CN103288902A - Preparation method for extracting icariin from herba epimedii - Google Patents
Preparation method for extracting icariin from herba epimedii Download PDFInfo
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- CN103288902A CN103288902A CN201310173012XA CN201310173012A CN103288902A CN 103288902 A CN103288902 A CN 103288902A CN 201310173012X A CN201310173012X A CN 201310173012XA CN 201310173012 A CN201310173012 A CN 201310173012A CN 103288902 A CN103288902 A CN 103288902A
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- China
- Prior art keywords
- ethanol
- extract
- herba epimedii
- icarin
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 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 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 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 abstract 4
- 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 abstract 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 77
- 239000000284 extract Substances 0.000 claims abstract description 35
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 6
- 239000008213 purified water Substances 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000967 suction filtration Methods 0.000 claims description 20
- 241000893536 Epimedium Species 0.000 claims description 10
- 239000000287 crude extract Substances 0.000 claims description 10
- 235000018905 epimedium Nutrition 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract 3
- 238000002156 mixing Methods 0.000 abstract 2
- 238000005406 washing Methods 0.000 abstract 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000012567 medical material Substances 0.000 abstract 1
- 230000003712 anti-aging effect Effects 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000004097 bone metabolism Effects 0.000 description 1
- 210000000748 cardiovascular system Anatomy 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000002607 hemopoietic effect Effects 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a preparation method for extracting icariin from herba epimedii. The method is characterized by comprising the following steps: a, washing, cleaning and crushing a herba epimedii medical material, crushing to 10-30 meshes, carrying out reflux extraction by 60-70% of ethanol for 3-4 hours by 2-4 times; b, combining and mixing the filtrates, suction-filtering, decompressing, concentrating and recovering ethanol to obtain a primary extract, and then washing by 80-90% ethanol and purified water and recovering; c, extracting, standing and suction-filtering the primary extract to obtain a coarse extract; d, absorbing the coarse extract by a macroporous resin column, respectively eluting the macroporous resin column by 20-30% ethanol, 50-60% ethanol and 70-80% ethanol, combining and mixing the elutants and suction-filtering; e, drying the suction filtrate to obtain product icariin. The method provided by the invention has the advantage that the icariin is convenient and rapid to extract, the raw material is abundant in source, the production cost is low, the separating effect is remarkable, and the extraction purity is high.
Description
Technical field
The present invention relates to Herba Epimedii extract, relate in particular to a kind of preparation method who from Herba Epimedii, extracts icarin.
Background technology
Herba Epimedii has the effect of male hormone sample, anti-aging effects, and disease can play a role to immunity system and cardiovascular systems, has very high pharmaceutical use.Prove that through scientific research and clinical application the extract icarin of Herba Epimedii has the cardiovascular and cerebrovascular of increasing volume of blood flow, promotes hemopoietic function, immunologic function and bone metabolism, also has kidney invigorating and YANG supporting, the anti-ageing effect of waiting for a long time.In recent years, it is found that in the big right plant Herba Epimedii and contain a large amount of icarin that oneself has obtained encouraging progress therefrom to extract icarin.Icarin preparation method of the prior art, gained icarin purity is low, and the process cost is big, and extraction efficiency is not high, and preparation time is long.
Therefore, be badly in need of a kind of improved technology and solve existing this problem in the prior art.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who from Herba Epimedii, extracts icarin.
The technical solution used in the present invention is:
A kind of preparation method who extracts icarin from Herba Epimedii may further comprise the steps:
A: epimedium herb is rinsed well and pulverized, be crushed to the 10-30 order, with alcohol reflux 3-4 hour of 60-70%, extraction time was 2-4 time;
B: the merging of above-mentioned filtrate is mixed, and suction filtration, concentrating under reduced pressure reclaim ethanol and obtain extract just, use ethanol, the purified water flushing reuse of 80-90% again;
C: with above-mentioned extract just extract, leave standstill, suction filtration, get crude extract;
D: above-mentioned crude extract is adsorbed with macroporous resin column, use the ethanol of ethanol, 70-80% of ethanol, the 50-60% of 20-30% to the macroporous resin column wash-out more respectively, elutriant merges and mixes suction filtration;
E: above-mentioned suction filtration thing is carried out drying, get the finished product icarin.
The mass ratio of epimedium herb powder and ethanol is 1:10-15 among the described step a.
The drying temperature of described step e is 40-60 ℃.
Advantage of the present invention is: extract convenient and swiftly, raw material sources are abundant, low production cost, and separating effect is obvious, the dna purity height.
Embodiment
Embodiment 1
A kind of preparation method who extracts icarin from Herba Epimedii of the present invention may further comprise the steps:
A: epimedium herb is rinsed well and pulverized, be crushed to 15 orders, the alcohol reflux with 60% 3 hours, extraction time are 3 times, and the mass ratio of epimedium herb powder and ethanol is 1:10;
B: the merging of above-mentioned filtrate is mixed, and suction filtration, concentrating under reduced pressure reclaim ethanol and obtain extract just, wash reuse with 85% ethanol, purified water again;
C: with above-mentioned extract just extract, leave standstill, suction filtration, get crude extract;
D: above-mentioned crude extract is adsorbed with macroporous resin column, use 25% ethanol, 55% ethanol, 75% ethanol to the macroporous resin column wash-out more respectively, elutriant merges and mixes suction filtration;
E: above-mentioned suction filtration thing is carried out drying, and drying temperature is 60 ℃, gets the finished product icarin.
Extract convenient and swiftly, raw material sources are abundant, low production cost, and separating effect is obvious, the dna purity height.
Embodiment 2
A kind of preparation method who extracts icarin from Herba Epimedii of the present invention may further comprise the steps:
A: epimedium herb is rinsed well and pulverized, be crushed to 20 orders, the alcohol reflux with 65% 4 hours, extraction time are 3 times, and the mass ratio of epimedium herb powder and ethanol is 1:12;
B: the merging of above-mentioned filtrate is mixed, and suction filtration, concentrating under reduced pressure reclaim ethanol and obtain extract just, wash reuse with 80% ethanol, purified water again;
C: with above-mentioned extract just extract, leave standstill, suction filtration, get crude extract;
D: above-mentioned crude extract is adsorbed with macroporous resin column, use 20% ethanol, 50% ethanol, 70% ethanol to the macroporous resin column wash-out more respectively, elutriant merges and mixes suction filtration;
E: above-mentioned suction filtration thing is carried out drying, and drying temperature is 40-60 ℃, gets the finished product icarin.
Extract convenient and swiftly, raw material sources are abundant, low production cost, and separating effect is obvious, the dna purity height.
Embodiment 3
A kind of preparation method who extracts icarin from Herba Epimedii of the present invention may further comprise the steps:
A: epimedium herb is rinsed well and pulverized, be crushed to 25 orders, the alcohol reflux with 70% 3.5 hours, extraction time are 4 times, and the mass ratio of epimedium herb powder and ethanol is 1:15;
B: the merging of above-mentioned filtrate is mixed, and suction filtration, concentrating under reduced pressure reclaim ethanol and obtain extract just, wash reuse with 90% ethanol, purified water again;
C: with above-mentioned extract just extract, leave standstill, suction filtration, get crude extract;
D: above-mentioned crude extract is adsorbed with macroporous resin column, use 30% ethanol, 60% ethanol, 80% ethanol to the macroporous resin column wash-out more respectively, elutriant merges and mixes suction filtration;
E: above-mentioned suction filtration thing is carried out drying, and drying temperature is 60 ℃, gets the finished product icarin.
Extract convenient and swiftly, raw material sources are abundant, low production cost, and separating effect is obvious, the dna purity height.
Claims (3)
1. preparation method who extracts icarin from Herba Epimedii is characterized in that: may further comprise the steps:
A: epimedium herb is rinsed well and pulverized, be crushed to the 10-30 order, with alcohol reflux 3-4 hour of 60-70%, extraction time was 2-4 time;
B: the merging of above-mentioned filtrate is mixed, and suction filtration, concentrating under reduced pressure reclaim ethanol and obtain extract just, use ethanol, the purified water flushing reuse of 80-90% again;
C: with above-mentioned extract just extract, leave standstill, suction filtration, get crude extract;
D: above-mentioned crude extract is adsorbed with macroporous resin column, use the ethanol of ethanol, 70-80% of ethanol, the 50-60% of 20-30% to the macroporous resin column wash-out more respectively, elutriant merges and mixes suction filtration;
E: above-mentioned suction filtration thing is carried out drying, get the finished product icarin.
2. a kind of preparation method who extracts icarin from Herba Epimedii according to claim 1, it is characterized in that: the mass ratio of epimedium herb powder and ethanol is 1:10-15 among the described step a.
3. a kind of preparation method who extracts icarin from Herba Epimedii according to claim 1, it is characterized in that: the drying temperature of described step e is 40-60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310173012XA CN103288902A (en) | 2013-05-13 | 2013-05-13 | Preparation method for extracting icariin from herba epimedii |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310173012XA CN103288902A (en) | 2013-05-13 | 2013-05-13 | Preparation method for extracting icariin from herba epimedii |
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| CN103288902A true CN103288902A (en) | 2013-09-11 |
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| CN201310173012XA Pending CN103288902A (en) | 2013-05-13 | 2013-05-13 | Preparation method for extracting icariin from herba epimedii |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589020A (en) * | 2016-12-31 | 2017-04-26 | 北京颐方生物科技有限公司 | Method for extracting icariin from epimedium |
| CN107973829A (en) * | 2017-12-18 | 2018-05-01 | 四川合盛生物科技有限公司 | A kind of method that icariin is extracted from Herba Epimedii |
| 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 |
| CN109289939A (en) * | 2018-10-26 | 2019-02-01 | 劲牌生物医药有限公司 | A kind of method of heavy metal ion in removal Shorthorned Epimedium P.E |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999047137A1 (en) * | 1998-03-19 | 1999-09-23 | Phytoceutica, Inc. | Preparations containing licariin |
| US20050100618A1 (en) * | 1999-07-01 | 2005-05-12 | Thompson Ronald J. | Method of using a compound of menthol and L-arginine as a preparation for the topical delivery of Icariin, a herbal product produced from the Epimedium genus of the Berberidaceal family of plants, for the treatment of sexual dysfunction |
| CN1955186A (en) * | 2005-10-25 | 2007-05-02 | 浙江瑞康生物技术有限公司 | Producing process of 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 |
| CN101812100A (en) * | 2010-04-08 | 2010-08-25 | 苏州宝泽堂医药科技有限公司 | Method for preparing icariin |
| CN102718819A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | A kind of technology for preparing icariin |
| CN102807595A (en) * | 2011-06-02 | 2012-12-05 | 汉中天然谷生物科技有限公司 | Technique for preparing high-content (98 percent) icariin from Epimedium plant |
-
2013
- 2013-05-13 CN CN201310173012XA patent/CN103288902A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999047137A1 (en) * | 1998-03-19 | 1999-09-23 | Phytoceutica, Inc. | Preparations containing licariin |
| US20050100618A1 (en) * | 1999-07-01 | 2005-05-12 | Thompson Ronald J. | Method of using a compound of menthol and L-arginine as a preparation for the topical delivery of Icariin, a herbal product produced from the Epimedium genus of the Berberidaceal family of plants, for the treatment of sexual dysfunction |
| CN1955186A (en) * | 2005-10-25 | 2007-05-02 | 浙江瑞康生物技术有限公司 | Producing process of 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 |
| CN101812100A (en) * | 2010-04-08 | 2010-08-25 | 苏州宝泽堂医药科技有限公司 | Method for preparing icariin |
| CN102807595A (en) * | 2011-06-02 | 2012-12-05 | 汉中天然谷生物科技有限公司 | Technique for preparing high-content (98 percent) icariin from Epimedium plant |
| CN102718819A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | A kind of technology for preparing icariin |
Non-Patent Citations (1)
| Title |
|---|
| 王欣，等: "淫羊藿中淫羊藿苷提取工艺研究", 《中国药房》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589020A (en) * | 2016-12-31 | 2017-04-26 | 北京颐方生物科技有限公司 | Method for extracting icariin from epimedium |
| CN106589020B (en) * | 2016-12-31 | 2019-03-22 | 北京颐方生物科技有限公司 | A method of extracting icariin from Herba Epimedii |
| CN107973829A (en) * | 2017-12-18 | 2018-05-01 | 四川合盛生物科技有限公司 | A kind of method that icariin is extracted from Herba Epimedii |
| 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 |
| CN109289939A (en) * | 2018-10-26 | 2019-02-01 | 劲牌生物医药有限公司 | A kind of method of heavy metal ion in removal Shorthorned Epimedium P.E |
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Application publication date: 20130911 |