CN102603819A - Preparation method of rosavin - Google Patents
Preparation method of rosavin Download PDFInfo
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- CN102603819A CN102603819A CN2011100261949A CN201110026194A CN102603819A CN 102603819 A CN102603819 A CN 102603819A CN 2011100261949 A CN2011100261949 A CN 2011100261949A CN 201110026194 A CN201110026194 A CN 201110026194A CN 102603819 A CN102603819 A CN 102603819A
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- rosavin
- ethyl acetate
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Abstract
The invention relates to a preparation method of rosavin, which comprises the following steps: using rose rhodiola as a raw material to break into 20-60 meshes, adding 5-10 times of 80-90% ethanol to perform cold soaking extraction for 2-3 times, recycling the ethanol from the extracted liquid; adding an appropriate amount of water into concentrated liquid to dilute; filtering and adding an equivalent volume of ethyl acetate into the filtrate, agitating sufficiently and abandoning an ethyl acetate layer; adding polyamide resin to adsorb impurities; collecting the liquid passed through the column, depressurizing and concentrating; adding alumina, agitating and drying and then adding into a medium-pressure alumina column, performing gradient elution to the ethyl acetate by methanol, tracing and monitoring by high performance liquid chromatography (HPLC), collecting rosavin flows and recycling reagents; dissolving by anhydrous ethanol and adding an appropriate amount of diethyl ether to refrigerate and crystallize, drying the crystallized matter to obtain pure rosavin. The preparation method provided by the invention adopts the medium-pressure alumina column for separation is short in separation period, large in preparation quantity and suitable for industrial production.
Description
Technical field:
The present invention relates to a kind of preparation method of Rosavin, press alumina column to prepare the method for Rosavin in especially a kind of the employing.
Background technology:
Rosavin (rosavin) is the plain glycoside of phenylpropyl alcohol, molecular formula C
20H
28O
10, molecular weight 428.43, molecular structure
Physical properties: be the transparent needle crystal of white, 171 ℃-173 ℃ of fusing points, water-soluble, ethanol, methyl alcohol, butanols are insoluble in ether, chloroform, ETHYLE ACETATE.
Rosavin is mainly used in antifatigue, anoxia, releases the pressure, increases work efficiency and treats neural functional type disease.
Rosavin is mainly derived from the dry root and rhizome of the rose-red red-spotted stonecrop of Crassulaceae plant.
Its unique chemical activity composition of Root of Kirilow Rhodiola is network plug dimension rosavin (activity is the strongest), Lip river fine linen rosin, Luo Sailin rosarin; Rhodiolin and rhodioside, Root of Kirilow Rhodiola has caused the extensive concern of domestic and international food the world of medicine with its unique function, has been widely used in treatment hemoptysis, spitting of blood, pneumonia cough, women at present and has carried; Prevent and treat senile disease, especially important application is arranged, human health care in fields such as sports medical science, military medicine, aerospace medicines; Improve the health and benefit; Can be medicinal, also can make protective foods, generally be used for sports nutrition article and fat-reducing nutrient article abroad.Old and feeble as control; Improve the purposes of aspects such as mental and muscle power; As far back as the eighties in 20th century; Soviet Union health care department approved rhodiola rosea formulated product uses as stimulant, be widely used in pilot, cosmonaut, frogman, the sportsmen builds up resistance and human body to the resistibility of adverse environment, be activator by human body self potential; China has health care tea of Rhodiola rosea L, Rhodiola rosea capsules, Rhodiola root oral liquid, Root of Kirilow Rhodiola syrup, Root of Kirilow Rhodiola medicinal extract, rhodiola root wine etc. and comes into the market; As new medicine and food resource development and use, along with the further investigation from health care, prevention, 3 aspects of treatment, the application of Root of Kirilow Rhodiola has potential important meaning to medicine and pharmacology, sports medical science.
The at present domestic method that from Root of Kirilow Rhodiola, prepares Rosavin is less.Like patent CN1534040 " a kind of rhodiola active ingredient preparation method of extract ", alcohol extracting is disclosed, organic solvent extraction; The D101 purification with macroreticular resin separates; The preparation method of operations such as water and 10%-90% ethanol gradient elution, Rosavin content is low, does not separate obtaining monomer.Also has document " Radix Rhodiolae is isolated compound (I) first "; The method that the document adopts is that Radix Rhodiolae dry root and root are pulverized; 95% alcohol reflux No. 3 times behind the extracting solution concentrating under reduced pressure, is used sherwood oil, vinyl acetic monomer and n-butanol extraction successively.N-butanol extraction partly carries out silica gel column chromatography, uses sherwood oil. and vinyl acetic monomer, vinyl acetic monomer-methanol solvate system gradient elution obtain 10 flow points.4th, 7 and 9,3 flow points are used Sephadex LH-20 column chromatography (methyl alcohol), ODS column chromatography and the separation and purification of semimicro preparation HPLC respectively.As stated, the method specificity that existing extraction prepares Rosavin is low, and loaded down with trivial details.
Summary of the invention:
The technical problem that the present invention will solve provides a kind of method of Rosavin preparation, and this method is simple to operate, and products obtained therefrom content is high.
In order to solve the problems of the technologies described above, technical scheme of the present invention is following:
A kind of preparation method of Rosavin is characterized in that this method comprises the following steps:
1) raw material pulverizing 20-60 order, add 5-10 and doubly measure 80-90% ethanol cold soaking extraction 2-3 time, extracting solution reclaims ethanol, gets liquid concentrator;
2) above-mentioned liquid concentrator adds the suitable quantity of water dilution, filters, and filtrating adds equal-volume ETHYLE ACETATE fully stirs, and abandons ethyl acetate layer, adds polyamide resin absorption again, collects post and passes through liquid;
3) above-mentioned post adds aluminum oxide and mixes the appearance oven dry through the liquid concentrating under reduced pressure, presses alumina column in the adding; The ethyl acetate methanol gradient elution, the HPLC tracking monitor is collected the Rosavin flow point; Reclaim reagent, anhydrous alcohol solution adds an amount of ether refrigeration crystallization, and crystallisate is drying to obtain product.
The described raw material of step 1) is rose-red red-spotted stonecrop.
The described aluminum oxide of step 3) is a neutral alumina, granularity 120-300 order.
The described ethyl acetate methanol gradient elution of step 3) is: and 7-10BV ethyl acetate methanol solution (20: 3-5) → ethyl acetate methanol (7: 3).
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment:
The wash-out of Rosavin is followed the tracks of and is adopted HPLC (with reference to " the HPLC method is measured 3 kinds of content of effective in the rose-red red-spotted stonecrop " documents such as Lu Yide) among the following embodiment, and concrete grammar is following:
High-efficient liquid phase chromatogram condition:
Chromatographic column: C18 post (250mm * 4.6mm, 5 μ m);
Moving phase: acetonitrile: 2% phosphoric acid water (13: 87);
Flow velocity: 1.0mL/min;
Detect wavelength: 254nm;
Column temperature: 30 ℃;
Sample size: 10 μ l.
Embodiment 1:
Get rose-red red-spotted stonecrop raw material pulverizing 20 orders, get 1kg, add 10 times of amount 80% ethanol cold soakings and extract 2 times, extracted 8 hours at every turn; United extraction liquid reclaims ethanol, adds the suitable quantity of water dilution, filters, and filtrating adds equal-volume ETHYLE ACETATE and fully stirs; Abandon ethyl acetate layer, mother liquor adds polyamide resin absorption, collects post through the liquid concentrating under reduced pressure, adds the 50g aluminum oxide and mixes the appearance oven dry; Press alumina column (blade diameter length ratio 1: 15) in the adding, get 10BV ethyl acetate methanol solution (20: 3) ethyl acetate methanol wash-out, use ethyl acetate methanol solution (7: 3) HPLC tracking monitor again; Collect high density Rosavin flow point, anhydrous alcohol solution behind the recovery reagent drips ether to muddy refrigeration crystallization; Crystallisate leaches drying, gets the white, needle-shaped crystals Rosavin, content 98.1%.
Embodiment 2:
Get rose-red red-spotted stonecrop raw material pulverizing 60 orders, get 1kg, add 5 times of amount 90% ethanol cold soakings and extract 3 times, extracted 4 hours at every turn; United extraction liquid reclaims ethanol, adds the suitable quantity of water dilution, filters, and filtrating adds equal-volume ETHYLE ACETATE and fully stirs; Abandon ethyl acetate layer, mother liquor adds polyamide resin absorption, collects post through the liquid concentrating under reduced pressure, adds the 80g aluminum oxide and mixes the appearance oven dry; Press alumina column (blade diameter length ratio 1: 15) in the adding, get 7BV ethyl acetate methanol solution (4: 1) ethyl acetate methanol wash-out, use ethyl acetate methanol solution (7: 3) HPLC tracking monitor again; Collect high density Rosavin flow point, anhydrous alcohol solution behind the recovery reagent drips ether to muddy refrigeration crystallization; Crystallisate leaches drying, gets the white, needle-shaped crystals Rosavin, content 98.3%.
Embodiment 3:
Get rose-red red-spotted stonecrop raw material pulverizing 40 orders, get 1kg, add 8 times of amount 85% ethanol cold soakings and extract 2 times, extracted 10 hours at every turn; United extraction liquid reclaims ethanol, adds the suitable quantity of water dilution, filters, and filtrating adds equal-volume ETHYLE ACETATE and fully stirs; Abandon ethyl acetate layer, mother liquor adds polyamide resin absorption, collects post through the liquid concentrating under reduced pressure, adds the 100g aluminum oxide and mixes the appearance oven dry; Press alumina column (blade diameter length ratio 1: 15) in the adding, get 8BV ethyl acetate methanol solution (5: 1) ethyl acetate methanol wash-out, use ethyl acetate methanol solution (7: 3) HPLC tracking monitor again; Collect high density Rosavin flow point, anhydrous alcohol solution behind the recovery reagent drips ether to muddy refrigeration crystallization; Crystallisate leaches drying, gets the white, needle-shaped crystals Rosavin, content 98.5%.
Claims (4)
1. the preparation method of a Rosavin is characterized in that this method comprises the following steps:
1) raw material pulverizing 20-60 order, add 5-10 and doubly measure 80-90% ethanol cold soaking extraction 2-3 time, extracting solution reclaims ethanol, gets liquid concentrator;
2) above-mentioned liquid concentrator adds the suitable quantity of water dilution, filters, and filtrating adds equal-volume ETHYLE ACETATE fully stirs, and abandons ethyl acetate layer, adds polyamide resin absorption again, collects post and passes through liquid;
3) above-mentioned post adds aluminum oxide and mixes the appearance oven dry through the liquid concentrating under reduced pressure, presses alumina column in the adding; The ethyl acetate methanol gradient elution, the HPLC tracking monitor is collected the Rosavin flow point; Reclaim reagent, anhydrous alcohol solution adds an amount of ether refrigeration crystallization, and crystallisate is drying to obtain product.
2. the preparation method of a kind of Rosavin as claimed in claim 1 is characterized in that the described raw material of step 1) is rose-red red-spotted stonecrop.
3. the preparation method of a kind of Rosavin as claimed in claim 1 is characterized in that the described aluminum oxide of step 3) is a neutral alumina, granularity 120-300 order.
4. the preparation method of a kind of Rosavin as claimed in claim 1 is characterized in that the described ethyl acetate methanol gradient elution of step 3) is: and 7-10BV ethyl acetate methanol solution (20: 3-5) → ethyl acetate methanol (7: 3).
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|---|---|---|---|
| CN2011100261949A CN102603819A (en) | 2011-01-25 | 2011-01-25 | Preparation method of rosavin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100261949A CN102603819A (en) | 2011-01-25 | 2011-01-25 | Preparation method of rosavin |
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| CN102603819A true CN102603819A (en) | 2012-07-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447901A (en) * | 2014-11-13 | 2015-03-25 | 安徽尚善生物科技股份有限公司 | Method for preparing rosavin from rose rhodiola rosea |
| CN111707742A (en) * | 2020-06-05 | 2020-09-25 | 太阳树（厦门）生物工程有限公司 | Method for simultaneously detecting multiple components in rhodiola rosea by HPLC |
| CN113956303A (en) * | 2021-09-30 | 2022-01-21 | 湖南绿蔓生物科技股份有限公司 | Method for simultaneously extracting salidroside, rosavin and polysaccharide from rhodiola rosea |
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| SU1162813A1 (en) * | 1983-11-28 | 1985-06-23 | Всесоюзный Научно-Исследовательский Институт Лекарственных Растений | Method of obtaining (3,7-dimethyl-octa-2,6-dien-1,4-diol)-1-0-beta-d-glucopyranoside |
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| WO2005072749A1 (en) * | 2004-01-29 | 2005-08-11 | Halevie-Goldman, Brian, D. | Compositions and methods for homocsyteine regulation |
| CN101392011A (en) * | 2008-11-05 | 2009-03-25 | 江南大学 | Isolation and purification method of natural salidroside |
| JP2009209045A (en) * | 2008-02-29 | 2009-09-17 | Univ Kinki | Fat metabolism-improving agent obtained from sedum sarmentosum, medicine or food containing the same and new megastigman and flavonoid compound obtained from the sedum sarmentosum |
| CN101775048A (en) * | 2010-02-01 | 2010-07-14 | 南京泽朗医药科技有限公司 | Method for preparing salidroside from rhodiola rosea |
| CN101775049A (en) * | 2010-02-08 | 2010-07-14 | 苏州宝泽堂医药科技有限公司 | Method for extracting and purifying salidroside from glossy privet fruit |
| CN101289478B (en) * | 2007-04-20 | 2011-04-20 | 中国科学院大连化学物理研究所 | Method for separating and preparing salidroside |
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2011
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Patent Citations (9)
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| SU1162813A1 (en) * | 1983-11-28 | 1985-06-23 | Всесоюзный Научно-Исследовательский Институт Лекарственных Растений | Method of obtaining (3,7-dimethyl-octa-2,6-dien-1,4-diol)-1-0-beta-d-glucopyranoside |
| WO2004030684A2 (en) * | 2002-10-03 | 2004-04-15 | Herbal Science, Llc | Kavalactone product |
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| WO2005072749A1 (en) * | 2004-01-29 | 2005-08-11 | Halevie-Goldman, Brian, D. | Compositions and methods for homocsyteine regulation |
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| JP2009209045A (en) * | 2008-02-29 | 2009-09-17 | Univ Kinki | Fat metabolism-improving agent obtained from sedum sarmentosum, medicine or food containing the same and new megastigman and flavonoid compound obtained from the sedum sarmentosum |
| CN101392011A (en) * | 2008-11-05 | 2009-03-25 | 江南大学 | Isolation and purification method of natural salidroside |
| CN101775048A (en) * | 2010-02-01 | 2010-07-14 | 南京泽朗医药科技有限公司 | Method for preparing salidroside from rhodiola rosea |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447901A (en) * | 2014-11-13 | 2015-03-25 | 安徽尚善生物科技股份有限公司 | Method for preparing rosavin from rose rhodiola rosea |
| CN111707742A (en) * | 2020-06-05 | 2020-09-25 | 太阳树（厦门）生物工程有限公司 | Method for simultaneously detecting multiple components in rhodiola rosea by HPLC |
| CN113956303A (en) * | 2021-09-30 | 2022-01-21 | 湖南绿蔓生物科技股份有限公司 | Method for simultaneously extracting salidroside, rosavin and polysaccharide from rhodiola rosea |
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Application publication date: 20120725 |