CN103965152A - Extraction and preparation method for licorice effective ingredients - Google Patents
Extraction and preparation method for licorice effective ingredients Download PDFInfo
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- CN103965152A CN103965152A CN201310027675.0A CN201310027675A CN103965152A CN 103965152 A CN103965152 A CN 103965152A CN 201310027675 A CN201310027675 A CN 201310027675A CN 103965152 A CN103965152 A CN 103965152A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
Abstract
The invention relates to an extraction and preparation method for licorice effective ingredients, mainly to a method for simultaneously extracting effective ingredients like glycyrrhizic acid, glycyrrhiza flavonoid and a licorice flavoring agent from licorice. The method comprises the following steps: with glycyrrhizic acid as a raw material, carrying out extraction so as to obtain licorice residue and extract liquid and subjecting the licorice residue to ethanol extraction so as to obtain a crude glycyrrhiza flavonoid product; removing impurities in the licorice extract liquid by using an ultrafiltration membrane device, carrying out concentration by using a nanofiltration membrane device, subjecting a nanofiltration membrane concentrate to acid precipitation and drying a precipitate so as to obtain glycyrrhizic acid; and subjecting a supernatant produced after acid precipitation to concentration with the nanofiltration membrane device and carrying out drying so as to obtain the licorice flavoring agent. The method adopts membrane separation technology for impurity removal and concentration of the extract liquid, so working conditions are mild, product purity and quality are guaranteed, and yield of licorice effective ingredients is high; the method has the advantages of simple production flow, low cost, small pollution, reusability of a nanofiltration membrane filtrate generated in production process, reduction in consumption of raw water and great decrease of waste water discharge.
Description
Technical field
The invention belongs to Chinese herbal medicine extracting processing technology, relate generally to a kind of method of simultaneously extracting the effective ingredients such as Potenlini, licoflavone and liquorice flavor agent from Radix Glycyrrhizae.
Background technology
Radix Glycyrrhizae is perennial root draft, it is the traditional Chinese medicine material of China, the Tang Dynasty < < property of medicine book on Chinese herbal medicine > > is called " state is old ", has to be in harmonious proportion the effect of many medicines, more has the saying of " without grass Cheng Fang not ".China Radix Glycyrrhizae is distributed more widely, nearly 17 kinds of kinds.Radix Glycyrrhizae happiness light, cold-resistant, drought-enduring, Salt And Alkali Tolerance are mainly distributed in arid, the semiarid zone of the north and the northwestward in China, wherein Glycyrrhiza uralensis Fisch. is mainly distributed in Jilin, Liaoning, the Inner Mongol, Ningxia, Qinghai, Xinjiang; Beads Radix Glycyrrhizae and Coriolis Radix Glycyrrhizae are mainly distributed in In The Eastern Xinjiang and the north; Glycyrrhiza glabra is distribution and Gansu, Xinjiang mainly; Glycyrrhiza inflate bat is mainly distributed in the Inner Mongol, Gansu, Xinjiang.In Radix Glycyrrhizae, main medicinal ingredients is flavonoid, polyose, Potenlini and glycyrrhetinic acid, and abundant Licorice and effectively pharmacological action make the extraction of Radix Glycyrrhizae active substance and purifying become the focus of modernization of cmm now.
Radix Glycyrrhizae is as the exclusive resource of China, at Chinese herbal medicine industry or pharmaceutical industries, there is its unique status, at present, domestic Radix Glycyrrhizae is mainly with the concentrated Radix Glycyrrhizae extractum of making of poach, make again Licorice sell, after industrially-advanced country's under-buys such as Japan, made high-content, high-quality Potenlini, licoflavone is domestic to export back at high price.At present, domestic minority producer starts to produce 30% content Potenlini and 20～40% content licoflavones, has met part market, but more than 30% above Potenlini and 40% licoflavone does not have manufacturer production.
The current technology of domestic Potenlini production industry and the subject matter of existence are:
1, wastewater flow rate is large, waste water ph 1.5 left and right, and specific conductivity 20000 μ m/cm, COD is 1600mg/L left and right, biodegradability is poor, adopts traditional method for treating wastewater cannot reach discharging standards;
The active substance compositions such as the licoflavone 2, containing in Radix Glycyrrhizae, licorice polysaccharide, liquorice pigment, with discharge of wastewater, have wasted valuable natural resources;
3, Potenlini yield is on the low side, because contain the following Potenlini of saturation concentration in waste water, water displacement is larger, loses larger.
This technological method fully utilizes Radix Glycyrrhizae, not only can improve Potenlini yield, can also obtain licoflavone and liquorice flavor agent, wherein licoflavone is a kind of quick, efficient, green whitening cosmetics additive, also have restraint of tyrosinase activity, remove oxyradical, its resistance of oxidation and vitamin-E are more approaching.In liquorice flavor agent, contain licorice polysaccharide, liquorice pigment, a small amount of Potenlini isoreactivity material, can be used as the additive of cigarette and food, beverage industry, this technology especially can significantly reduce factory effluent, reduces the pollution to environment.The technology of the present invention route is simply without being used poisonous organic solvent, and production process safety and environmental protection, is suitable for scale operation, has significantly improved the overall availability of Radix Glycyrrhizae and obtained high value added product to produce good Social benefit and economic benefit.
Summary of the invention
In order to overcome problem and the defect of existing technique, the invention provides a kind of method of simultaneously extracting the effective ingredients such as Potenlini, licoflavone and liquorice flavor agent from Radix Glycyrrhizae.Present method be take Radix Glycyrrhizae as raw material, multiple useful matter in comprehensive utilization Radix Glycyrrhizae, shorten Production Flow Chart, reduce cost, reduce and pollute, produce the high-quality Potenlini of high purity, licoflavone and liquorice flavor agent simultaneously, production process safety and environmental protection, can not produce secondary pollution and a large amount of waste water.
Object of the present invention can realize by following technical proposals:
Fully utilize Radix Glycyrrhizae and extract a separated method of preparing Potenlini, licoflavone and liquorice flavor agent, comprise the steps:
A, take quantitative Radix Glycyrrhizae and pulverize;
B, the water of 5～9 times will be added by its quality in the Radix Glycyrrhizae of the pulverizing in a step, add ammoniacal liquor to regulate pH value to 8.0～9.0, stirring and leaching 3h～4h, isolate after licorice extract, add again the water with amount, and adding again ammoniacal liquor to regulate pH value to 8.0～9.0, stirring and leaching 1h～2h, can obtain respectively glycyrrhiza residue and licorice extract through separation;
C, by the glycyrrhiza residue obtaining in b step, by its quality, add the ethanol of 13～15 times, alcohol concn is 85%～95%, lixiviate 3h～4h stirs and puts 1h～2h, filters, and reclaims ethanol and obtains licoflavone crude product;
D, twice licorice extract obtaining in b step merged, adopt ultra-filtration membrane device to process, remove the impurity in material, obtain ultra-filtration membrane filtrate;
E, the ultra-filtration membrane filtrate employing nano filter membrance device obtaining in d step is concentrated, obtains nanofiltration membrane concentrated solution, and its nanofiltration membrane filtrate can be back to b step;
F, by the nanofiltration membrane concentrated solution obtaining in e step, the sulfuric acid that is 25% by concentration, pH value is adjusted to 2.0～3.0, and to carry out acid heavy, through separation, is precipitated respectively thing and supernatant liquor;
G, the supernatant liquor employing nano filter membrance device obtaining in f step is concentrated, obtains liquorice flavor agent after enriched material is dry;
H, the throw out obtaining in f step is obtained to Potenlini after drying.
In described step a, Radix Glycyrrhizae being pulverized, is in order to guarantee that follow-up lixiviate completes fully.
In described step b, adding ammoniacal liquor to regulate pH value, is the Potenlini stripping in order to allow in material.
In described step c, adding ethanol, is the flavones stripping in order to allow in material system.
Ultra-filtration membrane device in described steps d, its ultrafiltration membrance filter aperture is 20～50nm, the working conditions of ultra-filtration membrane device is: pressure 0.3～0. 5MPa, 35～50 ℃ of temperature.
Nano filter membrance device in described step e, its nanofiltration membrane pore size filter is 0.5～1.5nm, the working conditions of nano filter membrance device is: pressure 1.5～2.0MPa, 45～50 ℃ of temperature.
Nano filter membrance device in described step g, its nanofiltration membrane pore size filter is 0.5～1.5nm, the working conditions of nano filter membrance device is: pressure 1.5～2.0MPa, 45～50 ℃ of temperature.
The present invention compares with now having at present technique, has the following advantages:
The present invention be take Radix Glycyrrhizae as raw material, the multiple useful matter in comprehensive utilization Radix Glycyrrhizae, and a production line can obtain three kinds of active substances such as Potenlini, licoflavone and liquorice flavor agent by while manufacture.
The present invention uses membrane separation technique to carry out removal of impurities and concentrated to vat liquor, its working conditions is gentle, and Radix Glycyrrhizae effective ingredient yield is higher, in production process without chemical reaction, change without phase transformation, and do not bring other impurity into and cause the decomposition sex change of product, guaranteed purity and the quality of product.
Production Flow Chart of the present invention is simple, cost is low, it is little to pollute, and the nanofiltration membrane filtrate producing in production process can reuse, has reduced former water consumption and has significantly reduced wastewater discharge.
Embodiment
Below in conjunction with embodiment, the present invention will be described in detail:
Embodiment 1:
Taking 5kg Radix Glycyrrhizae pulverizes, the Radix Glycyrrhizae of pulverizing is added to 25kg water, add ammoniacal liquor to regulate pH value to 8.0, stirring and leaching 3h, by after vat liquor filtering separation, in solid-state system, again add 25kg water, and add again ammoniacal liquor to regulate pH value to 8.0, stirring and leaching 1h, can obtain respectively glycyrrhiza residue and licorice extract through separation.Then by glycyrrhiza residue quality, add the ethanol of 13 times, alcohol concn is 85%, and lixiviate 3h stirs and puts 1h, filters, and reclaims ethanol and obtains the about 200g of licoflavone crude product.Twice licorice extract merged, in temperature, it is 35 ℃, intake pressure is under the condition of 0.3 Mpa, the ultra-filtration membrane device removal of impurities that is 50nm with pore size filter, obtaining ultra-filtration membrane filtrate, is 45 ℃ by ultra-filtration membrane filtrate in temperature, and intake pressure is under the condition of 1.5 Mpa, the nano filter membrance device that is 0.5nm with pore size filter is concentrated, obtains nanofiltration membrane concentrated solution.To obtain nanofiltration membrane concentrated solution, selecting concentration is 25% sulfuric acid, pH regulator to 2.0 is carried out to acid heavy, obtains respectively 967g Potenlini and clear liquid.By the clear liquid obtaining, in temperature, be 45 ℃, under the condition that intake pressure is 1.5Mpa, the nano filter membrance device that is 1.5nm with pore size filter is concentrated, after being dried, obtains liquorice flavor agent 429g.
Embodiment 2:
Taking 5kg Radix Glycyrrhizae pulverizes, the Radix Glycyrrhizae of pulverizing is added to 35kg water, add ammoniacal liquor to regulate pH value to 8.5, stirring and leaching 3.5h, by after vat liquor filtering separation, in solid-state system, again add 35kg water, and add again ammoniacal liquor to regulate pH value to 8.5, stirring and leaching 1.5h, can obtain respectively glycyrrhiza residue and licorice extract through separation.Then by glycyrrhiza residue quality, add the ethanol of 14 times, alcohol concn is 90%, and lixiviate 3.5h stirs and puts 1.5h, filters, and reclaims ethanol and obtains the about 230g of licoflavone crude product.Twice licorice extract merged, in temperature, it is 40 ℃, intake pressure is under the condition of 0.4 Mpa, the ultra-filtration membrane device removal of impurities that is 30nm with pore size filter, obtaining ultra-filtration membrane filtrate, is 45 ℃ by ultra-filtration membrane filtrate in temperature, and intake pressure is under the condition of 1.7 Mpa, the nano filter membrance device that is 1.0nm with pore size filter is concentrated, obtains nanofiltration membrane concentrated solution.To obtain nanofiltration membrane concentrated solution, selecting concentration is 25% sulfuric acid, pH regulator to 2.5 is carried out to acid heavy, obtains respectively 995g Potenlini and clear liquid.By the clear liquid obtaining, in temperature, be 45 ℃, under the condition that intake pressure is 1.5Mpa, the nano filter membrance device that is 1.0nm with pore size filter is concentrated, after being dried, obtains liquorice flavor agent 463g.
Embodiment 3:
Taking 5kg Radix Glycyrrhizae pulverizes, the Radix Glycyrrhizae of pulverizing is added to 45kg water, add ammoniacal liquor to regulate pH value to 9.0, stirring and leaching 4h, by after vat liquor filtering separation, in solid-state system, again add 45kg water, and add again ammoniacal liquor to regulate pH value to 9.0, stirring and leaching 2h, can obtain respectively glycyrrhiza residue and licorice extract through separation.Then by glycyrrhiza residue quality, add the ethanol of 15 times, alcohol concn is 95%, and lixiviate 4h stirs and puts 2h, filters, and reclaims ethanol and obtains the about 250g of licoflavone crude product.Twice licorice extract merged, in temperature, it is 50 ℃, intake pressure is under the condition of 0.5 Mpa, the ultra-filtration membrane device removal of impurities that is 20nm with pore size filter, obtaining ultra-filtration membrane filtrate, is 50 ℃ by ultra-filtration membrane filtrate in temperature, under the condition that intake pressure is 2.0Mpa, the nano filter membrance device that is 0.5nm with pore size filter is concentrated, obtains nanofiltration membrane concentrated solution.To obtain nanofiltration membrane concentrated solution, selecting concentration is 25% sulfuric acid, pH regulator to 2.0 is carried out to acid heavy, obtains respectively 1102g Potenlini and clear liquid.By the clear liquid obtaining, in temperature, be 50 ℃, under the condition that intake pressure is 2.0Mpa, the nano filter membrance device that is 0.5nm with pore size filter is concentrated, after being dried, obtains liquorice flavor agent 504g.
Claims (4)
1. Radix Glycyrrhizae effective ingredient is extracted a method for preparation, it is characterized in that carrying out according to the following steps:
A, take quantitative Radix Glycyrrhizae and pulverize;
B, the water of 5～9 times will be added by its quality in the Radix Glycyrrhizae of the pulverizing in a step, add ammoniacal liquor to regulate pH value to 8.0～9.0, stirring and leaching 3h～4h, isolate after licorice extract, add again the water with amount, and adding again ammoniacal liquor to regulate pH value to 8.0～9.0, stirring and leaching 1h～2h, can obtain respectively glycyrrhiza residue and licorice extract through separation;
C, by the glycyrrhiza residue obtaining in b step, by its quality, add the ethanol of 13～15 times, alcohol concn is 85%～95%, lixiviate 3h～4h stirs and puts 1h～2h, filters, and reclaims ethanol and obtains licoflavone crude product;
D, twice licorice extract obtaining in b step merged, adopt ultra-filtration membrane device to process, remove the impurity in material, obtain ultra-filtration membrane filtrate;
E, the ultra-filtration membrane filtrate employing nano filter membrance device obtaining in d step is concentrated, obtains nanofiltration membrane concentrated solution, and its nanofiltration membrane filtrate can be back to b step;
F, by the nanofiltration membrane concentrated solution obtaining in e step, the sulfuric acid that is 25% by concentration, pH value is adjusted to 2.0～3.0, and to carry out acid heavy, through separation, is precipitated respectively thing and supernatant liquor;
G, the supernatant liquor employing nano filter membrance device obtaining in f step is concentrated, obtains liquorice flavor agent after enriched material is dry;
H, the throw out obtaining in f step is obtained to Potenlini after drying.
2. a kind of Radix Glycyrrhizae effective ingredient according to claim 1 is extracted the method for preparation, it is characterized in that: the ultra-filtration membrane device in described steps d, its ultrafiltration membrance filter aperture is 20～50nm, and the working conditions of ultra-filtration membrane device is: pressure 0.3～0. 5MPa, 35～50 ℃ of temperature.
3. a kind of Radix Glycyrrhizae effective ingredient according to claim 1 is extracted the method for preparation, it is characterized in that: the nano filter membrance device in described step e, its nanofiltration membrane pore size filter is 0.5～1.5nm, and the working conditions of nano filter membrance device is: pressure 1.5～2.0MPa, 45～50 ℃ of temperature.
4. a kind of Radix Glycyrrhizae effective ingredient according to claim 1 is extracted the method for preparation, it is characterized in that: the nano filter membrance device in described step g, its nanofiltration membrane pore size filter is 0.5～1.5nm, and the working conditions of nano filter membrance device is: pressure 1.5～2.0MPa, 45～50 ℃ of temperature.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104387793A (en) * | 2014-11-20 | 2015-03-04 | 云南中烟工业有限责任公司 | Preparation method of liquorice pigment and application in cigarettes |
| CN104387792A (en) * | 2014-10-30 | 2015-03-04 | 洛阳蓝斯利科技有限公司 | Production method for preparing licorice yellow pigment by glycyrrhizic acid supernatant liquid |
| CN104479033A (en) * | 2014-10-30 | 2015-04-01 | 洛阳蓝斯利科技有限公司 | Method for comprehensive separation extraction of glycyrrhizic acid, licoflavone and glycyrrhiza polysaccharide from licorice root |
| CN105777521A (en) * | 2016-05-11 | 2016-07-20 | 西安兴博凯生物科技有限责任公司 | Industrial separating and purifying method for licoflavone series monomer |
| CN108359020A (en) * | 2018-01-18 | 2018-08-03 | 新疆乌拉尔甘草开发有限责任公司 | A kind of isolation and purification method of Radix Glycyrrhizae Thick many candies |
| CN109553654A (en) * | 2019-02-25 | 2019-04-02 | 湖南华诚生物资源股份有限公司 | The method of glycyrrhizin, licoflavone and licorice polysaccharide is extracted from Radix Glycyrrhizae |
| CN111012821A (en) * | 2019-12-31 | 2020-04-17 | 北京德科瑞医药科技有限公司 | Method for extracting effective components from plant |
| CN111100181A (en) * | 2019-12-31 | 2020-05-05 | 中国医药健康产业股份有限公司 | Method for extracting glycyrrhizic acid crude product from liquorice |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387792A (en) * | 2014-10-30 | 2015-03-04 | 洛阳蓝斯利科技有限公司 | Production method for preparing licorice yellow pigment by glycyrrhizic acid supernatant liquid |
| CN104479033A (en) * | 2014-10-30 | 2015-04-01 | 洛阳蓝斯利科技有限公司 | Method for comprehensive separation extraction of glycyrrhizic acid, licoflavone and glycyrrhiza polysaccharide from licorice root |
| CN104387793A (en) * | 2014-11-20 | 2015-03-04 | 云南中烟工业有限责任公司 | Preparation method of liquorice pigment and application in cigarettes |
| CN105777521A (en) * | 2016-05-11 | 2016-07-20 | 西安兴博凯生物科技有限责任公司 | Industrial separating and purifying method for licoflavone series monomer |
| CN108359020A (en) * | 2018-01-18 | 2018-08-03 | 新疆乌拉尔甘草开发有限责任公司 | A kind of isolation and purification method of Radix Glycyrrhizae Thick many candies |
| CN109553654A (en) * | 2019-02-25 | 2019-04-02 | 湖南华诚生物资源股份有限公司 | The method of glycyrrhizin, licoflavone and licorice polysaccharide is extracted from Radix Glycyrrhizae |
| CN109553654B (en) * | 2019-02-25 | 2019-06-07 | 湖南华诚生物资源股份有限公司 | The method of glycyrrhizin, licoflavone and licorice polysaccharide is extracted from Radix Glycyrrhizae |
| CN111012821A (en) * | 2019-12-31 | 2020-04-17 | 北京德科瑞医药科技有限公司 | Method for extracting effective components from plant |
| CN111100181A (en) * | 2019-12-31 | 2020-05-05 | 中国医药健康产业股份有限公司 | Method for extracting glycyrrhizic acid crude product from liquorice |
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Application publication date: 20140806 |