CN103305564A - Method for converting icariin to herba epimedii - Google Patents
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Abstract
The invention relates to a method for converting icariin to herba epimedii. The method comprises the following steps of: 1) performing enzymatic hydrolysis, specifically, 1.1) preparing resin adsorbed with icariin; 1.2) preparing an enzymatic dispersion solution; 1.3) adding the resin prepared in the step 1.1) in the enzymatic dispersion solution in the step 1.2) to form a reaction solution, and performing enzymatic hydrolysis in the condition of heating in water bath at 40-50 DEG C; 1.4) standing the reaction solution formed in the step 1.3) to room temperature, adding ethyl acetate and extracting, and recovering an ethyl acetate solution; 1.5) concentrating the ethyl acetate solution obtained in the step 1.4) to obtain a solid substance; and 1.6) performing reduced pressure distillation on the solid substance obtained in the step 1.5) to obtain ethyl acetate for later use; and 2) performing acidolysis reaction. The invention provides a method for converting icariin to herba epimedii, which is easy to control preparation process, and high in product purity.
Description
Technical field
The invention belongs to the chemical purification technical field, relate to a kind of preparation method of Icaritin, relate in particular to a kind of method that icarin is converted into Icaritin.
Background technology
Herba Epimedii is a kind of Chinese medicinal materials commonly used, Berberidaceae plant Herba Epimedii (Epimedium brevicornu Maxim), arrow leaf Herba Epimedii (Epimedium sagittatum Maxim), pubescence Herba Epimedii (Epimedium pubescens Maxim), Epimedium wushanense (Epimedium wushanenes), the dry leave of Herba Epimedii (Epimedium koreanum Nakai), Herba Epimedii has kidney invigorating and YANG supporting, strengthening the muscles and bones, the effect of dispelling rheumatism, be usually used in treating the impotence erectile problem; urinate dripping; weakness of the waist and knees and coronary heart disease; chronic bronchitis, the diseases such as neurasthenia and poliomyelitis.Modern pharmacological research shows, Herba Epimedii contains special chemical composition and significant physiologically active.
Icaritin is the icarin aglycon, and it can obviously promote the propagation of MCU-7 cell and the expression of cell inner estrogen acceptor mRNA, and icarin is not observed this obvious effect.Icaritin can promote proliferation and differentiation of osteoblasts and suppress differentiation of osteoclast, its activity is better than icarin, icariside I and icariside II, modern study show, icarin had been metabolized to icariside II and Icaritin in enteron aisle before absorbing.
Modern study shows, Icaritin is stronger than icarin at very many-sided physiologically active, and Icaritin content in the plant of Epimedium is very low, mainly obtains by the icarin hydrolysis.
At present, the production of Icaritin mainly is the method that adopts enzymolysis and acidolysis combination, general enzymolysis is taked β glucuroide or complex cellulase, hydrochloric acid soln or sulphuric acid soln are adopted in acidolysis, but because the process of operation and reaction conditions different, thereby making the bad control of reaction process, by product is many, the problem that product yield is low, thus cause the cost of product higher.
Summary of the invention
In order to solve the above-mentioned technical problem that exists in the background technology, the invention provides the method that icarin is converted into Icaritin that a kind of preparation process is easy to control and product purity is high.
Technical solution of the present invention is: the invention provides a kind of method that icarin is converted into Icaritin, its special character is: the described method that icarin is converted into Icaritin may further comprise the steps:
1) enzyme digestion reaction:
1.1) prepare and adsorb the resin that icarin is arranged;
1.2) preparation enzyme dispersion liquid;
1.3) with step 1.1) and in prepared resin add step 1.2) in the enzyme dispersion liquid in form reaction solution and carry out enzyme digestion reaction; The condition of described enzyme digestion reaction is to bathe heating at 40-50 ℃ of Water Under;
1.4) with step 1.3) after formed reaction solution places room temperature, add ethyl acetate and extract, and reclaim acetic acid ethyl fluid;
1.5) with step 1.4) and in the concentrated solid matter that obtains of the acetic acid ethyl fluid that obtains;
1.6) with step 1.5) and in the decompression of resulting solid matter steam ethyl acetate, for subsequent use;
2) acidolysis reaction:
2.1) solid matter that enzyme digestion reaction is finally obtained be added to that the 10-15 of solid matter weight doubly measures 5% sulfuric acid liquid in, under the condition of heating in water bath, continue to stir and form dispersion liquid, the temperature during described heating in water bath is 40-50 ℃;
2.2) resin that the 3-5 of solid matter weight is doubly measured is added to step 2.1) in the formed dispersion liquid;
2.3) with step 2.2) resulting reaction solution puts to room temperature, add the ethyl acetate that the 2-3 of reaction solution volume doubly measures and extract;
2.4) extraction liquid after will extracting merges, and reclaims acetic acid ethyl fluid, gets the Icaritin product.
Above-mentioned steps 1.1) specific implementation is:
1.1.1) be added in the icarin weight 5-8 acetate buffer doubly icarin and dispersed with stirring;
1.1.2) at step 1.1.1) and in add icarin weight 3-5 resin doubly in the formed solution, stir and spend the night, form the resin that absorption has icarin;
1.1.3) adopt deionized water to step 1.1.2) formed absorption has the resin of icarin to clean.
Above-mentioned steps 1.1.1) pH of acetate buffer is 4～5 in.
Above-mentioned steps 1.1.2) resin in is macroporous resin.
Above-mentioned resin is D101 type, LSD-632 type, LSA-700 type, XDA-7 type or XDA-6 type.
Above-mentioned steps 1.2) specific implementation is:
Complex cellulase or β glucuroide be added in the icarin weight 5-8 acetate buffer doubly and to it fully stir; The pH of described acetate buffer is 4～5.
The consumption of above-mentioned complex cellulase or β glucuroide is not less than 1/20 of icarin weight.
Ethyl acetate consumption when extracting above-mentioned steps 1.4) is step 1.3) in formed reaction solution 2-3 doubly.
Above-mentioned steps 2.2) resin in is macroporous resin.
Above-mentioned resin is D101 type, LSD-632 type, LSA-700 type, XDA-7 type or XDA-6 type.
Advantage of the present invention is:
The present invention will disclose a kind of simple to operate, and the method that icarin is converted into Icaritin that transformation efficiency is high, the method are to extract good icarin powder, first absorption, again enzymolysis, again absorption, then wash-out, after elutriant is concentrated, adsorb again, again acidolysis, again absorption, last wash-out, elutriant is concentrated after, namely obtain the Icaritin product.Adopt preparation method disclosed by the invention, separate the Icaritin yield that obtains high, stable yield, simple to operate, process is easy to control, and product purity is high.Owing to having added resin, thereby limited to a greater extent the generation of side reaction, made more thorough that reaction carries out, and this reaction process is easy to control, have product yield stable, the characteristics that yield is high.
Embodiment
Principle of work of the present invention is: utilize macroporous adsorbent resin to the difference of icarin, intermediate product and Icaritin adsorptive power.First part is enzyme digestion reaction: before reaction does not occur; resin absorption be icarin; when enzyme digestion reaction occurs; resin is stronger to the adsorptive power of the intermediate product of generation; the intermediate product that is to say generation has been replaced original icarin; thereby reaction can be carried out smoothly, also protected the intermediate product that generates, avoided the generation of side reaction.Second section is acidolysis reaction: before reaction does not occur; resin absorption be intermediate product; when acidolysis reaction occurs; resin is stronger to the adsorptive power of the Icaritin of generation; the Icaritin that is to say generation has been replaced original intermediate product; thereby reaction can be carried out smoothly, also protected the Icaritin that generates.
Embodiment 1
Enzymolysis process:
(1) (content is 10% with icarin, HPLC detects) add in the acetate buffer of 5 times of amounts (icarin weight), dispersed with stirring is opened, and adds the resin (model D101) of 3 times of amounts (icarin weight) again, placement is spent the night, during do not stop to stir.
(2) with resin filter, and use a small amount of water rinse resin, for subsequent use.
(3) the β glucuroide is joined in the acetate buffer of 8 times of amounts (icarin weight), place appropriate containers, and use heating in water bath, dispersed with stirring is opened, and adjusts bath temperature at 40-50 ℃.
(4) resin with second step joins in the dispersion liquid of the 3rd enzyme that goes on foot, and stirs, when treating that temperature reaches specified temperature, and the beginning timing.
(5) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(6) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid.
(7) acetic acid ethyl fluid is concentrated into small volume after, place, namely obtain solid matter.
(8) decompression of this solid matter is steamed ethyl acetate after, for subsequent use.
The acidolysis process
(9) solid matter that enzymolysis is obtained joins in 5% the sulfuric acid liquid of 15 times of amounts (solid matter weight), places appropriate containers, and uses heating in water bath, and dispersed with stirring is opened, and to adjust bath temperature be 45 ℃.
(10) resin with 5 times of amounts (solid matter weight) joins in the dispersion liquid in the 9th step, and continuously stirring is used heating in water bath, and adjusting bath temperature is 45 ℃.
(11) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(12) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid, namely get the Icaritin product.
(13) transformation efficiency of icarin is 59.2%.
Embodiment 2
Enzymolysis process:
(1) (content is 30% with icarin, HPLC detects) add in the acetate buffer of 4 times of amounts (icarin weight), dispersed with stirring is opened, and adds the resin (model LSA-700) of 3 times of amounts (icarin weight) again, placement is spent the night, during do not stop to stir.
(2) with resin filter, and use a small amount of water rinse resin, for subsequent use.
(3) complex cellulase is joined in the acetate buffer of 8 times of amounts (icarin weight), place appropriate containers, and use heating in water bath, dispersed with stirring is opened, and adjusts bath temperature at 45 ℃.
(4) resin with second step joins in the dispersion liquid of the 3rd enzyme that goes on foot, and stirs, when treating that temperature reaches specified temperature, and the beginning timing.
(5) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(6) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid.
(7) acetic acid ethyl fluid is concentrated into small volume after, place, namely obtain solid matter.
(8) decompression of this solid matter is steamed ethyl acetate after, for subsequent use.
The acidolysis process
(9) solid matter that enzymolysis is obtained joins in 5% the sulfuric acid liquid of 15 times of amounts (solid matter weight), places appropriate containers, and uses heating in water bath, and dispersed with stirring is opened, and to adjust bath temperature be 45 ℃.
(10) resin (model LSA-700) with 4 times of amounts (solid matter weight) joins in the dispersion liquid in the 9th step, and continuously stirring is used heating in water bath, and adjusting bath temperature is 45 ℃.
(11) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(12) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid, namely get the Icaritin product.
(13) transformation efficiency of icarin is 61.4%.
Embodiment 3
Enzymolysis process:
(1) (content is 30% with icarin, HPLC detects) add in the acetate buffer of 4 times of amounts (icarin weight), dispersed with stirring is opened, and adds the resin (model LSA-700) of 3 times of amounts (icarin weight) again, placement is spent the night, during do not stop to stir.
(2) with resin filter, and use a small amount of water rinse resin, for subsequent use.
(3) complex cellulase is joined in the acetate buffer of 8 times of amounts (icarin weight), place appropriate containers, and use heating in water bath, dispersed with stirring is opened, and adjusts bath temperature at 45 ℃.
(4) resin with second step joins in the dispersion liquid of the 3rd enzyme that goes on foot, and stirs, when treating that temperature reaches specified temperature, and the beginning timing.
(5) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(6) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid.
(7) acetic acid ethyl fluid is concentrated into small volume after, place, namely obtain solid matter.
(8) decompression of this solid matter is steamed ethyl acetate after, for subsequent use.
The acidolysis process
(9) solid matter that enzymolysis is obtained joins in 5% the sulfuric acid liquid of 15 times of amounts (solid matter weight), places appropriate containers, and uses heating in water bath, and dispersed with stirring is opened, and to adjust bath temperature be 45 ℃.
(10) resin (model LSA-700) with 4 times of amounts (solid matter weight) joins in the dispersion liquid in the 9th step, and continuously stirring is used heating in water bath, and adjusting bath temperature is 45 ℃.
(11) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(12) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid, namely get the Icaritin product.
(13) transformation efficiency of icarin is 60.4%.
Embodiment 4
Enzymolysis process:
(1) (content is 45% with icarin, HPLC detects) add in the acetate buffer of 4 times of amounts (icarin weight), dispersed with stirring is opened, and adds the resin (model D101) of 3 times of amounts (icarin weight) again, placement is spent the night, during do not stop to stir.
(2) with resin filter, and use a small amount of water rinse resin, for subsequent use.
(3) complex cellulase is joined in the acetate buffer of 8 times of amounts (icarin weight), place appropriate containers, and use heating in water bath, dispersed with stirring is opened, and adjusts bath temperature at 50 ℃.
(4) resin with second step joins in the dispersion liquid of the 3rd enzyme that goes on foot, and stirs, when treating that temperature reaches specified temperature, and the beginning timing.
(5) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(6) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid.
(7) acetic acid ethyl fluid is concentrated into small volume after, place, namely obtain solid matter.
(8) decompression of this solid matter is steamed ethyl acetate after, for subsequent use.
The acidolysis process
(9) solid matter that enzymolysis is obtained joins in 5% the sulfuric acid liquid of 15 times of amounts (solid matter weight), places appropriate containers, and uses heating in water bath, and dispersed with stirring is opened, and to adjust bath temperature be 45 ℃.
(10) resin (model D101) with 4 times of amounts (solid matter weight) joins in the dispersion liquid in the 9th step, and continuously stirring is used heating in water bath, and adjusting bath temperature is 50 ℃.
(11) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(12) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid, namely get the Icaritin product.
(13) transformation efficiency of icarin is 61.0%.
Embodiment 5
Enzymolysis process:
(1) (content is 98% with icarin, HPLC detects) add in the acetate buffer of 4 times of amounts (icarin weight), dispersed with stirring is opened, and adds the resin (model LSA-700) of 3 times of amounts (icarin weight) again, placement is spent the night, during do not stop to stir.
(2) with resin filter, and use a small amount of water rinse resin, for subsequent use.
(3) complex cellulase is joined in the acetate buffer of 8 times of amounts (icarin weight), place appropriate containers, and use heating in water bath, dispersed with stirring is opened, and adjusts bath temperature at 45 ℃.
(4) resin with second step joins in the dispersion liquid of the 3rd enzyme that goes on foot, and stirs, when treating that temperature reaches specified temperature, and the beginning timing.
(5) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(6) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid.
(7) acetic acid ethyl fluid is concentrated into small volume after, place, namely obtain solid matter.
(8) decompression of this solid matter is steamed ethyl acetate after, for subsequent use.
The acidolysis process
(9) solid matter that enzymolysis is obtained joins in 5% the sulfuric acid liquid of 15 times of amounts (solid matter weight), places appropriate containers, and uses heating in water bath, and dispersed with stirring is opened, and to adjust bath temperature be 45 ℃.
(10) resin (model LSA-700) with 4 times of amounts (solid matter weight) joins in the dispersion liquid in the 9th step, and continuously stirring is used heating in water bath, and adjusting bath temperature is 45 ℃.
(11) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(12) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid, namely get the Icaritin product.
(13) transformation efficiency of icarin is 61.5%.
Embodiment 6
Enzymolysis process:
(1) (content is 80% with icarin, HPLC detects) add in the acetate buffer of 4 times of amounts (icarin weight), dispersed with stirring is opened, and adds the resin (model LSD-632) of 3 times of amounts (icarin weight) again, placement is spent the night, during do not stop to stir.
(2) with resin filter, and use a small amount of water rinse resin, for subsequent use.
(3) complex cellulase is joined in the acetate buffer of 8 times of amounts (icarin weight), place appropriate containers, and use heating in water bath, dispersed with stirring is opened, and adjusts bath temperature at 48 ℃.
(4) resin with second step joins in the dispersion liquid of the 3rd enzyme that goes on foot, and stirs, when treating that temperature reaches specified temperature, and the beginning timing.
(5) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(6) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid.
(7) acetic acid ethyl fluid is concentrated into small volume after, place, namely obtain solid matter.
(8) decompression of this solid matter is steamed ethyl acetate after, for subsequent use.
The acidolysis process
(9) solid matter that enzymolysis is obtained joins in 5% the sulfuric acid liquid of 15 times of amounts (solid matter weight), places appropriate containers, and uses heating in water bath, and dispersed with stirring is opened, and to adjust bath temperature be 45 ℃.
(10) resin (model LSD-632) with 4 times of amounts (solid matter weight) joins in the dispersion liquid in the 9th step, and continuously stirring is used heating in water bath, and adjusting bath temperature is 50 ℃.
(11) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(12) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid, namely get the Icaritin product.
(13) transformation efficiency of icarin is 62.1%.
Embodiment 7
Enzymolysis process:
(1) (content is 60% with icarin, HPLC detects) add in the acetate buffer of 4 times of amounts (icarin weight), dispersed with stirring is opened, and adds the resin (model D101) of 3 times of amounts (icarin weight) again, placement is spent the night, during do not stop to stir.
(2) with resin filter, and use a small amount of water rinse resin, for subsequent use.
(3) complex cellulase is joined in the acetate buffer of 8 times of amounts (icarin weight), place appropriate containers, and use heating in water bath, dispersed with stirring is opened, and adjusts bath temperature at 48 ℃.
(4) resin with second step joins in the dispersion liquid of the 3rd enzyme that goes on foot, and stirs, when treating that temperature reaches specified temperature, and the beginning timing.
(5) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(6) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid.
(7) acetic acid ethyl fluid is concentrated into small volume after, place, namely obtain solid matter.
(8) decompression of this solid matter is steamed ethyl acetate after, for subsequent use.
The acidolysis process
(9) solid matter that enzymolysis is obtained joins in 5% the sulfuric acid liquid of 15 times of amounts (solid matter weight), places appropriate containers, and uses heating in water bath, and dispersed with stirring is opened, and to adjust bath temperature be 45 ℃.
(10) resin (model D101) with 4 times of amounts (solid matter weight) joins in the dispersion liquid in the 9th step, and continuously stirring is used heating in water bath, and adjusting bath temperature is 48 ℃.
(11) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(12) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid, namely get the Icaritin product.
(13) transformation efficiency of icarin is 61.8%.
Embodiment 8
Enzymolysis process:
(1) (content is 50% with icarin, HPLC detects) add in the acetate buffer of 5 times of amounts (icarin weight), dispersed with stirring is opened, and adds the resin (model XDA-7) of 3 times of amounts (icarin weight) again, placement is spent the night, during do not stop to stir.
(2) with resin filter, and use a small amount of water rinse resin, for subsequent use.
(3) complex cellulase is joined in the acetate buffer of 8 times of amounts (icarin weight), place appropriate containers, and use heating in water bath, dispersed with stirring is opened, and adjusts bath temperature at 48 ℃.
(4) resin with second step joins in the dispersion liquid of the 3rd enzyme that goes on foot, and stirs, when treating that temperature reaches specified temperature, and the beginning timing.
(5) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(6) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid.
(7) acetic acid ethyl fluid is concentrated into small volume after, place, namely obtain solid matter.
(8) decompression of this solid matter is steamed ethyl acetate after, for subsequent use.
The acidolysis process
(9) solid matter that enzymolysis is obtained joins in 5% the sulfuric acid liquid of 15 times of amounts (solid matter weight), places appropriate containers, and uses heating in water bath, and dispersed with stirring is opened, and to adjust bath temperature be 48 ℃.
(10) resin (model XDA-7) with 4 times of amounts (solid matter weight) joins in the dispersion liquid in the 9th step, and continuously stirring is used heating in water bath, and adjusting bath temperature is 45 ℃.
(11) after question response finishes, reaction solution is put to room temperature, the ethyl acetate that adds 3 times of amounts (reaction solution volume) extracts.
(12) after extraction finishes, extraction liquid is merged, reclaim acetic acid ethyl fluid, namely get the Icaritin product.
(13) transformation efficiency of icarin is 60.8%.
Claims (10)
1. method that icarin is converted into Icaritin is characterized in that: said method comprising the steps of:
1) enzyme digestion reaction:
1.1) prepare and adsorb the resin that icarin is arranged;
1.2) preparation enzyme dispersion liquid;
1.3) with step 1.1) and in prepared resin add step 1.2) in the enzyme dispersion liquid in form reaction solution and carry out enzyme digestion reaction; The condition of described enzyme digestion reaction is to bathe heating at 40-50 ℃ of Water Under;
1.4) with step 1.3) after formed reaction solution places room temperature, add ethyl acetate and extract, and reclaim acetic acid ethyl fluid;
1.5) with step 1.4) and in the concentrated solid matter that obtains of the acetic acid ethyl fluid that obtains;
1.6) with step 1.5) and in the decompression of resulting solid matter steam ethyl acetate, for subsequent use;
2) acidolysis reaction:
2.1) solid matter that enzyme digestion reaction is finally obtained be added to that the 10-15 of solid matter weight doubly measures 5% sulfuric acid liquid in, under the condition of heating in water bath, continue to stir and form dispersion liquid, the temperature during described heating in water bath is 40-50 ℃;
2.2) resin that the 3-5 of solid matter weight is doubly measured is added to step 2.1) in the formed dispersion liquid;
2.3) with step 2.2) resulting reaction solution puts to room temperature, add the ethyl acetate that the 2-3 of reaction solution volume doubly measures and extract;
2.4) extraction liquid after will extracting merges, and reclaims acetic acid ethyl fluid, gets the Icaritin product.
2. the method that icarin is converted into Icaritin according to claim 1, it is characterized in that: specific implementation described step 1.1) is:
1.1.1) be added in the icarin weight 5-8 acetate buffer doubly icarin and dispersed with stirring;
1.1.2) at step 1.1.1) and in add icarin weight 3-5 resin doubly in the formed solution, stir and spend the night, form the resin that absorption has icarin;
1.1.3) adopt deionized water to step 1.1.2) formed absorption has the resin of icarin to clean.
3. the method that icarin is converted into Icaritin according to claim 2 is characterized in that: the pH of acetate buffer is 4～5 described step 1.1.1).
4. the method that icarin is converted into Icaritin according to claim 3, it is characterized in that: the resin described step 1.1.2) is macroporous resin.
5. the method that icarin is converted into Icaritin according to claim 4, it is characterized in that: described resin is D101 type, LSD-632 type, LSA-700 type, XDA-7 type or XDA-6 type.
6. the method that icarin is converted into Icaritin according to claim 5, it is characterized in that: specific implementation described step 1.2) is:
Complex cellulase or β glucuroide be added in the icarin weight 5-8 acetate buffer doubly and to it fully stir; The pH of described acetate buffer is 4～5.
7. the method that icarin is converted into Icaritin according to claim 6, it is characterized in that: the consumption of described complex cellulase or β glucuroide is not less than 1/20 of icarin weight.
8. the method that icarin is converted into Icaritin according to claim 7, it is characterized in that: the ethyl acetate consumption when extracting described step 1.4) is step 1.3) in formed reaction solution 2-3 doubly.
9. the described method that icarin is converted into Icaritin of arbitrary claim according to claim 1-8, it is characterized in that: the resin described step 2.2) is macroporous resin.
10. the method that icarin is converted into Icaritin according to claim 9, it is characterized in that: described resin is D101 type, LSD-632 type, LSA-700 type, XDA-7 type or XDA-6 type.
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| CN104711300A (en) * | 2013-12-13 | 2015-06-17 | 北京珅奥基医药科技有限公司 | Preparation method of icaritin |
| CN106755214A (en) * | 2016-12-08 | 2017-05-31 | 江苏大学 | A kind of method that two-phase enzyme hydrolysis obtains precious leaves of pulse plants glycosides I |
| CN106995829A (en) * | 2017-05-12 | 2017-08-01 | 南京林业大学 | A kind of method that enzymatic conversion method barren wort total chromocor prepares epimedium aglucone |
| 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 |
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| CN104711300A (en) * | 2013-12-13 | 2015-06-17 | 北京珅奥基医药科技有限公司 | Preparation method of icaritin |
| CN104711300B (en) * | 2013-12-13 | 2018-07-24 | 北京珅奥基医药科技有限公司 | The preparation method of icariine |
| CN106755214A (en) * | 2016-12-08 | 2017-05-31 | 江苏大学 | A kind of method that two-phase enzyme hydrolysis obtains precious leaves of pulse plants glycosides I |
| CN106755214B (en) * | 2016-12-08 | 2020-06-26 | 江苏大学 | Method for obtaining baohuoside I by means of two-phase enzymatic hydrolysis |
| CN106995829A (en) * | 2017-05-12 | 2017-08-01 | 南京林业大学 | A kind of method that enzymatic conversion method barren wort total chromocor prepares epimedium aglucone |
| CN106995829B (en) * | 2017-05-12 | 2021-03-30 | 南京林业大学 | Method for preparing icariin by converting total flavonoids of epimedium herb through enzyme method |
| 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 |
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