CN111440222A - Method for extracting icariin - Google Patents
Method for extracting icariin Download PDFInfo
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- CN111440222A CN111440222A CN202010441939.7A CN202010441939A CN111440222A CN 111440222 A CN111440222 A CN 111440222A CN 202010441939 A CN202010441939 A CN 202010441939A CN 111440222 A CN111440222 A CN 111440222A
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- epimedium
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- TZJALUIVHRYQQB-XFDQAQKOSA-N Icariin Natural products O(C)c1ccc(C2=C(O[C@H]3[C@@H](O)[C@H](O)[C@@H](O)[C@H](C)O3)C(=O)c3c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O4)c(C/C=C(\C)/C)c3O2)cc1 TZJALUIVHRYQQB-XFDQAQKOSA-N 0.000 title claims abstract description 77
- TZJALUIVHRYQQB-XLRXWWTNSA-N icariin Chemical compound C1=CC(OC)=CC=C1C1=C(O[C@H]2[C@@H]([C@H](O)[C@@H](O)[C@H](C)O2)O)C(=O)C2=C(O)C=C(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-XLRXWWTNSA-N 0.000 title claims abstract description 77
- TZJALUIVHRYQQB-UHFFFAOYSA-N icariine Natural products C1=CC(OC)=CC=C1C1=C(OC2C(C(O)C(O)C(C)O2)O)C(=O)C2=C(O)C=C(OC3C(C(O)C(O)C(CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000002994 raw material Substances 0.000 claims abstract description 60
- 238000000605 extraction Methods 0.000 claims abstract description 54
- 241000893536 Epimedium Species 0.000 claims abstract description 51
- 235000018905 epimedium Nutrition 0.000 claims abstract description 51
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 23
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 44
- 239000002904 solvent Substances 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 8
- 238000002137 ultrasound extraction Methods 0.000 claims description 5
- 239000003814 drug Substances 0.000 abstract description 2
- 239000000284 extract Substances 0.000 description 18
- 239000000706 filtrate Substances 0.000 description 16
- 238000001514 detection method Methods 0.000 description 15
- 238000001035 drying Methods 0.000 description 14
- 239000012535 impurity Substances 0.000 description 14
- 238000001914 filtration Methods 0.000 description 12
- 238000011068 loading method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010298 pulverizing process Methods 0.000 description 7
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 241000133570 Berberidaceae Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241001362421 Epimedium brevicornu Species 0.000 description 1
- 241000893531 Epimedium koreanum Species 0.000 description 1
- 241001660849 Epimedium pubescens Species 0.000 description 1
- 241001362411 Epimedium sagittatum Species 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229930183477 epimedin Natural products 0.000 description 1
- 235000020696 epimedium extract Nutrition 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- RPDAUEIUDPHABB-UHFFFAOYSA-N potassium ethoxide Chemical compound [K+].CC[O-] RPDAUEIUDPHABB-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention belongs to the technical field of traditional Chinese medicine extraction, and particularly relates to an icariin extraction method, which comprises the following steps: mixing fresh epimedium raw material with weak base-containing alcohol solution, heating and extracting; the weak base-containing alcohol solution is prepared by mixing an alcohol solution with the mass fraction of 50-95% and an ammonia water solution with the mass fraction of 25-28% according to the volume ratio of 90-99: 1-10, mixing; the alcoholic solution is methanol solution or ethanol solution. The method for extracting icariin provided by the invention can obviously improve the content of icariin in epimedium raw materials, especially can enable the content of icariin in epimedium raw materials in a Bashu region to reach more than 0.5%, and obviously improves the utilization rate of the epimedium raw materials.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine extraction, and particularly relates to an extraction method of icariin.
Background
Herba Epimedii is dry leaf of Epimedium brevicornum Maxim, Epimedium sagittatum Maxim, Epimedium pubescens Maxim or Epimedium koreanum nakai of berberidaceae, has effects of invigorating kidney yang, strengthening tendons and bones, and dispelling pathogenic wind and dampness, and contains flavonoids as main ingredient, wherein the higher content of ingredients include icariin, epimedin c, icarisid and icariin.
In recent years, with the increasing demand of epimedium herb extracts in the market, a large number of epimedium herb raw materials are dug with roots, so that wild raw material data are deficient, and the raw material yield is reduced year by year. However, the epimedium raw materials in the regions of the Chinese and Sichuan provinces and other Pacholymus have more raw materials, but the content of icariin in the raw materials of the epimedium in the regions is generally low, so that the utilization rate of the raw materials in the market is not high, and the waste of raw material resources is caused. Therefore, the method for efficiently extracting the icariin is provided, and particularly has important value for improving the utilization rate of the epimedium raw material in the Bashu region.
Disclosure of Invention
The invention provides an extraction method of icariin, which can obviously improve the content of the icariin in epimedium raw materials, particularly can enable the content of the icariin in epimedium raw materials in a Bashu region to reach more than 0.5 percent, and obviously improves the utilization rate of the epimedium raw materials.
The extraction method of icariin provided by the invention is to mix alcohol solution containing weak base with fresh epimedium raw material as solvent and then heat and extract;
the weak base-containing alcoholic solution is prepared from 50-95% by mass of alcoholic solution and 25-28% by mass of ammonia water solution according to the volume ratio of 90-99: 1-10, mixing;
wherein the alcohol solution is a methanol solution or an ethanol solution.
Preferably, the icariin is extracted by mixing alcohol solution containing weak base with fresh epimedium herb raw material and heating for extraction;
the weak base-containing alcoholic solution is prepared from 50-95% by mass of alcoholic solution and 25-28% by mass of ammonia water solution according to the volume ratio of 90-97: 3-10, mixing;
wherein the alcohol solution is a methanol solution or an ethanol solution.
Preferably, the heating extraction is reflux extraction or ultrasonic extraction.
More preferably, the reflux extraction is carried out for 3 times at 80 ℃ for 0.5-2.5 hours, the first feed-liquid ratio is 1kg: 7L, the second feed-liquid ratio is 1kg: 5L, and the third feed-liquid ratio is 1kg: 4L.
More preferably, the ultrasonic extraction is carried out for 1 hour at the temperature of 50-60 ℃, and the material-liquid ratio is 1kg: 20L.
Compared with the prior art, the invention has the following effects:
1. according to the extraction method of the icariin, the fresh epimedium raw material is heated and extracted by using an alcohol solution containing weak base as a solvent, and as a plurality of substances with similar structures to the icariin exist in the epimedium raw material, partial acyl substituted derivatives or other unknown derivatives can be deacylated and converted into the icariin under the condition of weak base, so that the content of the icariin in the epimedium extract is obviously increased;
2. the original enzyme system can be destroyed by treating the icariin with the weak base-containing alcohol solution, so that the icariin is prevented from being further degraded, and the loss of the icariin in the extraction process is reduced;
3. the content of the icariin in the sample obtained by the method is detected by adopting an icariin detection method provided in 'Chinese pharmacopoeia' of 2015 edition, so that the content of the icariin is remarkably improved, and particularly, the content of the icariin in epimedium raw materials in a Bashu region is improved to more than 0.5 percent from 0.01 to 0.1 percent, so that the utilization rate of the epimedium raw materials is remarkably improved;
4. the weak base alcohol solution is used as a solvent for extraction, compared with direct extraction by using a dilute ammonia solution, the subsequent purification treatment is more convenient, no solvent residue exists in the obtained extract, and the energy consumption can be saved; and the recovered alcohol can be recycled after being regulated into salt by hydrochloric acid, so that the alcohol loss is saved, compared with the extraction by inorganic salt, the reaction condition is more mild, simple and controllable, and the quality of the obtained extract is more stable.
Detailed Description
The embodiments of the present invention will be specifically described below by way of examples, which are intended to illustrate the present invention without further limiting the invention.
Example 1
A method for extracting icariin comprises removing impurities from fresh herba Epimedii raw material, pulverizing into small pieces with length not more than 2cm, loading into an extraction tank with addition amount not more than 1/2, adding prepared weak base-containing methanol solution, heating to 80 deg.C, reflux-extracting for 3 times (2.5 hr each time) with material-liquid ratio of 100kg: 700L for the first time, 100kg: 500L for the second time, 100kg: 400L for the third time, mixing the extractive solutions, filtering, concentrating the filtrate, and drying to obtain icariin extract;
wherein the methanol solution containing weak base is prepared by mixing a methanol solution with the mass fraction of 50% and an ammonia water solution with the mass fraction of 25% according to the volume ratio of 99: 1.
Through detection, the content of icariin is 0.52 percent based on dry epimedium raw material.
Example 2
A method for extracting icariin comprises removing impurities from fresh herba Epimedii raw material, pulverizing into small pieces with length not more than 2cm, loading into an extraction tank with addition amount not more than 1/2, adding prepared weak base-containing methanol solution, heating to 80 deg.C, reflux-extracting for 3 times (2.0 hr each time) with material-liquid ratio of 100kg: 700L for the first time, 100kg: 500L for the second time, 100kg: 400L for the third time, mixing the three extractive solutions, filtering, concentrating the filtrate, and drying to obtain icariin extract;
wherein the methanol solution containing weak base is prepared by mixing a methanol solution with the mass fraction of 95% and an ammonia water solution with the mass fraction of 28% according to the volume ratio of 90: 10.
Through detection, the content of icariin is 0.56 percent based on dry epimedium raw material.
Example 3
A method for extracting icariin comprises removing impurities from fresh herba Epimedii raw material, pulverizing into small pieces with length not more than 2cm, loading into extraction tank with addition amount not more than 1/2 of the volume of the extraction tank, adding prepared methanol solution containing weak base, heating to 80 deg.C, reflux-extracting for 3 times (0.5 hr each time) with first material-liquid ratio of 100kg: 700L, second material-liquid ratio of 100kg: 500L, and third material-liquid ratio of 100kg: 400L, mixing the three extractive solutions, filtering, concentrating the filtrate, and drying to obtain icariin extract;
wherein the methanol solution containing weak base is prepared by mixing a methanol solution with the mass fraction of 95% and an ammonia water solution with the mass fraction of 28% according to the volume ratio of 90: 10.
Through detection, the content of icariin is 0.61 percent based on dry epimedium raw material.
Example 4
A method for extracting icariin comprises removing impurities from fresh herba Epimedii raw material, pulverizing into small pieces with length not more than 2cm, loading into an extraction tank with addition amount not more than 1/2 of the volume of the extraction tank, adding prepared weak base-containing methanol solution, heating to 80 deg.C, reflux-extracting for 3 times (1.5 hr each time), with first material-liquid ratio of 100kg: 700L, second material-liquid ratio of 100kg: 500L, and third material-liquid ratio of 100kg: 400L, mixing the three extractive solutions, filtering, concentrating the filtrate, and drying to obtain icariin extract;
wherein the methanol solution containing weak base is prepared by mixing a methanol solution with the mass fraction of 70% and an ammonia water solution with the mass fraction of 28% according to the volume ratio of 24: 1.
Through detection, the content of icariin is 0.67 percent based on dry epimedium raw material.
Example 5
A method for extracting icariin comprises removing impurities from fresh herba Epimedii raw material, pulverizing into small pieces with length not more than 2cm, loading into extraction tank with addition amount not more than 1/2 of the volume of the extraction tank, adding prepared weak base-containing methanol solution, heating to 80 deg.C, reflux-extracting for 3 times (1.0 hr each time), with first material-liquid ratio of 100Kg: 700L, second material-liquid ratio of 100Kg: 500L, and third material-liquid ratio of 100Kg: 400L, mixing the three extractive solutions, filtering, concentrating the filtrate, and drying to obtain icariin extract;
wherein the methanol solution containing weak base is prepared by mixing a methanol solution with the mass fraction of 50% and an ammonia water solution with the mass fraction of 25% according to the volume ratio of 97: 3.
Through detection, the content of icariin is 0.56 percent based on dry epimedium raw material.
Example 6
A method for extracting icariin comprises the following steps of removing impurities from fresh epimedium raw materials, crushing the fresh epimedium raw materials into small pieces with the length not exceeding 2cm, filling the small pieces into an extraction tank with the addition amount not exceeding 1/2 of the volume of the extraction tank, finally adding 4% ammonia water solution serving as a solvent, heating to 80 ℃, carrying out reflux extraction for 3 times with 1.0 hour each time, wherein the material-liquid ratio of the first time is 100Kg: 700L, the material-liquid ratio of the second time is 100Kg: 500L, the material-liquid ratio of the third time is 100Kg: 400L, combining three extracting solutions, filtering, concentrating the filtrate and drying to obtain the icariin extract.
Through detection, the content of icariin is 0.53 percent based on dry epimedium raw material.
Example 7
A method for extracting icariin comprises removing impurities from fresh herba Epimedii raw material, pulverizing into small pieces with length not more than 2cm, loading into an extraction tank with addition amount not more than 1/2, adding prepared weak base-containing methanol solution, heating to 80 deg.C, reflux-extracting for 3 times (1.5 hr each time) with a first material-liquid ratio of 100kg: 700L, a second material-liquid ratio of 100kg: 500L, a third material-liquid ratio of 100kg: 400L, mixing the three extractive solutions, filtering, concentrating the filtrate, and drying to obtain icariin extract;
wherein the weak base-containing methanol solution is prepared by mixing a methanol solution with the mass fraction of 70% and an ammonia water solution with the mass fraction of 28% according to the volume ratio of 24: 1.
Through detection, the content of icariin is 0.84 percent based on dry epimedium raw material.
Example 8
A method for extracting icariin comprises removing impurities from fresh herba Epimedii, pulverizing into small pieces with length not more than 2cm, loading into an extraction tank with addition amount not more than 1/2, adding prepared weak base-containing methanol solution, heating to 80 deg.C, reflux-extracting for 3 times (1.5 hr each time) at a first material-liquid ratio of 100kg: 700L, a second material-liquid ratio of 100kg: 500L, a third material-liquid ratio of 100kg: 400L, mixing the three extractive solutions, filtering, concentrating the filtrate, and drying to obtain icariin extract;
wherein the weak base-containing methanol solution is prepared by mixing a methanol solution with the mass fraction of 70% and an ammonia water solution with the mass fraction of 28% according to the volume ratio of 24: 1.
Through detection, the content of icariin is 0.89 percent based on dry epimedium raw materials.
Comparative example 1
A method for extracting icariin comprises the following steps of removing impurities from fresh epimedium raw materials, crushing the fresh epimedium raw materials into small pieces with the length not exceeding 2cm, filling the small pieces into an extraction tank with the addition amount not exceeding 1/2 of the volume of the extraction tank, finally adding 70% by mass of methanol solution, performing reflux extraction at 80 ℃ for 3 times with 1.5 hours each time, wherein the material-liquid ratio of the first time is 100kg: 700L, the material-liquid ratio of the second time is 100kg: 500L, the material-liquid ratio of the third time is 100kg: 400L, combining the three extracting solutions, filtering, concentrating and drying the filtrate into powder, and obtaining the icariin extract.
Through detection, the content of icariin is 0.09 percent based on dry epimedium raw materials.
Comparative example 2
A method for extracting icariin comprises the following steps of removing impurities from fresh epimedium raw materials, crushing the fresh epimedium raw materials into small pieces with the length not more than 2cm, putting the small pieces into an extraction tank, adding 1/2 with the addition amount not more than the volume of the extraction tank, adding NaOH solution with the pH value of 9 as an extraction solvent, extracting for 3 times at the temperature of 80 ℃ for 2.0 hours each time, combining the three extracting solutions, filtering, concentrating the filtrate, and drying to obtain the icariin extract, wherein the material-liquid ratio of the first time is 100kg: 700L, the material-liquid ratio of the second time is 100kg: 500L, and the material-liquid ratio of the third time is 100kg: 400L.
Through detection, the content of icariin is 0.38 percent based on dry epimedium raw material.
Comparative example 3
A method for extracting icariin comprises the following steps of removing impurities from fresh epimedium raw materials, crushing the fresh epimedium raw materials into small pieces with the length not more than 2cm, filling the small pieces into an extraction tank, adding 1/2 with the addition amount not more than the volume of the extraction tank, using a methanol solution with the mass fraction of 70% as an extraction solvent, extracting for 3 times and 2.5 hours each time at 80 ℃ with the mass fraction of 1% of potassium ethoxide solution, combining the three extracting solutions, filtering, concentrating and drying the filtrate into powder to obtain the icariin extract, wherein the first material-liquid ratio is 100kg: 700L, the second material-liquid ratio is 100kg: 500L, and the third material-liquid ratio is 100kg: 400L.
Through detection, the content of icariin is 0.26 percent based on dry epimedium raw material.
Comparative example 4
A method for extracting icariin comprises the following steps of removing impurities from fresh epimedium raw materials picked in the wild Sichuan Nantong, crushing the fresh epimedium raw materials into small pieces with the length not more than 2cm, loading the small pieces into an extraction tank, adding 1/2 with the addition not more than the volume of the extraction tank, performing ultrasonic extraction for 2 hours by using an ethanol solution with the mass fraction of 90% as an extraction solvent according to the material-liquid ratio of 10g to 200m L, filtering an extraction solution, concentrating and drying a filtrate into powder to obtain the icariin extract.
Through detection, the content of icariin is 0.06 percent based on dry epimedium raw materials.
Comparative example 5
A method for extracting icariin comprises the following steps of removing impurities from fresh epimedium raw materials picked in Gansu wild, crushing the fresh epimedium raw materials into small pieces with the length not exceeding 2cm, filling the small pieces into an extraction tank, adding 1/2 with the addition not exceeding the volume of the extraction tank, taking 70% ethanol solution as an extraction solvent, carrying out reflux extraction at 80 ℃ for 3 times and 1.5 hours each time, wherein the material-liquid ratio of the first time is 100kg: 700L, the material-liquid ratio of the second time is 100kg: 500L, the material-liquid ratio of the third time is 100kg: 400L, combining filtrates of the three times, concentrating and drying the filtrate into powder, and obtaining the icariin extract.
Through detection, the content of icariin is 0.69 percent based on dry epimedium raw material.
Comparative example 6
A method for extracting icariin comprises the following steps of removing impurities from fresh epimedium raw materials picked in Korean wild, crushing the fresh epimedium raw materials into small pieces with the length not more than 2cm, loading the small pieces into an extraction tank, adding 1/2 with the addition not more than the volume of the extraction tank, taking 70% ethanol solution as an extraction solvent, carrying out reflux extraction at 80 ℃ for 3 times and 1.5 hours each time, wherein the material-liquid ratio of the first time is 100kg: 700L, the material-liquid ratio of the second time is 100kg: 500L, the material-liquid ratio of the third time is 100kg: 400L, combining filtrates of the three times, concentrating and drying the filtrate into powder, and obtaining the icariin extract.
Through detection, the content of icariin is 0.65 percent based on dry epimedium raw material.
Compared with the comparative examples 1-8 and the comparative examples 1-6, the extraction method provided by the application can obviously improve the content of icariin in the epimedium raw materials, and can improve the content of icariin in epimedium in a Bashu region to more than 0.5%, so that the utilization rate of the epimedium raw materials is obviously improved.
It should be noted that when the following claims refer to numerical ranges, it should be understood that both ends of each numerical range and any value between the two ends can be selected, and since the steps and methods used are the same as those of the embodiments, the preferred embodiments of the present invention have been described for the purpose of preventing redundancy, but once the basic inventive concept is known, those skilled in the art may make other variations and modifications to the embodiments. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (5)
1. A method for extracting icariin is characterized in that a weak base-containing alcohol solution is used as a solvent, and the solvent is mixed with a fresh epimedium herb raw material and then is heated and extracted;
the weak base-containing alcoholic solution is prepared from 50-95% by mass of alcoholic solution and 25-28% by mass of ammonia water solution according to the volume ratio of 90-99: 1-10, mixing;
wherein the alcohol solution is a methanol solution or an ethanol solution.
2. The method for extracting icariin according to claim 1, wherein the icariin is extracted by heating after mixing an alcohol solution containing weak base with a fresh epimedium raw material in the region of Bashu;
the weak base-containing alcoholic solution is prepared from 50-95% by mass of alcoholic solution and 25-28% by mass of ammonia water solution according to the volume ratio of 90-97: 3-10, mixing;
wherein the alcohol solution is a methanol solution or an ethanol solution.
3. The method for extracting icariin according to claim 1 or 2, wherein the heating extraction is reflux extraction or ultrasonic extraction.
4. The icariin extraction method according to claim 3, wherein the reflux extraction is carried out for 3 times at 80 ℃ for 0.5-2.5 hours each time, and the first feed-liquid ratio is 1kg: 7L, the second feed-liquid ratio is 1kg: 5L, and the third feed-liquid ratio is 1kg: 4L.
5. The method for extracting icariin according to claim 3, wherein the ultrasonic extraction is carried out for 1 hour at 50-60 ℃, and the material-liquid ratio is 1kg: 20L.
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| CN202010441939.7A CN111440222A (en) | 2020-05-22 | 2020-05-22 | Method for extracting icariin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114249777A (en) * | 2021-11-19 | 2022-03-29 | 安徽金源药业有限公司 | A kind of method for extracting icariin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020013280A1 (en) * | 2000-06-16 | 2002-01-31 | Zhongcheng Xin | Pharmaceutical composition for preventing and treating sexual dysfunction and vasculargenic disease comprising icariin |
| CN101416995A (en) * | 2007-10-24 | 2009-04-29 | 南京宇道科技开发有限公司 | Epimedium extract and preparation method, preparation and use thereof |
| CN106831913A (en) * | 2017-02-15 | 2017-06-13 | 鲁南制药集团股份有限公司 | A kind of preparation technology of icariin |
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2020
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