CN104711301A - Icaritin preparation method - Google Patents
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Abstract
The invention provides an icaritin preparation method which comprises the following steps: a, performing the enzymatic hydrolysis reaction of an epimedium extract under the action of Beta-glycosidase; b, filtering an enzymatic hydrolysis reaction product obtained in step a; c, dissolving filter cake obtained after filtration into acetone; and d, adding water to an acetone solution, performing reflux dissolution, keeping the solution standing, performing filtration, and collecting a crystal substance to obtain icaritin. According to the icaritin preparation method, the yield of icaritin is up to 20% relative to the epimedium extract, and the purity of icaritin is up to 99.8%.
Description
Technical field
The present invention relates to a kind of preparation method of Icaritin, belong to field of medicaments.
Background technology
A Kelading, has another name called Icaritin, epimedium aglucone, and be the new effective monomer that extraction and isolation obtains from Chinese medicinal materials Herba Epimedii Herba Epimedii extract obtains through enzymatic conversion, its structure is as shown in the formula shown in (I):
The preparation method of this compound is disclosed in CN101302548B.The method is raw material with icarin, is hydrolyzed with beta-glucosidase, the centrifugal precipitation acetone solution obtained of hydrolysate, filters and obtains supernatant liquor.Again this supernatant liquor water is carried out recrystallization, obtain Icaritin sterling.
Be disclose a kind of method adopting naringinase to obtain epimedium aglucone from icarin in the Chinese patent of 201010517793.6 at application number, icarin standard substance are dissolved in alcohol solvent by the method, under 40-70 DEG C of condition, add naringinase carry out enzymolysis, obtain epimedium aglucone.
Be the preparation method disclosing a kind of epimedium aglucone in the Chinese patent of 200910184282.4 at application number, the method is raw material with Herba Epimedii, and by methanol extraction, the steps such as helicase hydrolysis obtain epimedium aglucone crude product.
But, with icarin in above preparation method, or with Herba Epimedii methanol extract for raw material carries out enzyme-squash techniqued Icaritin.With Herba Epimedii methanol extract for Icaritin prepared by raw material, what obtain is Icaritin crude product; Take icarin as raw material when preparing Icaritin, another composition epimedin in Herba Epimedii can not be converted into Icaritin.So, in above three kinds of methods, all there is enzymolysis low conversion rate, the defect that finished product impurity is many.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Icaritin, the Icaritin prepared by the method has the advantage that transformation efficiency is high, purity is high and impurity is few.
The invention provides a kind of preparation method of Icaritin, the method comprises the following steps:
A. first Herba Epimedii extract is carried out enzyme digestion reaction under the effect of beta-glycosidase;
B. the enzyme digestion reaction product then obtained by step a filters;
C. again by the filter cake acetone solution after filtration;
D. in acetone soln, add water, backflow is dissolved, and by solution left standstill, filters, collects crystallisate, obtain described Icaritin.
Preferably, in the Herba Epimedii extract in described step a, the mass content summation of icarin and epimedin is at least 5%.
Preferably, in described step a, Herba Epimedii extract being scattered in pH value is in the buffered soln of 3.5-7.5, and when temperature is elevated to 35-65 DEG C, under the effect of beta-glycosidase, carries out enzyme digestion reaction.
Preferably, described buffered soln is the Sodium phosphate dibasic-potassium primary phosphate of pH value 4.0-7.0, acetic acid-sodium acetate, phosphoric acid-sodium phosphate, citric acid-sodium citrate or Sodium phosphate dibasic-citric acid solution.
Most preferably, described volume of buffer solution/L and the quality of Herba Epimedii extract/Kg is than being 5-30:1.
Preferably, the enzyme digestion reaction time described in step a is 8-48 hour, and enzyme digestion reaction temperature is 35-65 DEG C.
Preferably, the Herba Epimedii extract in step a and the mass ratio of beta-glycosidase are 1-50:1.
More preferably, in step a, the mass ratio of Herba Epimedii extract and beta-glycosidase is 2-30:1.
Most preferably, in step a, the mass ratio of Herba Epimedii extract and beta-glycosidase is 5-20:1.
Preferably, in described step c, first by the filtration cakes torrefaction after filtering, then pulverize, then the filter cake after pulverizing is scattered in acetone solvent and is dissolved, the volume/L of acetone solvent is equivalent to pulverize the 2-20 of filter cake quality/Kg doubly, obtains acetone soln.
Preferably, in described steps d, the volume/L adding water in acetone soln is equivalent to the 2-20 of filter cake quality/Kg doubly, and described solution at room temperature leaves standstill.
Preferably, in described step a, Herba Epimedii extract, is obtained by ethonal extraction for raw material with Herba Epimedii Chinese medicinal materials.
Preferably, described alcohol solvent is ethanol water mixed solvent, the extract that ethanol water mixed solvent extraction Herba Epimedii Chinese medicinal materials obtains is first through concentrated, then adsorbed by macroporous resin column, carry out wash-out with the ethanol water solvent that water and volumetric concentration are 30%-100% respectively again, obtain the Herba Epimedii extract for enzyme digestion reaction.
Preferably, in described ethanol water mixed solvent, the volume ratio of second alcohol and water is 40:10-160, and the volume/L of mixed solvent is 4-20 times of Herba Epimedii Chinese medicinal materials quality/Kg, extracts 1-5 time altogether, each backflow 1-5 hour.
Preferably, described macroporous resin column is HPD-300 type macroporous resin column, in macroporous resin column absorption, first with the distilled water wash-out of 4-12 times amount column volume, the elution flow rate of distilled water be 1-2 times of column volume/hour, discard elutriant; Then with the ethanol water solvent washing column bed of the 20%-40% volumetric concentration of 4-10 times of column volume, ethanol water solvent flow velocity be 0.5-2 times of column volume/hour, discard elutriant; Again with the ethanol water solvent washing column bed of 4-10 times of column volume 45%-100% volumetric concentration, ethanol water solvent flow velocity be 0.5-2 times of column volume/hour, collect elutriant, reclaim ethanol and be also concentrated into thick paste, drying obtains described Herba Epimedii extract.
Beneficial effect of the present invention is: 1. the present invention take Herba Epimedii extract as raw material, not only the icarin in extract is converted into A Kela fixed, and it is fixed the epimedin in extract to be also converted into A Kela, takes full advantage of herb resource.2. Herba Epimedii extract of the present invention have employed beta-glycosidase in enzyme digestion reaction process, compared with existing naringinase, helicase, the transformation efficiency that beta-glycosidase hydrolysis Herba Epimedii extract generates A Kela fixed is higher, can reach 98%, follow-up purifying is more prone to.And polygalacturonase hydrolysis Herba Epimedii extract generates, and the fixed transformation efficiency of A Kela is the highest only reaches 90%; Secondly, it is faster that beta-glycosidase hydrolysis Herba Epimedii extract generates the fixed speed of response of A Kela, and reaction only needs within 10-18 hour, just to make transformation efficiency reach 98%.3. the present invention is in enzymolysis process, using buffering salt as solvent, make the volume of reaction solvent be the 5-15 of Herba Epimedii extract quality doubly, substantially increase production efficiency.In addition, the present invention is except with except acetone solution filter cake, also dilute acetone soln by water, because Icaritin itself is dissolved in acetone, water insoluble, utilize the character of dissolving each other between acetone and water simultaneously, effectively can remove the water-soluble impurity in Icaritin acetone soln, improve the purity of Icaritin, the purity of Icaritin reaches 99.8%.Icaritin after purification can reach more than 20% relative to the yield of Herba Epimedii extract.
Accompanying drawing explanation
First figure of Fig. 1 represents the high-efficient liquid phase chromatogram of the total flavones in embodiment 1 step 1.1 ethanol extract.
Second figure of Fig. 1 represents the high-efficient liquid phase chromatogram of total flavones in the ethanol extract after embodiment 1 step 1.2 purifying.
Fig. 2 represents the preparation flow of Herba Epimedii extract of the present invention.
Fig. 3 represents that A Kela determines the high-efficient liquid phase chromatogram of sterling.
Embodiment
Unless otherwise indicated, term " enzyme digestion reaction " herein refers to the hydrolysis reaction under enzyme effect.
Unless otherwise indicated, " Herba Epimedii extract " of term refers to the extract obtained by ethanol water solvent extraction Herba Epimedii herein, contains Icaritin at interior flavones ingredient and other compositions in extract.
Unless otherwise indicated, term " column volume " herein refers to the cumulative volume of macroporous resin column inner stuffing.
Unless otherwise indicated, the beta-glycosidase that term " beta-glycosidase " is herein Japanese Tian Ye company, trade name is Aromase H2.
Embodiment 1
1. the preparation of Herba Epimedii extract
1.1 extract
The present embodiment gradation is extracted except stem, and Folium Epimedii amounts to 490Kg, is rubbed broken, uses 14 times, the aqueous ethanolic solution refluxing extraction of 10 times amount (v/w) 40% volumetric concentration 2 times respectively, each 1 hour.Recovery ethanol without alcohol taste to extracting solution, detects the total flavones in this extracting solution by high performance liquid chromatography, sees first figure of accompanying drawing 1;
1.2 macroporous resin purification
Ethanol extraction step 1.1 obtained, after concentrated removal ethanol, uses macroporous resin purification.First use the distilled water wash-out macroporous resin column of macroporous resin column volume 8 times, the flow velocity of distilled water wash-out be 1 times of column volume/hour, after wash-out terminates, discard elutriant;
With macroporous resin column volume 6 times amount volumetric concentration 25% ethanol water solvent washing macroporous resin column bed, after wash-out terminates, discard elutriant;
It is the macroporous resin column in the ethanol water solvent washing step 2 of 70% by volumetric concentration, ethanol water solvent volume is 4 times of column volume, regulate ethanol water solvent flow velocity be 1 times of column volume/hour, collect elutriant now, be concentrated into thick paste, spraying dry, is ground into fine powder, sieves to obtain Herba Epimedii extract and amount to 9.8Kg.Herba Epimedii extract after the macroporous resin purification that above three-step approach obtains detects flavone component wherein by high performance liquid chromatography, sees second figure of Fig. 1.
Macroporous resin in the present embodiment is purchased from Hebei Bao En sorbing material company limited, and model is HPD-300 type.
High performance liquid chromatography (HPLC) condition: chromatographic column: C18 post; Moving phase: acetonitrile-water (wherein containing volume fraction is the trifluoroacetic acid of 0.0125%), gradient sees the following form 1, elution time 60min, flow velocity: 1.0mL/min, column temperature: 35 DEG C.UV-detector determined wavelength is respectively 254,272,320nm.
Table 1 solvent gradient elution table
Result shows: except the peak of appearance 3 minutes time is except solvent peak, goes out 22 minutes, 24 minutes, 46 minutes and 52 minutes the peak that peak is flavone component.
After macroporous resin purification, in Herba Epimedii extract, total flavones composition obtains effective enrichment, and in the Herba Epimedii extract wherein after purifying, the yield of total flavones reaches 2.0 ~ 10.0%.
2. enzyme digestion reaction prepares Icaritin
Take the above-mentioned Herba Epimedii extract 9.8Kg through macroporous resin purification, join in 196L0.5mol/L pH=4.7 acetic acid-sodium acetate buffer solution, stirring velocity is make it dissolve in 100rpm situation.Until system temperature constant 58-60 DEG C of condition time, add 2.0Kg beta-glycosidase stirring reaction.Isothermal reaction is after 28 hours, and stop stirring, reaction solution is cooled to 30 DEG C.
3. the purifying of Icaritin
After enzyme digestion reaction terminates, reaction solution carries out centrifugal, collects filter cake, after dry, weight is 7.59Kg, add 88.45Kg acetone after pulverizing, stir after 1 hour and filter, be warming up to 60 DEG C add 64.80Kg purified water in acetone soln after and system solvent refluxing is clarified to solution.After solution slow cooling to 4 DEG C, insulation 2 hours, filters, and collects filter cake and dry, obtains Icaritin crystallized product 1.96Kg, sees Fig. 3, went out at 20.403 minutes the peak that peak is Icaritin.
Embodiment 2
1. enzyme digestion reaction prepares Icaritin
Take commercial Herba Epimedii extract 10Kg, join in 100L pH=5.5 Sodium phosphate dibasic-citric acid solution, stirring velocity is make it dissolve in 100rpm situation.Until system temperature constant 57 DEG C of conditions time, add 1.5Kg beta-glycosidase stirring reaction.Isothermal reaction is after 16 hours, and stop stirring, reaction solution is cooled to 25 DEG C.
2. the purifying of Icaritin
After enzyme digestion reaction terminates, reaction solution carries out centrifugal, collects filter cake, after dry, weight is 7.85Kg, add 88.11Kg acetone after pulverizing, stir after 1 hour and filter, be warming up to 63 DEG C add 64.55Kg purified water in acetone soln after and system solvent refluxing is clarified to solution.Be incubated 2 hours after solution slow cooling to room temperature, filter, collect filter cake and drying, obtain Icaritin crystallized product 1.17Kg.
Embodiment 3
1. enzyme digestion reaction prepares Icaritin
Take commercial Herba Epimedii extract 8.7Kg, join in 174L pH=4.8 citric acid-sodium citrate buffer, stirring velocity is make it dissolve in 100rpm situation.Until system temperature constant 45 DEG C of conditions time, add 0.435Kg beta-glycosidase stirring reaction.Isothermal reaction is after 20 hours, and stop stirring, reaction solution is cooled to 30 DEG C.
2. the purifying of Icaritin
After enzyme digestion reaction terminates, reaction solution carries out centrifugal, collects filter cake, and after dry, weight is 6.55Kg, adds 76.34Kg acetone after pulverizing, stirs after 1 hour and filters, be warming up to 62 DEG C system solvent refluxing is clarified to solution in acetone soln after 55.93Kg purified water.After solution slow cooling to 25 DEG C, insulation 2 hours, filters, and collects filter cake and dry, obtains Icaritin crystallized product 1.01Kg.
Embodiment 4
1. enzyme digestion reaction prepares Icaritin
Take commercial Herba Epimedii extract 8.0Kg, join in 80L pH=6.0 phosphoric acid-buffer solution of sodium phosphate, stirring velocity is make it dissolve in 100rpm situation.Until system temperature constant 55 DEG C of conditions time, add 1.2Kg beta-glycosidase stirring reaction.Isothermal reaction is after 18 hours, and stop stirring, reaction solution is cooled to 25 DEG C.
2. the purifying of Icaritin
After enzyme digestion reaction terminates, reaction solution carries out centrifugal, collects filter cake, and after dry, weight is 6.23Kg, adds 73.25Kg acetone after pulverizing, stirs after 1 hour and filters, be warming up to 64 DEG C system solvent refluxing is clarified to solution in acetone soln after 53.66Kg purified water.After solution slow cooling to 25 DEG C, insulation 2 hours, filters, and collects filter cake and dry, obtains Icaritin crystallized product 1.12Kg.
Claims (10)
1. a preparation method for Icaritin, the method comprises the following steps:
A. first Herba Epimedii extract is carried out enzyme digestion reaction under the effect of beta-glycosidase;
B. the enzyme digestion reaction product then obtained by step a filters;
C. again by the filter cake acetone solution after filtration;
D. in acetone soln, add water, backflow is dissolved, and by solution left standstill, filters, collects crystallisate, obtain described Icaritin.
2. method according to claim 1, is characterized in that, in described step a, in Herba Epimedii extract, the mass content summation of icarin and epimedin is at least 5%.
3. method according to claim 1, is characterized in that, in described step a, Herba Epimedii extract being scattered in pH value is in the buffered soln of 3.5-7.5, and when temperature is elevated to 35-65 DEG C, under the effect of beta-glycosidase, carries out enzyme digestion reaction; Preferably, described buffered soln is the Sodium phosphate dibasic-potassium primary phosphate of pH value 4.0-7.0, acetic acid-sodium acetate buffer solution, phosphoric acid-sodium phosphate, citric acid-sodium citrate or Sodium phosphate dibasic-citric acid solution; Most preferably, described volume of buffer solution/L and the quality of Herba Epimedii extract/Kg is than being 5-30:1.
4. method according to claim 1, is characterized in that, the enzyme digestion reaction time described in step a is 8-48 hour, and enzyme digestion reaction temperature is 35-65 DEG C; Preferably, the Herba Epimedii extract in step a and the mass ratio of beta-glycosidase are 1-50:1; More preferably, in step a, the ratio of Herba Epimedii extract and beta-glycosidase is 2-30:1; Most preferably, in step a, the mass ratio of Herba Epimedii extract and beta-glycosidase is 5-20:1.
5. method according to claim 1, it is characterized in that, in described step c, first by the filtration cakes torrefaction after filtration, then pulverize, be scattered in acetone solvent by filter cake after pulverizing and dissolve, the volume/L of acetone solvent is equivalent to 2-20 times that pulverizes filter cake quality/Kg, obtains acetone soln.
6. method according to claim 1, is characterized in that, in described steps d, the volume/L adding water in acetone soln is equivalent to the 2-20 of filter cake quality/Kg doubly, and described solution at room temperature leaves standstill.
7. method according to claim 1, is characterized in that, in described step a, Herba Epimedii extract, is obtained by ethonal extraction for raw material with Herba Epimedii Chinese medicinal materials.
8. method according to claim 7, it is characterized in that, described alcohol solvent is ethanol water mixed solvent, the extract that ethanol water mixed solvent extraction Herba Epimedii Chinese medicinal materials obtains is first through concentrated, then adsorbed by macroporous resin column, carry out wash-out with the ethanol water solvent that water and volumetric concentration are 30%-100% respectively again, obtain the Herba Epimedii extract for enzyme digestion reaction.
9. method according to claim 8, in described ethanol water mixed solvent, the volume ratio of second alcohol and water is 40:10-160, and the volume/L of mixed solvent is 4-20 times of Herba Epimedii Chinese medicinal materials quality/Kg, extracts 1-5 time altogether, each backflow 1-5 hour.
10. method according to claim 8, described macroporous resin column is HPD-300 type macroporous resin column, in macroporous resin column absorption, first with the distilled water wash-out of 4-12 times amount column volume, the elution flow rate of distilled water be 1-2 times of column volume/hour, discard elutriant; Then with the ethanol water solvent washing column bed of the 20%-40% volumetric concentration of 4-10 times of column volume, ethanol water solvent flow velocity be 0.5-2 times of column volume/hour, discard elutriant; Again with the ethanol water solvent washing column bed of 4-10 times of column volume 45%-100% volumetric concentration, ethanol water solvent flow velocity be 0.5-2 times of column volume/hour, collect elutriant, reclaim ethanol and be also concentrated into thick paste, drying obtains described Herba Epimedii extract.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108558812A (en) * | 2018-03-26 | 2018-09-21 | 北京珅奥基医药科技有限公司 | A kind of method that acidolysis prepares icariine |
| CN110699263A (en) * | 2019-10-29 | 2020-01-17 | 浙江工业大学 | Aspergillus niger YH-6 and application thereof in improving content of icaritin in epimedium |
| CN111575330A (en) * | 2020-05-21 | 2020-08-25 | 成都蓓乐康生物科技有限公司 | Method for hydrolyzing epimedium extract by plant-derived enzyme |
| CN113355373A (en) * | 2021-06-29 | 2021-09-07 | 劲牌持正堂药业有限公司 | Preparation method of low polycyclic aromatic hydrocarbon icaritin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558812A (en) * | 2018-03-26 | 2018-09-21 | 北京珅奥基医药科技有限公司 | A kind of method that acidolysis prepares icariine |
| CN110699263A (en) * | 2019-10-29 | 2020-01-17 | 浙江工业大学 | Aspergillus niger YH-6 and application thereof in improving content of icaritin in epimedium |
| CN111575330A (en) * | 2020-05-21 | 2020-08-25 | 成都蓓乐康生物科技有限公司 | Method for hydrolyzing epimedium extract by plant-derived enzyme |
| CN111575330B (en) * | 2020-05-21 | 2022-04-15 | 成都蓓乐康生物科技有限公司 | Method for hydrolyzing epimedium extract by plant-derived enzyme |
| CN113355373A (en) * | 2021-06-29 | 2021-09-07 | 劲牌持正堂药业有限公司 | Preparation method of low polycyclic aromatic hydrocarbon icaritin |
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Address after: 100085 A201 room, No. 5, Pioneer Road, Beijing, Haidian District Patentee after: Beijing shengnuoji Pharmaceutical Technology Co., Ltd Address before: 100085 A201 room, No. 5, Pioneer Road, Beijing, Haidian District Patentee before: Beijing Shengnuoji Medicine Technology Co., Ltd. |