CN104788517A - Method of using epimedium medicinal material to extract icariin - Google Patents
Method of using epimedium medicinal material to extract icariin Download PDFInfo
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- CN104788517A CN104788517A CN201510200937.8A CN201510200937A CN104788517A CN 104788517 A CN104788517 A CN 104788517A CN 201510200937 A CN201510200937 A CN 201510200937A CN 104788517 A CN104788517 A CN 104788517A
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- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
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- 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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Abstract
The invention relates to a method of using an epimedium medicinal material to extract icariin. The method comprises the steps of crushing, extracting twice, concentrating, extracting, dissolving, taking a reaction, performing chromatography, washing, eluting, concentrating, drying and the like. The method can improve the extraction efficiency of icariin, solves the raw material shortage problem, prolongs the service life of resin, reduces the environmental pollution, increases the content and the yield of icariin, and relieves the production stress of a production enterprise.
Description
Technical field
The invention belongs to medicinal material extract technical field, be specifically related to a kind of method that epimedium herb extracts icariine.
Background technology
In existing extraction Herba Epimedii, the equipment great majority of icariine are the extractor of band agitating function, and when extracting, put in extractor by raw material epimedium herb, add the ethanol of 60% as Extraction solvent, under the condition of 70 DEG C, return stirring extracts; Or raw material epimedium herb is dropped in extractor, stir under the condition of add tap water as Extraction solvent, heat, boiling and extract.
But there are the following problems for the method for icariine in existing extraction Herba Epimedii:
When 1, adopting the extractor of band agitating function to extract icariine in Herba Epimedii, need extraction 3 times, first pass extraction time is 2 hours, and second time and the 3rd time is all 1.5 hours, like this, make to extract that extraction time of icariine is long, extraction yield is low, plant produced cost is large.
2, icariine refining in, existing technique adopts resin concentration to remove impurity in extracting solution.This method seems high-tech, and greatly, the burden of factory is large in waste actually.Extracting solution bring huge pollution without selective extraction to the duct of resin, the life-span of resin must be changed again at 2 months, not only brings huge financial loss to factory, also give country environment bring very large pollution.
In view of the above-mentioned technological deficiency of prior art, in the urgent need to developing a kind of novel method extracting icariine from epimedium herb.
Summary of the invention
The object of the invention is to overcome the shortcoming existed in prior art, a kind of epimedium herb is provided to extract the method for icariine, the method can improve the extraction efficiency of icariine, solve the nervous problem of raw material, and can extend resin work-ing life, reduce environmental pollution, the content improving icariine and yield, alleviate the production pressure of manufacturing enterprise.
To achieve these goals, the invention provides following technical scheme: a kind of epimedium herb extracts the method for icariine, and it comprises the following steps: (1) pulverizes: the epimedium herb pulverizer of drying is crushed to meal; (2) first time extracts: put into by meal in the extractor with ultrasonic generator, then the alcohol solvent adding 60% of 8 times of meal weight soaks, soak time is 0.5 ~ 1 hour, carry out first time after immersion to extract, in leaching process, whole process is opened stirring and is extracted, and stirring velocity is 30 turns/min, Extracting temperature is 60 degrees Celsius, during extraction, the power of ultrasonic generator is 600W, and extraction time is 50 minutes, thus obtains the extracting solution of first time extraction; (3) second time is extracted: after taking out the extracting solution of first time extraction, the alcohol solvent adding 60% of 7 times of meal weight again in extractor soaks, soak time is 0.5 ~ 1 hour, carry out second time after immersion to extract, in leaching process, whole process is opened stirring and is extracted, and stirring velocity is 30 turns/min, Extracting temperature is 60 degrees Celsius, during extraction, the power of ultrasonic generator is 600W, and extraction time is 30 minutes, thus obtains the extracting solution of second time extraction; (4) concentrated: the rear Plate Filtration of extracting solution mixing that the extracting solution extract first time and second time are extracted, concentrate with decompression concentrator after filtration, thickening temperature is 60 DEG C, makes the concentrated solution of acquisition be 1/10 of extracting liquid volume by concentration and recovery ethanol; (5) extract: make concentrated solution repeatedly extract 2 ~ 3 times through the column extractor that ethyl acetate and propyl carbinol are housed and be extracted liquid; (6) dissolve: add in described extraction liquid 2 times amount, 30% spirituous solution dissolve, obtain reaction solution, and the concentration of Epimedin A, Epimedin B and epimedin in detection reaction liquid; (7) react: reaction solution is placed in reactor, control temperature is 45 ± 5 DEG C, respectively by Epimedin A, Epimedin B, epimedin weight 5% amount add the catalyzer making their scission of links, then 80 ± 5 DEG C degrees Celsius are warming up to, carry out back flow reaction, during reaction, stirring velocity is 30 turns/min, and the reaction times is 1h ~ 1.5h; Afterwards, be cooled to rapidly 45 ± 5 DEG C, the concentration then slowly adding 1wt% is the HCl of 1mol/L, then reacts 1h, and filtration obtains icariine conversion fluid; (8) chromatography: the DM130 type macroporous adsorbent resin handled well is inserted in chromatography column, adding 80 DEG C of water, to dilute above-mentioned icariine conversion fluid to icariine concentration be 12 ~ 15g/L, by the icariine conversion fluid after dilution by carrying out chromatography in described chromatography column, wherein, when chromatography, the PH of upper prop liquid is adjusted to 3.8, and loading speed is 0.6 ~ 1.0BV/h; (9) clean: the effluent liquid detecting chromatography, when there being effective constituent to ooze out, the deionized water of 2-3BV cleans, and cleaning speed is 1BV/h; (10) wash-out: after cleaning, carry out wash-out with the elutriant of 3BV, elution speed is 0.3BV/h, and collects elutriant; (11) concentrate drying: carry out vacuum concentration to elutriant, when the proportion being concentrated to concentrated solution is 1.1-1.25, carries out spraying dry with spray-drying tower, must be not less than the icariine of 85% purity.
Further, wherein, the ethyl acetate in described column extractor and the mass ratio of propyl carbinol are 2: 1.
Compared with the method extracting icariine with existing epimedium herb, the method that epimedium herb of the present invention extracts icariine has following Advantageous Effects:
1, the shortcoming that traditional extraction technology extraction efficiency is low is overcome.In ultrasonic-assisted extraction Herba Epimedii icariine process in, ultrasonic wave, by cytoclasis, enables organic solvent enter cell fast and efficiently, thus shorten extraction time, substantially increase extraction efficiency; Meanwhile, hyperacoustic Extracting temperature is low, save energy.
2, the deficiency of raw material is solved.Epimedium herb feed distribution in the Inner Mongol, Beijing, Hebei, Shaanxi, Gansu, Sichuan and area, northeast, and Icarrin is not less than the raw material of the Jin You Longnan Prefecture of 0.5% in raw material, in the raw material in other area, Icarrin is very low, is unsuitable for the extraction carrying out icariine; Meanwhile, epimedium herb is wild, manually can not cultivate, and excavates with the not science of people, causes raw material worsening shortages.The present invention is in the leaching process of icariine, epimedin in Herba Epimedii can be changed into icariine, thus medicinal material in all parts of the country can be utilized, avoid the anxiety of wild Herba Epimedii raw material, also increase the possibility of cultivation epimedium herb.
3, the low pollution caused to environment of resin utilization rate is reduced to greatest extent.Common resin absorption is the material that absorption has same characteristic, DM130 resin absorption Flavonoid substances is better, it also adsorbs other flavones in extracting solution in the lump while absorption icariine, resin is caused to only have 2 months work-ing life, and the content of the product icariine obtained is 7% ~ 19%, while the production pressure of manufacturing enterprise is large, also result in serious environmental pollution.In the present invention, after epimedin conversion, revising, obtain the conversion fluid that relative purity is higher, then utilize the absorption of resin, make icariine obtain enrichment.In the present invention, epimedin is directive changes into icariine to adopt scission of link, resynthesis technology in chemical industry synthesis to make, the icariine purity of extracting solution is improved, binding resin absorption makes icariine separate again, the work-ing life of resin extends to 18 months, and the icariine product content that manufacturing enterprise obtains is 85% ~ 90%.
Accompanying drawing explanation
Fig. 1 is the schema that epimedium herb of the present invention extracts the method for icariine.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described, and embodiment is not as the restriction to protection scope of the present invention.
Fig. 1 shows the schema that epimedium herb of the present invention extracts the method for icariine.See Fig. 1, the method that epimedium herb of the present invention extracts icariine comprises the following steps:
(1) pulverize.
Epimedium herb is dried, and the epimedium herb pulverizer of drying is crushed to meal.Described pulverizer can be any conventional pulverizer.The concrete granularity of described meal is different according to the difference of pulverizer.Being ground into the object of meal, is for the ease of follow-up immersion and extraction.
(2) first time extracts.
The meal be ground into is put in the extractor with ultrasonic generator.Then the alcohol solvent adding 60% soaks, and soak time is 0.5 ~ 1 hour.Wherein, the amount of the alcohol solvent added is 8 times of the weight of meal.Carry out first time after immersion to extract.In leaching process, whole process is opened stirring and is extracted, and stirring velocity is 30 turns/min, and Extracting temperature is 60 degrees Celsius, and extraction time is 50 minutes.During extraction, the power of ultrasonic generator is 600W.Extracted by first time and obtain the extracting solution of first time extraction.
(3) second time is extracted.
After taking out the extracting solution that first time extracts, stayed in extractor by the dregs of a decoction, then the alcohol solvent adding 60% in extractor soaks, soak time is 0.5 ~ 1 hour.Wherein, the amount of the alcohol solvent added is 7 times of the weight of meal.Carry out second time after immersion to extract.In leaching process, whole process is opened stirring and is extracted, and stirring velocity is 30 turns/min, and Extracting temperature is 60 degrees Celsius, and extraction time is 30 minutes.During extraction, the power of ultrasonic generator is 600W.Extracted by second time and obtain the extracting solution of second time extraction.
In the present invention, in the leaching process that first time extracts and second time is extracted, due to the existence of ultrasonic generator, make it possible to send ultrasonic wave, by ultrasonic wave by cytoclasis, make organic solvent, namely alcohol solvent can enter cell fast and efficiently, thus shorten extraction time, substantially increase extraction efficiency; Meanwhile, hyperacoustic Extracting temperature is low, save energy, reduces the production cost of enterprise.
(4) concentrated.
The rear Plate Filtration of extracting solution mixing that the extracting solution extract first time and second time are extracted, gets rid of the dregs of a decoction etc. contained in extracting solution.Concentrate with decompression concentrator after filtration, thickening temperature is 60 DEG C.Concentrated solution is obtained by concentration and recovery alcohol solvent.Wherein, the concentrated solution obtained is 1/10 of mixed extracting liquid volume.
(5) extract.
Make concentrated solution repeatedly extract 2 ~ 3 times through the column extractor that ethyl acetate and propyl carbinol are housed and be extracted liquid.Preferably, the ethyl acetate in described column extractor and the mass ratio of propyl carbinol are 2: 1, like this, can obtain better effect of extracting.Wherein, by extraction, the macromole impurity in concentrated solution is removed, ensure the mutually limpid, transparent of icariine, transmittance is not less than 92%.
(6) dissolve.
The spirituous solution adding 30% in described extraction liquid dissolves, and obtains reaction solution.Wherein, the weight of the spirituous solution added is 2 times of described extraction liquid.Detect the concentration of Epimedin A, Epimedin B and epimedin in the reaction solution obtained, so that calculate the content of Epimedin A in reaction solution, Epimedin B and epimedin.
(7) react.
Reaction solution is placed in reactor, and the temperature controlling reactor is 45 ± 5 DEG C, in reactor, then add the catalyzer that can make Epimedin A, Epimedin B, epimedin scission of link respectively.Wherein, the add-on of the catalyzer of Epimedin A scission of link can be made to be 5% of the content of Epimedin A; The add-on of the catalyzer of Epimedin B scission of link can be made to be 5% of the content of Epimedin B; The add-on of the catalyzer of epimedin scission of link can be made to be 5% of the content of epimedin.
After adding catalyzer, make reactor be warming up to 80 ± 5 DEG C degrees Celsius, carry out back flow reaction.During reaction, stirring velocity is 30 turns/min, and the reaction times is 1h ~ 1.5h.Afterwards, make reactor be cooled to rapidly 45 ± 5 DEG C, the concentration then slowly adding 1wt% is the HCl of 1mol/L, then reacts 1h, and filtration obtains icariine conversion fluid.Preferably, in reaction process, control PH is about 3.0.
In the present invention, Epimedin A, Epimedin B and epimedin can be made to change into icariine by above-mentioned reaction process.Like this, the lower epimedium herb of Icarrin can be made also to be used for extracting icariine, to expand available raw material range, alleviate raw material crisis.
(8) chromatography.
The DM130 type macroporous adsorbent resin handled well is inserted in chromatography column, form layers analysis apparatus.In above-mentioned icariine conversion fluid, add the water of 80 DEG C, thus above-mentioned icariine conversion fluid is diluted to icariine concentration is 12 ~ 15g/L.By the icariine conversion fluid after dilution by carrying out chromatography in described chromatography column.When chromatography, the PH of the upper prop liquid in chromatography column is adjusted to about 3.8, and meanwhile, loading speed is 0.6 ~ 1.0BV/h.Wherein, BV is resin volume, and 1BV is a resin volume.
(9) clean.
Detect the effluent liquid of chromatography, when there being effective constituent to ooze out in effluent liquid, in described chromatography column, adding deionized water clean.In the present invention, clean with the deionized water of 2-3BV, cleaning speed is 1BV/h.
(10) wash-out.
After cleaning, carry out wash-out with the elutriant of 3BV, elution speed is 0.3BV/h, and collects elutriant.
(11) concentrate drying.
Vacuum concentration is carried out to the elutriant collected, when the proportion being concentrated to concentrated solution is 1.1-1.25, carries out spraying dry with spray-drying tower, the icariine of 85% purity must be not less than.
The method of epimedium herb extraction Herba Epimedii of the present invention can improve the extraction efficiency of icariine, solves the problem that in leaching process, extraction time is long and extraction yield is low.Meanwhile, epimedin is changed into icariine by the mode of epimedin scission of link, correction by it, makes the epimedium herb of Icarrin also can be used for extracting icariine, can solve the anxiety of raw material.Finally, it can extend the work-ing life of resin, reduces environmental pollution, improves content and the yield of icariine, alleviates the production pressure of manufacturing enterprise.
The above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (2)
1. epimedium herb extracts a method for icariine, and it comprises the following steps:
(1) pulverize: the epimedium herb pulverizer of drying is crushed to meal;
(2) first time extracts: put into by meal in the extractor with ultrasonic generator, then the alcohol solvent adding 60% of 8 times of meal weight soaks, soak time is 0.5 ~ 1 hour, carry out first time after immersion to extract, in leaching process, whole process is opened stirring and is extracted, and stirring velocity is 30 turns/min, Extracting temperature is 60 degrees Celsius, during extraction, the power of ultrasonic generator is 600W, and extraction time is 50 minutes, thus obtains the extracting solution of first time extraction;
(3) second time is extracted: after taking out the extracting solution of first time extraction, the alcohol solvent adding 60% of 7 times of meal weight again in extractor soaks, soak time is 0.5 ~ 1 hour, carry out second time after immersion to extract, in leaching process, whole process is opened stirring and is extracted, and stirring velocity is 30 turns/min, Extracting temperature is 60 degrees Celsius, during extraction, the power of ultrasonic generator is 600W, and extraction time is 30 minutes, thus obtains the extracting solution of second time extraction;
(4) concentrated: the rear Plate Filtration of extracting solution mixing that the extracting solution extract first time and second time are extracted, concentrate with decompression concentrator after filtration, thickening temperature is 60 DEG C, makes the concentrated solution of acquisition be 1/10 of extracting liquid volume by concentration and recovery ethanol;
(5) extract: make concentrated solution repeatedly extract 2 ~ 3 times through the column extractor that ethyl acetate and propyl carbinol are housed and be extracted liquid;
(6) dissolve: add in described extraction liquid 2 times amount, 30% spirituous solution dissolve, obtain reaction solution, and the concentration of Epimedin A, Epimedin B and epimedin in detection reaction liquid;
(7) react: reaction solution is placed in reactor, control temperature is 45 ± 5 DEG C, respectively by Epimedin A, Epimedin B, epimedin weight 5% amount add the catalyzer making their scission of links, then 80 ± 5 DEG C degrees Celsius are warming up to, carry out back flow reaction, during reaction, stirring velocity is 30 turns/min, and the reaction times is 1h ~ 1.5h; Afterwards, be cooled to rapidly 45 ± 5 DEG C, the concentration then slowly adding 1wt% is the HCl of 1mol/L, then reacts 1h, and filtration obtains icariine conversion fluid;
(8) chromatography: the DM130 type macroporous adsorbent resin handled well is inserted in chromatography column, adding 80 DEG C of water, to dilute above-mentioned icariine conversion fluid to icariine concentration be 12 ~ 15g/L, by the icariine conversion fluid after dilution by carrying out chromatography in described chromatography column, wherein, when chromatography, the PH of upper prop liquid is adjusted to 3.8, and loading speed is 0.6 ~ 1.0BV/h;
(9) clean: the effluent liquid detecting chromatography, when there being effective constituent to ooze out in effluent liquid, the deionized water of 2-3BV cleans, and cleaning speed is 1BV/h;
(10) wash-out: after cleaning, carry out wash-out with the elutriant of 3BV, elution speed is 0.3BV/h, and collects elutriant;
(11) concentrate drying: carry out vacuum concentration to elutriant, when the proportion being concentrated to concentrated solution is 1.1-1.25, carries out spraying dry with spray-drying tower, must be not less than the icariine of 85% purity.
2. epimedium herb according to claim 1 extracts the method for icariine, and wherein, the ethyl acetate in described column extractor and the mass ratio of propyl carbinol are 2: 1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108440620A (en) * | 2018-04-26 | 2018-08-24 | 赣州禾绿康健生物技术有限公司 | A kind of preparation method of high-content icariin extract |
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| CN101747393A (en) * | 2008-12-17 | 2010-06-23 | 中国科学院大连化学物理研究所 | Method for simultaneously preparing chemical references of icariin, epimedin A, epimedin B and epimedin C |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101747393A (en) * | 2008-12-17 | 2010-06-23 | 中国科学院大连化学物理研究所 | Method for simultaneously preparing chemical references of icariin, epimedin A, epimedin B and epimedin C |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108440620A (en) * | 2018-04-26 | 2018-08-24 | 赣州禾绿康健生物技术有限公司 | A kind of preparation method of high-content icariin extract |
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