the alcoholic solution storage tank, stop to concentrate after isolated ethanol reaches eluting liquid measure 90% when being concentrated into, remain 10% concentrated solution and deliver to evaporator evaporation recovery residue ethanol, obtain refining Radix Notoginseng total arasaponins extractum; Spray-driedly again obtain dry essence and carry product.
The pilot scale example:
After 10Kg Radix Notoginseng raw material cleaned, dries, pulverizes, send in the extraction pot, add 80 liter 70% alcoholic solution, be heated to 75 ℃ of reflux, extract, 3 hours, collect 75 liters of extracting solution; Cooling clarification, membrance concentration also reclaims ethanol, when reaching 67.5 liters, the alcoholic solution amount that sees through stops to concentrate, 7.5 liters of 2.8 liters of thick water lift liquid of residue after ethanol is reclaimed in evaporation of concentrated solution, change macroporous resin column over to and carry out upper prop separation purification, carry out eluting with 80 liter of 70% alcoholic solution, obtain 80 liters of eluents, eluent is imported film condensing device after the decolorizing column decolouring concentrate, 72 liters of ethanol of Separation and Recovery, remaining 8 liters of eluting concentrated solutions, concentrated solution obtains 1.28 kilograms of Radix Notoginseng total arasaponins extracts, extraction ratio 94.5% after directly sending into the evaporator evaporation drying; Wherein the membrance concentration rate of Radix Notoginseng total arasaponins crude extract and eluent all reaches 90%, i.e. concentrated solution: permeate=1: 9, reduce concentrating link evaporation energy consumption 90%.160 liters of shared 70% ethanol, membrance concentration reclaim 139.5 liters, evaporate 12 liters of recovery, reclaim 151.5 liters, the response rate 94.7% altogether in the whole process.
Characteristics of the present invention:
1, energy-conservation: replace the operation of the evaporation Recycled ethanol of prior art, arasaponin extract and eluent evaporation technology section reduce the steam use amount more than 90%, fractional energy savings＞80%.
2, consumption reduction: improve solvent recovering rate, reduce the ethanol loss more than 70%.
3, operating efficiency significantly improves.
4, superior product quality: traditional evaporation and concentration, even in the situation of reduction vaporization, temperature also more than the 70-80 degree, is at high temperature evaporated for a long time, easily decomposition of effective ingredient, polymerization, malformation etc. destroy or loss active ingredient. Because it is not have concentrating of phase transformation that normal temperature concentrates, the notoginseng total saponin effective component content is got to the limit to be kept, and part salt and heavy metal can see through film when film concentrates, and the effect of certain desalination and removing heavy metals is arranged, and end product quality and drug effect also will have substantial raising.
Claims (7)
1. a Radix Notoginseng total arasaponins extracts the purification new energy-saving process, it is characterized in that: comprise that raw material pulverizing, solvent refluxing extraction, extracting solution cooling clarification, extracting solution membrance concentration, chromatography are purified, decolorizing column is decoloured, the eluent membrance concentration, evaporator evaporation specifically comprises following operation:
A, the Radix Notoginseng raw material cleaned, dries, pulverizes after, send in the extraction pot, add 5-10 and doubly measure 70% left and right sides alcoholic solution, be heated to 75 ℃ and extracted about 3 hours;
B, will cool off clarifying extracting solution and import film condensing device and concentrate and reclaim ethanol, reaching 90% o'clock of extracting liquid measure to isolating alcoholic solution amount stops to concentrate, the ethanol that reclaims goes back to storage tank to be continued to use as extracting with solvent, concentrated solution or directly send into evaporator evaporation residue ethanol after obtain the Radix Notoginseng total arasaponins crude extract and send into the C operation and carry out separation and purification;
C, change macroporous resin column over to from the crude extract of B operation and carry out upper prop and separate and purify, the alcoholic solution with 70% carries out eluting as eluent, and the collection ethanol elution is sent into decolorizing column earlier and decoloured;
D, the eluent after will decolouring import film condensing device and concentrate, isolating alcoholic solution changes storage tank over to be continued to use with ethanol as eluting, reach 90% o'clock of eluting liquid measure until the alcoholic solution amount that sees through and stop to concentrate, concentrated solution is directly sent into and is obtained the smart extracted extract of Radix Notoginseng total arasaponins after evaporator evaporation reclaims residue ethanol.
2. Radix Notoginseng total arasaponins as claimed in claim 1 extracts the purification new energy-saving process, and it is characterized in that: described film condensing device comprises nanofiltration device and attached pretreatment micro-filtration thereof.
3. Radix Notoginseng total arasaponins as claimed in claim 1 extracts the purification new energy-saving process, and it is characterized in that: described clarification operation is finished by centrifuge or microporous filter.
4. Radix Notoginseng total arasaponins as claimed in claim 1 extracts the purification new energy-saving process, it is characterized in that: add 5-10 in the described A operation and doubly measure 75% alcoholic solution, be heated to 75 ℃ and extracted about 3 hours.
5. Radix Notoginseng total arasaponins as claimed in claim 1 extracts the purification new energy-saving process, and it is characterized in that: in the described C operation, the alcoholic solution with 75% carries out eluting as eluent, and eluent enters the decolorizing column decolouring again.
6. Radix Notoginseng total arasaponins as claimed in claim 1 extracts the purification new energy-saving process, and it is characterized in that: described chromatographic column is a macroporous adsorptive resins.
7. Radix Notoginseng total arasaponins as claimed in claim 1 extracts the purification new energy-saving process, and it is characterized in that: described decolorizing column is the alumina adsorption post.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102416028A (en) * | 2011-09-12 | 2012-04-18 | 中国科学院昆明植物研究所 | Preparation method of cooked panax notoginseng extract and total ripe panax notoginseng saponins |
| CN103830298A (en) * | 2014-03-26 | 2014-06-04 | 南京中医药大学 | Method for preparing panax notoginseng saponins by adopting membrane coupling technology |
| CN107847891A (en) * | 2015-07-27 | 2018-03-27 | 明尼苏达-达科塔农民合作社 | The method that saponin(e is extracted from agricultural product |
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| CN1508149A (en) * | 2002-12-18 | 2004-06-30 | 中南大学 | Method for extracting total triterpenic acid, ursolic acid and oleanolic acid from Taiwan lectuce herb tea |
| US20050037094A1 (en) * | 2003-07-31 | 2005-02-17 | Xijun Yan | Composition for heart disease, its active ingredients, method to prepare same and uses thereof |
| CN1634970A (en) * | 2004-11-18 | 2005-07-06 | 张平 | Process for preparing notoginsen triterpenes |
| CN1721026A (en) * | 2005-05-18 | 2006-01-18 | 戴群 | Integrated membrane circulation extracting process |
| CN1721028A (en) * | 2005-05-18 | 2006-01-18 | 戴群 | Integrated membrane circulation extracting apparatus |
| CN101450091A (en) * | 2008-12-30 | 2009-06-10 | 云南云科药业有限公司 | Purification method of Panax notoginseng saponins |
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2010
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1508149A (en) * | 2002-12-18 | 2004-06-30 | 中南大学 | Method for extracting total triterpenic acid, ursolic acid and oleanolic acid from Taiwan lectuce herb tea |
| US20050037094A1 (en) * | 2003-07-31 | 2005-02-17 | Xijun Yan | Composition for heart disease, its active ingredients, method to prepare same and uses thereof |
| CN1634970A (en) * | 2004-11-18 | 2005-07-06 | 张平 | Process for preparing notoginsen triterpenes |
| CN1721026A (en) * | 2005-05-18 | 2006-01-18 | 戴群 | Integrated membrane circulation extracting process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102416028A (en) * | 2011-09-12 | 2012-04-18 | 中国科学院昆明植物研究所 | Preparation method of cooked panax notoginseng extract and total ripe panax notoginseng saponins |
| CN103830298A (en) * | 2014-03-26 | 2014-06-04 | 南京中医药大学 | Method for preparing panax notoginseng saponins by adopting membrane coupling technology |
| CN107847891A (en) * | 2015-07-27 | 2018-03-27 | 明尼苏达-达科塔农民合作社 | The method that saponin(e is extracted from agricultural product |
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Effective date of registration: 20210805 Address after: 650106 Xinming lane, Kegao Road, high tech Zone, Kunming City, Yunnan Province Patentee after: YUNNAN HUOCAOTANG BIOTECHNOLOGY Co.,Ltd. Address before: Building 1, Kunming Electrical Factory, 723 Chuanjin Road, Kunming, Yunnan, 650224 Patentee before: Dai Qun |
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