CN103288900A - Icariin preparation process flow - Google Patents

Icariin preparation process flow Download PDF

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Publication number
CN103288900A
CN103288900A CN2013101730007A CN201310173000A CN103288900A CN 103288900 A CN103288900 A CN 103288900A CN 2013101730007 A CN2013101730007 A CN 2013101730007A CN 201310173000 A CN201310173000 A CN 201310173000A CN 103288900 A CN103288900 A CN 103288900A
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Prior art keywords
solution
gained
temperature
extract
filter residue
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Pending
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CN2013101730007A
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Chinese (zh)
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张洋
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张洋
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Priority to CN2013101730007A priority Critical patent/CN103288900A/en
Publication of CN103288900A publication Critical patent/CN103288900A/en
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Abstract

The invention discloses an icariin preparation process flow which is characterized by comprising the following steps: a, taking herba epimedii medicinal materials, soaking the herba epimedii at normal temperature, soaking in a water bath at the temperature of 50-60 DEG C, filtering, and separating the filter residue and initial extract solution; b, putting the obtained filter residue in a water bath at the temperature of 60-80 DEG C, filtering, and separating the filter residue and the solution; c, merging the initial extract solution and solution, standing for 1-2 hours, separating the supernatant, and performing vacuum concentration to obtain the crude extract; d, allowing the obtained crude extract in step c to pass through a chromatographic column provided with a macroporous resin, introducing deionized water into the chromatographic column, introducing 70-80 percent ethanol into the chromatographic column, and collecting the eluent; and e, standing, crystallizing and filtering the eluent in step d, drying in the environment at the temperature of 50-60 DEG C for 5-6 hours to obtain the finished product. The preparation process flow has the advantages that the extraction process yield is high, the separation process is simple and convenient, no labor is consumed, and the extraction is convenient, simple and rapid.

Description

A kind of preparation technology's flow process of icarin
Technical field
The present invention relates to Herba Epimedii extract, relate in particular to a kind of preparation technology's flow process of icarin.
Background technology
Herba Epimedii is the cauline leaf of multiple Herba Epimedii such as Berberidaceae plant Herba Epimedii, arrow leaf Herba Epimedii, Epimedium wushanense, Herba Epimedii.Tool kidney invigorating and YANG supporting, strengthening the muscles and bones, the effect of dispelling rheumatism are usually used in treating sun dripping, the weakness of the waist and knees of erectile problem, urine and diseases such as coronary heart disease, chronic tracheitis, neurasthenia and poliomyelitis repeatly.Icarin is the main component of Herba Epimedii.To exist productive rate low for the extraction process of icarin in the prior art, and sepn process is very consuming time, consumption power, extracts shortcomings such as difficulty.
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 preparation technology's flow process that the purpose of this invention is to provide a kind of icarin.
The technical solution used in the present invention is:
A kind of preparation technology's flow process of icarin may further comprise the steps:
A: get epimedium herb, prior to soaking in water 2-5 hour under the normal temperature, placing temperature then is that 50-60 ℃ water-bath was soaked 4-5 hour, filters, and separates filter residue and extract solution just;
B: it is 60-80 ℃ water-bath 2-3 hour that the filter residue of gained among the step a is placed temperature, filters, and separates filter residue and solution;
C: the solution of gained among the first solution of the extract of gained and the step b among the combining step a, left standstill 1-2 hour, separate the top stillness of night, concentrating under reduced pressure gets crude extract;
D: the crude extract after the concentrating of gained among the step c by the chromatography column of macroporous resin is housed, is fed deionized water then toward chromatography column in, look for until effluent liquid, often feed the ethanol of 70-80% again in the chromatography column, the collection elutriant;
E: with the elutriant of gained in the steps d leave standstill, crystallization, filtration, be under 50-60 ℃ the environment dry 5-6 hour in temperature again, get the Herba Epimedii extract icarin.
Being evaporated to the crude drug mass ratio among the described step c is 1:0.5-1.
Drying means is spraying drying or vacuum-drying among the described step e.
Advantage of the present invention is: this extraction process productive rate height, and sepn process is easy, does not consume power, extracts conveniently succinctly fast, and this technical process is convenient to promote.
Embodiment
Embodiment 1
Preparation technology's flow process of a kind of icarin of the present invention may further comprise the steps:
A: get epimedium herb, prior to soaking in water 2 hours under the normal temperature, placing temperature then is that 60 ℃ water-bath was soaked 5 hours, filters, and separates filter residue and extract solution just;
B: it is 60 ℃ water-bath 2 hours that the filter residue of gained among the step a is placed temperature, filters, and separates filter residue and solution;
C: the solution of gained among the first solution of the extract of gained and the step b among the combining step a, left standstill 1 hour, separate the top stillness of night, concentrating under reduced pressure and crude drug mass ratio are 1:0.5, get crude extract;
D: the crude extract after the concentrating of gained among the step c by the chromatography column of macroporous resin is housed, is fed deionized water then toward chromatography column in, look for until effluent liquid, often feed 70% ethanol again in the chromatography column, the collection elutriant;
E: with the elutriant of gained in the steps d leave standstill, crystallization, filtration, be spraying drying 5 hours under 50 ℃ the environment in temperature again, get the Herba Epimedii extract icarin.
This extraction process productive rate height, sepn process is easy, does not consume power, extracts conveniently succinctly fast, and this technical process is convenient to promote.
Embodiment 2
Preparation technology's flow process of a kind of icarin of the present invention may further comprise the steps:
A: get epimedium herb, prior to soaking in water 5 hours under the normal temperature, placing temperature then is that 55 ℃ water-bath was soaked 4 hours, filters, and separates filter residue and extract solution just;
B: it is 70 ℃ water-bath 2.5 hours that the filter residue of gained among the step a is placed temperature, filters, and separates filter residue and solution;
C: the solution of gained among the first solution of the extract of gained and the step b among the combining step a, left standstill 1.2 hours, separate the top stillness of night, concentrating under reduced pressure and crude drug mass ratio are 1:0.8, get crude extract;
D: the crude extract after the concentrating of gained among the step c by the chromatography column of macroporous resin is housed, is fed deionized water then toward chromatography column in, look for until effluent liquid, often feed 75% ethanol again in the chromatography column, the collection elutriant;
E: with the elutriant of gained in the steps d leave standstill, crystallization, filtration, be vacuum-drying 6 hours under 60 ℃ the environment in temperature again, get the Herba Epimedii extract icarin.
Drying means is spraying drying or drying among the described step e.。
Embodiment 3
Preparation technology's flow process of a kind of icarin of the present invention may further comprise the steps:
A: get epimedium herb, prior to soaking in water 5 hours under the normal temperature, placing temperature then is that 60 ℃ water-bath was soaked 4 hours, filters, and separates filter residue and extract solution just;
B: it is 80 ℃ water-bath 2 hours that the filter residue of gained among the step a is placed temperature, filters, and separates filter residue and solution;
C: the solution of gained among the first solution of the extract of gained and the step b among the combining step a, left standstill 2 hours, separate the top stillness of night, concentrating under reduced pressure and crude drug mass ratio are 1:1, get crude extract;
D: the crude extract after the concentrating of gained among the step c by the chromatography column of macroporous resin is housed, is fed deionized water then toward chromatography column in, look for until effluent liquid, often feed 80% ethanol again in the chromatography column, the collection elutriant;
E: with the elutriant of gained in the steps d leave standstill, crystallization, filtration, be spraying drying 5 hours under 60 ℃ the environment in temperature again, get the Herba Epimedii extract icarin.
This extraction process productive rate height, sepn process is easy, does not consume power, extracts conveniently succinctly fast, and this technical process is convenient to promote.

Claims (3)

1. preparation technology's flow process of an icarin is characterized in that: may further comprise the steps:
A: get epimedium herb, prior to soaking in water 2-5 hour under the normal temperature, placing temperature then is that 50-60 ℃ water-bath was soaked 4-5 hour, filters, and separates filter residue and extract solution just;
B: it is 60-80 ℃ water-bath 2-3 hour that the filter residue of gained among the step a is placed temperature, filters, and separates filter residue and solution;
C: the solution of gained among the first solution of the extract of gained and the step b among the combining step a, left standstill 1-2 hour, separate the top stillness of night, concentrating under reduced pressure gets crude extract;
D: the crude extract after the concentrating of gained among the step c by the chromatography column of macroporous resin is housed, is fed deionized water then toward chromatography column in, look for until effluent liquid, often feed the ethanol of 70-80% again in the chromatography column, the collection elutriant;
E: with the elutriant of gained in the steps d leave standstill, crystallization, filtration, be under 50-60 ℃ the environment dry 5-6 hour in temperature again, get the Herba Epimedii extract icarin.
2. preparation technology's flow process of a kind of icarin according to claim 1, it is characterized in that: being evaporated to the crude drug mass ratio among the described step c is 1:0.5-1.
3. preparation technology's flow process of a kind of icarin according to claim 1, it is characterized in that: drying means is spraying drying or vacuum-drying among the described step e.
CN2013101730007A 2013-05-13 2013-05-13 Icariin preparation process flow Pending CN103288900A (en)

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Application Number Priority Date Filing Date Title
CN2013101730007A CN103288900A (en) 2013-05-13 2013-05-13 Icariin preparation process flow

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104829667A (en) * 2015-05-20 2015-08-12 诸城市浩天药业有限公司 Icariin H1 crystal form, as well as production method, pharmaceutical composition and application thereof
CN104844668A (en) * 2015-05-20 2015-08-19 诸城市浩天药业有限公司 Icariin form-alpha crystal, preparation method thereof and medicinal combination and application thereof
CN106421006A (en) * 2016-08-31 2017-02-22 无锡正大生物股份有限公司 Epimedium compound extract and preparation method thereof
CN111662346A (en) * 2020-07-07 2020-09-15 南京宸翔医药研究有限责任公司 Preparation of green intelligent high-purity icariin and pharmaceutical composition thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1283627A (en) * 2000-07-12 2001-02-14 徐绥绪 Process for extracting icariin from epimedium
CN1460684A (en) * 2003-06-05 2003-12-10 张利民 Epimedium extract and its production method
US20060134243A1 (en) * 2004-12-17 2006-06-22 Bionovo, Inc. Method of using extracts of epimedium species
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1283627A (en) * 2000-07-12 2001-02-14 徐绥绪 Process for extracting icariin from epimedium
CN1460684A (en) * 2003-06-05 2003-12-10 张利民 Epimedium extract and its production method
US20060134243A1 (en) * 2004-12-17 2006-06-22 Bionovo, Inc. Method of using extracts of epimedium species
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

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104829667A (en) * 2015-05-20 2015-08-12 诸城市浩天药业有限公司 Icariin H1 crystal form, as well as production method, pharmaceutical composition and application thereof
CN104844668A (en) * 2015-05-20 2015-08-19 诸城市浩天药业有限公司 Icariin form-alpha crystal, preparation method thereof and medicinal combination and application thereof
CN104844668B (en) * 2015-05-20 2017-12-19 诸城市浩天药业有限公司 A kind of icariside F orm alpha-crystal forms, its preparation method and its pharmaceutical composition and application
CN106421006A (en) * 2016-08-31 2017-02-22 无锡正大生物股份有限公司 Epimedium compound extract and preparation method thereof
CN111662346A (en) * 2020-07-07 2020-09-15 南京宸翔医药研究有限责任公司 Preparation of green intelligent high-purity icariin and pharmaceutical composition thereof

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Application publication date: 20130911