CN103833806A - Preparation method of traditional Chinese medicine chemical component - Google Patents
Preparation method of traditional Chinese medicine chemical component Download PDFInfo
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Abstract
The invention relates to a separation of a natural chemical component, and in particular to a method for extracting high-purity liquiritin from licorice medicinal material. The method mainly comprises the following steps: adding a proper amount of dilute ethanol into a licorice powder for extraction; concentrating the extract or percolating liquid; adding a proper amount of water for dissolution; filtering; separating by macroporous adsorption resin to obtain a liquiritin crude product; adding a proper amount of a solvent; heating for dissolving; filtering; standing for crystallization; filtering; and drying to obtain high-purity liquiritin. The product is determined by high performance liquid chromatography to have purity higher than 95%. The liquiritin produced by the technical scheme of the invention has high purity and large preparation volume; and the method has low cost, and stable and reliable process, and is especially suitable for separating and preparing of a large amount of high-purity liquiritin compound from the traditional Chinese medicine licorice.
Description
Technical field
The invention belongs to medical technical field, be specifically related to a kind of method of extracting the high-purity liquorice glycosides preparing from licorice medicinal materials.
Background technology
Radix Glycyrrhizae is the root and rhizome of pulse family (Leguminosae) Glycyrrhiza (Glycyrrhiza Linn.) plant Glycyrrhiza uralensis Fisch., glycyrrhiza glabra, glycyrrhiza inflate bat, distributes all over global each continent.Radix Glycyrrhizae is used as medicine with a long history, and Shennong's Herbal is classified as on medicine and taken advantage of, have invigorate the spleen and benefit qi, effect of clearing heat and detoxicating, expelling phlegm for arresting cough, relieving spasm to stop pain, coordinating the actions of various ingredients in a prescription.Radix Glycyrrhizae chemical composition kind is more, mainly containing compositions such as triterpenes saponins and flavonoids.Liquirtin is the main component in Radix Glycyrrhizae total flavones, is activeconstituents main in Radix Glycyrrhizae, has the effects such as antidepressant, anti-oxidant, anti-arrhythmia, antiulcer agent, anticancer, anti-cancer, preventing tumor, has good DEVELOPMENT PROSPECT.At present, flavones in relevant Radix Glycyrrhizae, the preparation method's of liquirtin composition patent is more.
Liquirtin structural formula
China Pharmaceutical Research & Development Center Co., Ltd has applied for the patent (application number is 200310115114.2) that a key name is " extracting the method for licoflavone in a kind of glycyrrhiza residue ", this patent technique mainly adopts organic solvent extraction, resin column chromatography, the technology such as dry, the product obtaining is Radix Glycyrrhizae total flavones mixture, and liquirtin content is low.
Shi Renbing etc. have applied for the patent (application number is 200710111227.3) that a key name is " Radix Glycyrrhizae total flavones and total saponin extracts and preparation method thereof ", this patent technique mainly adopts any one methods such as solvent-extraction process, solvent extration, Amberlyst process, lead salt precipitation, column chromatography, liquid-liquid adverse current partition chromatography, or the arbitrary combination of these methods prepares Radix Glycyrrhizae total flavones and total saponin extracts.This patent adopts solvent extration, column chromatography step, and complex steps and the finished product liquirtin content are low, has the different of essence from the target product in the present invention.
Dalian Inst of Chemicophysics, Chinese Academy of Sciences has applied for the patent (application number 200710011041.0) that a key name is " a kind of preparation method of liquirtin ", this patent technique is after licorice medicinal materials water extract-alcohol precipitation, elder generation, to separate through molecular weight membrane sepn instrument, macroporous resin, efficient industrial chromatography post, lyophilize obtains liquirtin, this complex process, high to equipment requirements, complicated operation, is not suitable for a large amount of production.The patent (application number is 201110287907.7) of Tianjin spike Natural products research development corporation, Ltd. application one " extracting the method for liquirtin from Radix Glycyrrhizae ", for upper hybrid resin after water extraction separate recrystallize method, separating the filler that adopts is the mixture of polymeric amide, resin, separate filler complexity used, and polymeric amide is frangible, should not reuse unsuitable industrial applications.
In sum, technique required high, complicated operation, product content low to plant and instrument in the past, was unfavorable for industrialized production.The present invention utilizes modernization of Chinese medicine separating and purifying technology, overcomes the deficiency of technique in the past, taking licorice medicinal materials as raw material, prepares a kind of highly purified liquirtin.Adopt Diluted Alcohol heating to extract or diacolation, after extracting solution is concentrated, be dissolved in water, then by macroporous resin column, Diluted Alcohol wash-out obtains liquirtin crude product, after crystallization treatment, thereby obtains that a kind of content is high, good stability, liquirtin that cost is low.New technology of the present invention, easy and simple to handle, energy-conserving and environment-protective, have good practicality, there is no at present Patents or bibliographical information.
Summary of the invention
The object of this invention is to provide a kind of high-purity liquorice glycosides that obtains from licorice medicinal materials, and a kind of easy, favorable reproducibility, be applicable to the method for preparation of industrialization high-purity liquorice glycosides.
For achieving the above object, the technical solution used in the present invention is:
(l) extracting Radix Glycyrrhizae medicinal material, pulverizes, and adds aqueous ethanolic solution to extract, and extracting solution is concentrated, adds suitable quantity of water heating for dissolving, filtration, obtains filtrate;
(2) by filtrate, cross macroporous adsorbent resin and separate, wash with water to colourless, then use ethanolic soln wash-out, collect ethanol eluate concentrated, place crystallization, obtain liquirtin crude product;
(3) get above-mentioned liquirtin crude product, add appropriate organic solvent, heating for dissolving, filters, and places crystallization, filters, dry, obtains liquirtin.
Be preferably:
(l) extracting Radix Glycyrrhizae medicinal material, pulverizes as meal, and with 30～80% aqueous ethanolic solutions extractions, extracting solution concentrating under reduced pressure, adds 2～5 times of water gaging heating for dissolving, filtration, obtains filtrate;
(2) by filtrate, crossing macroporous adsorbent resin separates, wash with water, be washed till elutriant closely colourless, and then with 3～7 times of volumes, 20%～50% ethanolic soln wash-out, collect ethanol eluate concentrating under reduced pressure, place crystallization, filter, and with a small amount of 20% ethanol water liquid drip washing, dry, obtain liquirtin crude product.
(3) get above-mentioned liquirtin crude product, add the mixing solutions of ethanol, methyl alcohol, acetone or alcohol, methyl alcohol, acetone and water, heating for dissolving, filters, and places crystallization, filters, dry, obtains purity higher than 95% liquirtin.
More preferably:
(l) extracting Radix Glycyrrhizae medicinal material, pulverizes as meal, uses 60% aqueous ethanolic solution, adopts heating reflux method to extract, and consumption is 14 times of licorice medicinal materials amount, and extracting solution concentrating under reduced pressure adds 4 times of water gaging heating for dissolving, filtration, obtains filtrate;
(2) by filtrate, cross macroporous adsorbent resin and separate, wash with water, be washed till elutriant closely colourless, and then with 4 times of volumes, 30% ethanolic soln wash-out, collect ethanol eluate concentrating under reduced pressure, and place crystallization, filter, and with a small amount of 20% ethanol water liquid drip washing, dry, obtain liquirtin crude product.
(3) get above-mentioned liquirtin crude product, add 60% acetone or 60% aqueous ethanolic solution, heating for dissolving, filters, and places crystallization, filters, dry, obtains purity higher than 95% liquirtin.
In above-mentioned steps (1), the concentration of ethanol is preferably 60% ethanol; Consumption is 12～18 times of licorice medicinal materials amount, more preferably 14 times of amounts; Extract and preferably adopt heating and refluxing extraction, insufficient because the too low meeting of temperature makes to extract, can extract one or many, extraction time is 1～3 hour, is preferably 2 hours; Extracting solution is concentrated into relative density and is preferably 1.05～1.15 (60 DEG C); Add 2～5 times of water dissolution, be preferably 4 times, water too thickness of solution very little, crosses column resistance large, and solution upper column quantity is too large too much for water, and the production cycle is long; Heating for dissolving, filters while hot, and filtrate is for subsequent use; Liquirtin solubleness in hot water is large.
In above-mentioned steps (2), macroporous resin used comprises polar macroporous adsorption resin, intermediate-polarity macroporous adsorption resin, nonpolar macroporous adsorption resin.The model of macroporous resin is HPD300(Cangzhou Bao En Chemical Co., Ltd.), HPD600(Cangzhou Bao En Chemical Co., Ltd.), Cangzhou Weiyuan Chemical Co., Ltd. of YDW-03G1(China), Cangzhou Weiyuan Chemical Co., Ltd. of YDW-04(China) pass through applied sample amount, samples contg, the Integrated Selection contrast of the each side factors such as sample yield, preferably YDW-04 model macroporous resin is best, after upper prop completes, wash the impurity that polarity is large, then use a certain proportion of ethanol elution, by yield and the content thereof of Comprehensive Assessment sample, the concentration of determining elutriant ethanol is 20%～50%, be preferably 30%, eluting solvent consumption is 3～7 times of amounts of cylinder accumulated amount, is preferably 4 times of amounts, because excessive wash-out, can increase impurity level, reduce the purity of liquirtin, collecting the another device collection of 30% elutriant, 1 times of elutriant originally, rear 2～5 times of elutriants are collected together, the preferred technical scheme according to the present invention,, can select according to the needs of actual production without particular requirement chromatography column used, Diluted Alcohol elutriant concentrating under reduced pressure temperature is 60～75 DEG C, is preferably 70 DEG C, what elutriant was evaporated to effluent volume is 0.4～0.8 times of charging capacity, preferably 0.5 times, volume is excessive be difficult for crystallization or yield too low, volume too small impure too much, shade deviation, Tc is room temperature, crystallization time can be 20～48 hours, is preferably 30 hours, and the too short crystallization of crystallization time is incomplete.
In above-mentioned steps (3), crystallization solvent used can be ethanol, methyl alcohol, acetone and the mixed solvents at different levels with water thereof, is preferably 60% acetone or 60% aqueous ethanolic solution; In experimental study, 17%, 33%, 40%, 50%, 60%, 78%, 95% ethanol, dehydrated alcohol, methyl alcohol, acetone, 60% methyl alcohol, 60% acetone equal solvent are considered to comparison from crystallization purity, yield etc., when discovery solvent adopts 60% ethanol and 60% acetone, crystallization purity is high, and yield is higher than 80%.Solvent load is 15～25 times of amounts (g/mL) of thick liquirtin, is preferably 20 times of amounts, and solvent load is excessive is difficult for crystallization or yield is too low, and the too small content of consumption reduces; Tc is room temperature, is preferably 20 DEG C; Crystallization time is 20～36 hours, is preferably 24 hours.
The purity test of above-mentioned liquirtin adopts high performance liquid chromatography (HPLC) method, adopts HPLC method to be: chromatographic column: taking octadecylsilane chemically bonded silica as packing material in test; Moving phase acetonitrile-0.03% phosphate aqueous solution (20:80); Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Detect wavelength and adopt diode-array detector 200～400nm all-wave long, preferably 230nm and 276nm; Theoretical plate number is pressed liquirtin peak and is calculated, and should be not less than 6000.Sample purity inspection collection of illustrative plates is shown in attached, Fig. 1～Fig. 4, and the liquirtin of measuring, purity is higher than 95%.
According to technical scheme of the present invention, the feasible method of employing science from licorice medicinal materials through with Diluted Alcohol refluxing extraction, concentrated, cross the series of steps such as resin column, crystallization, recrystallization, the liquirtin content making, more than 95%, reaches as high as 99%.Compared with preparation technology's patent before, have advantages of energy-conserving and environment-protective, production cost low, easy and simple to handle, can suitability for industrialized production.Preparation technology of the present invention produces checking by many batches, proves that its repeatability, stability are all good, is applicable to suitability for industrialized production, is easy to promote, and has very strong practicality.
The present invention has the following advantages:
Sample purity is high: the product purity of macroporous resin elutriant primary crystallization of the present invention reaches 90%, and the product purity of secondary crystal reaches more than 95%.
Favorable reproducibility: technique of the present invention is simple, to equipment require lowly, can ensure circulation ratio and stability prepared by liquirtin.
Be applicable to suitability for industrialized production: the technique that the present invention adopts is simple, to equipment require lowly, easily realize stdn, be suitable for industrialization scale operation.
figure of description
Fig. 1 liquirtin HPLC collection of illustrative plates;
The three-dimensional HPLC collection of illustrative plates of Fig. 2 liquirtin DAD;
Fig. 3 methanol solvate HPLC collection of illustrative plates;
The three-dimensional HPLC collection of illustrative plates of Fig. 4 methanol solvate DAD;
Liquirtin purity detecting HPLC collection of illustrative plates in Fig. 5 embodiment 1;
Liquirtin purity detecting HPLC collection of illustrative plates in Fig. 6 embodiment 2;
Liquirtin purity detecting HPLC collection of illustrative plates in Fig. 7 embodiment 3;
Liquirtin purity detecting HPLC collection of illustrative plates in Fig. 8 embodiment 4;
Liquirtin purity detecting HPLC collection of illustrative plates in Fig. 9 embodiment 5;
Liquirtin purity detecting HPLC collection of illustrative plates in Figure 10 embodiment 6.
Embodiment
In following examples, licorice medicinal materials used is purchased from Tianjin Medical Herb Pieces Factory, and assay is with reference substance all purchased from Nat'l Pharmaceutical & Biological Products Control Institute, and ethanol used is pharmaceutical grade, and water is purified water, and other solvents are analytical pure.
embodiment 1
(1) extracting Radix Glycyrrhizae medicinal material 15Kg, pulverizes, and uses 60% aqueous ethanolic solution, heating and refluxing extraction 2 times, adds 120L for the first time, extracts 2 hours, for the second time, 90L, refluxing extraction 1 hour, filter, it is the clear cream of 1.05 (60 DEG C) that extracting solution is evaporated to relative density, heavy 10.5kg, 40L adds water in clear cream, heating for dissolving, filters, and obtains filtrate.
(2), by filtrate, crossing diameter is 20cm YDW-04 type macroporous adsorptive resins, washes with water, be washed till elutriant closely colourless, and then with 5 times of column volumes, 30% ethanolic soln wash-out, collect 30% ethanol eluate, and be evaporated to small volume (8L), room temperature is placed 30 hours, separate out white crystals, filter, and with a small amount of 20% ethanol water liquid drip washing, dry, obtain liquirtin crude product 140.6g.
(3) get above-mentioned liquirtin crude product, add 3L 60% acetone-water mixed solvent, heat 80 DEG C of dissolvings, filter, place 30 DEG C of crystallizations, filter, dry, obtain high-purity liquorice glycosides.
Measure through HPLC, in color atlas (Fig. 5), have no other impurity peaks, this batch of liquirtin content is 98.7%.
embodiment 2
(1) extracting Radix Glycyrrhizae medicinal material, pulverizes, by 15 times of 60% aqueous ethanolic solution heating and refluxing extraction 2 times, 8 times of amounts for the first time, extract 7 times for the second time 2 hours, extract 1 hour, filter, it is the clear cream of 1.09 (60 DEG C) that extracting solution is evaporated to relative density, heavy 11.5kg, 4 times of amounts add water in clear cream, heating for dissolving, filters, and obtains filtrate.
(2), by filtrate, crossing diameter is HPD300 macroporous adsorptive resins, washes with water, be washed till elutriant closely colourless, and then with 50L volume 40% ethanolic soln wash-out, collect 40% ethanol eluate, and be evaporated to small volume (6L), room temperature is placed 20 hours, separate out white crystals, filter, and with a small amount of 20% ethanol water liquid drip washing, dry, obtain liquirtin crude product.
(3) get above-mentioned liquirtin crude product, add 5L 60% ethanol-water mixed solvent, heat 80 DEG C of dissolvings, filter, place 20 DEG C of crystallizations, filter, dry, obtain high-purity liquorice glycosides.
Measure through HPLC, in color atlas (Fig. 6), have no other impurity peaks, this batch of liquirtin content is 98.2%.
embodiment 3
(1) extracting Radix Glycyrrhizae medicinal material 15Kg, pulverizes, and uses 30% aqueous ethanolic solution, heating and refluxing extraction 2 times, adds 120L for the first time, extracts 2 hours, for the second time, 90L, refluxing extraction 1 hour, filter, it is the clear cream of 1.15 (60 DEG C) that extracting solution is evaporated to relative density, heavy 10.5kg, 40L adds water in clear cream, heating for dissolving, filters, and obtains filtrate.
(2), by filtrate, crossing diameter is 20cm YDW-04 macroporous adsorptive resins, washes with water, be washed till elutriant closely colourless, and then with 40L volume 25% ethanolic soln wash-out, collect 25% ethanol eluate, and be evaporated to small volume (8L), room temperature is placed 30 hours, separate out white crystals, filter, and with a small amount of 20% ethanol water liquid drip washing, dry, obtain liquirtin crude product 140.6g.
(3) get above-mentioned liquirtin crude product, add 3L40% acetone-water mixed solvent, heat 80 DEG C of dissolvings, filter, place 15 DEG C of crystallizations, filter, dry, obtain high-purity liquorice glycosides.
Measure through HPLC, in color atlas (Fig. 7), have no other impurity peaks, this batch of liquirtin content is 96.7%.
embodiment 4
(1) extracting Radix Glycyrrhizae medicinal material 20Kg, pulverizes, with 16 times of 70% aqueous ethanolic solution, heating and refluxing extraction 2 times,, extracts 2 hours by 9 times for the first time, for the second time, 7 times, extract 1 hour, filter, it is the clear cream of 1.11 (60 DEG C) that extracting solution is evaporated to relative density, heavy 14.5kg, 50L adds water in clear cream, heating for dissolving, filters, and obtains filtrate.
(2), by filtrate, crossing diameter is 20cm YDW-03G1 type macroporous adsorptive resins, washes with water, be washed till elutriant closely colourless, and then with 60L volume 50% ethanolic soln wash-out, collect 50% ethanol eluate, and be evaporated to small volume (9L), room temperature is placed 30 hours, separates out white crystals, filters, and with a small amount of 20% ethanol water liquid drip washing, dry, obtain liquirtin crude product, 151.1g.
(3) get above-mentioned liquirtin crude product, add 6L 50% ethanol-water mixed solvent, heat 80 DEG C of dissolvings, filter, place 10 DEG C of crystallizations, filter, dry, obtain high-purity liquorice glycosides.
Measure through HPLC, in color atlas (Fig. 8), have no other impurity peaks, this batch of liquirtin content is 97.8%.
embodiment 5
(1) extracting Radix Glycyrrhizae medicinal material 10Kg, pulverizes, and by 14 times of 50% aqueous ethanolic solution, heating and refluxing extraction 2 times, 8 times for the first time, extracts 2 hours; For the second time, 6 times, refluxing extraction 1 hour, filters, and it is the clear cream of 1.08 (60 DEG C) that extracting solution is evaporated to relative density, heavy 7.5kg, and the 25L that adds water in clear cream, heating for dissolving, filters, and obtains filtrate.
(2) by filtrate, cross YDW-04 macroporous adsorptive resins, wash with water, be washed till elutriant closely colourless, and then with 30L volume 40% ethanolic soln wash-out, collect 40% ethanol eluate, and be evaporated to small volume (6L), room temperature is placed 36 hours, separate out white crystals, filter, and with a small amount of 30% ethanol water liquid drip washing, dry, obtain liquirtin crude product.98.16g。
(3) get above-mentioned liquirtin crude product, add 2.5L 70% acetone-water mixed solvent, heat 80 DEG C of dissolvings, filter, place 4 DEG C of crystallizations, filter, dry, obtain high-purity liquorice glycosides.
Measure through HPLC, in color atlas (Fig. 9), have no other impurity peaks, this batch of liquirtin content is 99.7%.
embodiment 6
(1) extracting Radix Glycyrrhizae medicinal material 20Kg, pulverizes, and by 18 times of 80% aqueous ethanolic solution, heating and refluxing extraction 2 times, 10 times for the first time, extracts 2 hours; For the second time, 8 times, refluxing extraction 1 hour, filters, and it is the clear cream of 1.12 (60 DEG C) that extracting solution is evaporated to relative density, heavy 15.5kg, and the 60L that adds water in clear cream, heating for dissolving, filters, and obtains filtrate.
(2) by filtrate, cross YDW-04 macroporous adsorptive resins, wash with water, be washed till elutriant closely colourless, and then with 60L volume 20% ethanolic soln wash-out, collect 20% ethanol eluate, and be evaporated to small volume (10L), room temperature is placed 48 hours, separate out white crystals, filter, and with a small amount of 20% ethanol water liquid drip washing, dry, obtain liquirtin crude product.98.16g。
(3) get above-mentioned liquirtin crude product, add 2.5L 70% ethanol-water mixed solvent, heat 80 DEG C of dissolvings, filter, place 20 DEG C of crystallizations, filter, dry, obtain high-purity liquorice glycosides.
Measure through HPLC, in color atlas (Figure 10), have no other impurity peaks, this batch of liquirtin content is 97.5%.
Claims (10)
1. from licorice medicinal materials, extract a method of preparing liquirtin, it is characterized in that: comprise the following steps:
(l) extracting Radix Glycyrrhizae medicinal material, pulverizes, and adds aqueous ethanolic solution to extract, and extracting solution is concentrated; Be dissolved in water, filter, obtain filtrate;
(2) by step (1) gained filtrate, cross macroporous adsorbent resin and separate, wash with water to colourless, then use ethanolic soln wash-out, collect ethanol eluate concentrated, place crystallization, obtain liquirtin crude product;
(3) get above-mentioned liquirtin crude product, add organic solvent, heating for dissolving, filters, and places crystallization, filters, dry, obtains liquirtin.
2. preparation method according to claim 1, is characterized in that: comprise the following steps:
(l) extracting Radix Glycyrrhizae medicinal material, pulverizes as meal, adds 30～80% aqueous ethanolic solutions to extract, extracting solution concentrating under reduced pressure; Add 2～5 times of water gaging heating for dissolving, filtration, obtain filtrate; Described extracting method can soak method, thermal backflow, percolation for temperature; Described aqueous ethanolic solution consumption is 12～18 times of licorice medicinal materials amount;
(2) by step (1) gained filtrate, cross macroporous adsorbent resin and separate, wash with water to colourless, then use 3～7 times of volumes, 20%～50% ethanolic soln wash-out, collect ethanol eluate concentrated, place crystallization, filter, dry, obtain liquirtin crude product;
(3) get above-mentioned liquirtin crude product, add the mixing solutions of ethanol, methyl alcohol, acetone or alcohol, methyl alcohol, acetone and water, heating for dissolving, filters, and places crystallization, filters, dry, obtains liquirtin.
3. preparation method according to claim 2, is characterized in that: comprise the following steps:
(l) extracting Radix Glycyrrhizae medicinal material, pulverizes as meal, adds 60% aqueous ethanolic solution, adopts heating reflux method to extract, and aqueous ethanolic solution consumption is 14 times of licorice medicinal materials amount, and it is 1.05～1.15 that extracting solution is evaporated to relative density; Add 4 times of water gaging heating for dissolving, filtration, obtain filtrate;
(2) by filtrate, cross macroporous adsorbent resin and separate, wash with water to colourless, then use 4 times of volumes, 30% ethanolic soln wash-out, collect ethanol eluate concentrated, place crystallization, filter, dry, obtain liquirtin crude product;
(3) get above-mentioned liquirtin crude product, add 60% acetone or 60% aqueous ethanolic solution, heating for dissolving, filters, and places crystallization, filters, dry, obtains liquirtin.
4. according to the preparation method described in claim 1-3 any one, it is characterized in that: described step (1) is extracted as extraction one or many; Described extraction time is 1～3 hour, is preferably 2 hours.
5. according to the preparation method described in claim 1-3 any one, it is characterized in that: the macroporous resin in described step (2) comprises polar macroporous adsorption resin, intermediate-polarity macroporous adsorption resin, nonpolar macroporous adsorption resin.
6. preparation method according to claim 5, is characterized in that: the macroporous resin in described step (2) is HPD300, HPD600, YDW-03G1, YDW-04 type macroporous adsorbent resin; Be preferably YDW-04.
7. according to the preparation method described in claim 1-3 any one, it is characterized in that: in described step (2), crystallization time is 20～48 hours, is preferably 30 hours.
8. according to the preparation method described in claim 1-3 any one, it is characterized in that: the recrystallisation solvent consumption in described step (3) is 10～25 times (g/mL) of liquirtin crude product, is preferably 20 times (g/mL).
9. according to the preparation method described in claim 1-3 any one, it is characterized in that: in described step (3), heating for dissolving temperature is 80 DEG C, and Tc is 30 DEG C～4 DEG C.
10. according to the preparation method described in claim 1-3 any one, it is characterized in that: described step (3) crystallization time is 20～36 hours, is preferably 24 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112094306A (en) * | 2020-11-18 | 2020-12-18 | 大湾汉唯(广州)医药科技集团有限公司 | An extract containing liquiritin and its preparation method |
| CN113666977A (en) * | 2021-08-17 | 2021-11-19 | 甘肃亚兰药业有限公司 | Production process for combined separation of multiple active ingredients of liquorice |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544449A (en) * | 2003-11-21 | 2004-11-10 | 中国医药研究开发中心有限公司 | Licorice flavone extracting method from licorice dregs |
| CN1865273A (en) * | 2005-05-16 | 2006-11-22 | 厦门倍尔思生化科技有限公司 | Method for extracting multiple liquorice flavone form liquorice |
| CN101073595A (en) * | 2007-06-18 | 2007-11-21 | 石任兵 | Glycyrrhiza total flavonoid and total saponin extract and its production |
| CN101289480A (en) * | 2007-04-20 | 2008-10-22 | 中国科学院大连化学物理研究所 | Method for separating and preparing liquiritin |
| CN102336791A (en) * | 2011-09-27 | 2012-02-01 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting isoliquiritin from licorice root |
| CN102391330A (en) * | 2011-09-26 | 2012-03-28 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting liquiritin from liquorice |
| CN102633895A (en) * | 2012-04-19 | 2012-08-15 | 南京中医药大学 | Extraction and preparation method by comprehensively utilizing liquorice |
-
2012
- 2012-11-22 CN CN201210479494.7A patent/CN103833806A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544449A (en) * | 2003-11-21 | 2004-11-10 | 中国医药研究开发中心有限公司 | Licorice flavone extracting method from licorice dregs |
| CN1865273A (en) * | 2005-05-16 | 2006-11-22 | 厦门倍尔思生化科技有限公司 | Method for extracting multiple liquorice flavone form liquorice |
| CN101289480A (en) * | 2007-04-20 | 2008-10-22 | 中国科学院大连化学物理研究所 | Method for separating and preparing liquiritin |
| CN101073595A (en) * | 2007-06-18 | 2007-11-21 | 石任兵 | Glycyrrhiza total flavonoid and total saponin extract and its production |
| CN102391330A (en) * | 2011-09-26 | 2012-03-28 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting liquiritin from liquorice |
| CN102336791A (en) * | 2011-09-27 | 2012-02-01 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting isoliquiritin from licorice root |
| CN102633895A (en) * | 2012-04-19 | 2012-08-15 | 南京中医药大学 | Extraction and preparation method by comprehensively utilizing liquorice |
Non-Patent Citations (6)
| Title |
|---|
| 何明珍等，: "甘草中甘草苷、异甘草苷对照品的制备及鉴定.", 《江西中医学院学报》 * |
| 冯月等，: "甘草酸及甘草苷的提取纯化方法和药理作用研究进展", 《人参研究》 * |
| 吕子明等，: "甘草总黄酮的大孔吸附树脂纯化工艺优选.", 《中国实验方剂学杂志》 * |
| 方玉婷等，: "大孔吸附树脂法分离精制芍药甘草汤.", 《现代中药研究与实践》 * |
| 苏国林等，: "甘草苷的提取纯化方法和药理作用研究进展.", 《中国现代中药》 * |
| 韩涛等，: "大孔吸附树脂纯化三七和甘草药材有效成分的工艺研究.", 《中药与天然药物》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094306A (en) * | 2020-11-18 | 2020-12-18 | 大湾汉唯(广州)医药科技集团有限公司 | An extract containing liquiritin and its preparation method |
| CN112094306B (en) * | 2020-11-18 | 2021-03-09 | 大湾汉唯(广州)医药科技集团有限公司 | An extract containing liquiritin and its preparation method |
| CN113666977A (en) * | 2021-08-17 | 2021-11-19 | 甘肃亚兰药业有限公司 | Production process for combined separation of multiple active ingredients of liquorice |
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