CN1246325C - Preparation method of hongjintian effective component extract - Google Patents
Preparation method of hongjintian effective component extract Download PDFInfo
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- CN1246325C CN1246325C CN 03116051 CN03116051A CN1246325C CN 1246325 C CN1246325 C CN 1246325C CN 03116051 CN03116051 CN 03116051 CN 03116051 A CN03116051 A CN 03116051A CN 1246325 C CN1246325 C CN 1246325C
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Abstract
The present invention discloses a method for preparing the effective component extracts of rhodiola root, which belongs to the technical field of plant chemistry. Extracts with different active components are prepared from the same parts in rhodiola root, and contain 5% to 95% of rhodiola root glycoside and 95% to 5% of Rosavin in a content ratio.
Description
Technical field
The invention belongs to the vegetable chemistry technical field.Be specifically related to a kind of rhodiola active ingredient preparation method of extract.
Background technology
Root of Kirilow Rhodiola (Rhodiola rosea) is perennial herb or shrub plant, mainly be distributed in USSR (Union of Soviet Socialist Republics) the Far East Area and Northeast China, northwest, high and cold area such as southwest, its pharmacologically active is similar to west pool Leah genseng, glossy ganoderma, Radix Panacis Quinquefolii mainly shows: anti-hypoxia, antifatigue, resisting microwave radiation, remove interior free yl, regulate and recovery human body metabolism balance.Wherein studying maximum activeconstituentss is rhodioside (Salidroside) and tyrosol (Tyrosol), along with deepening continuously of domestic and international research, find to have in the Root of Kirilow Rhodiola a kind of than the active better composition-Rosavin of rhodioside, and this activeconstituents is widely used in the protective foods.
Rosavin, English Rosavin by name, chemistry β by name-(E)-Chinese cassia tree alcohol radical-O-(6 '-O-α-L-arabopyranose base)-the D-glucopyranoside, its structural formula is as follows:
The content of Rosavin in the Root of Kirilow Rhodiola crude drug is very low, because the chemical polarity of Rosavin and rhodioside is very near, from thin-layer chromatography (TLC), both Rf values are approaching, be difficult to the two is separated, so the monomeric technology difficulty of preparation Rosavin is bigger.In addition, contain Rosavin this activeconstituents Root of Kirilow Rhodiola medicinal material kind also seldom, resources supplIes is relatively limited, so like this for the constraint beyond doubt of the large-scale development of health rhodiola product.
Studies show that Root of Kirilow Rhodiola has anti-hypoxia, antifatigue, resisting microwave radiation, remove interior free yl, regulate and the effect of recovery human body metabolism equilibrated.Initial application is to be used to improve sports achievement as the protective foods of cosmonaut's anti-hypoxia and passive movement person, and the raw material that has added Radix Rhodiolae extract in the increasing protective foods has been arranged now.
In the past people to study more activeconstituents be Root of Kirilow Rhodiola and tyrosol, along with domestic and international further investigation is in recent years found, the pharmacologically active of Rosavin in the Root of Kirilow Rhodiola (Rosavin) composition far is better than rhodioside and tyrosol, thereby become the new lover of healthy food material, so better develop this activeconstituents of Rosavin, expanded very big space for the development of health industry undoubtedly.
Summary of the invention
Technical problem to be solved by this invention is to design a kind of preparation method, can extract effectively to obtain different effective component extracts in the Root of Kirilow Rhodiola.
The invention provides a kind of rhodiola active ingredient preparation method of extract, this method comprises the following steps:
1. draw materials: choose Radix Rhodiolae raw material 200g, the ethanolic soln that adds 5-8 times of 65-85% extracts three times, obtains extracting solution.Reclaim the ethanol in the extracting solution, obtain medicinal extract, use ethyl acetate and n-butanol extraction respectively, select the n-butanol extraction position.
2. separation and purification: get n-butyl alcohol extract, add 3-5 water-dispersion doubly, use activated carbon decolorizing then, the filtrate that obtains is gone up macroporous resin column, and first water wash-out is used the ethanol elution of 10-90% gradient then, be TLC and HPLC simultaneously and follow the tracks of, collect the ethanol eluate of 50-70%.
3. obtain finished product: with the ethanol eluate of collecting, reclaim ethanol, drying obtains the ratio extract.
4. check: content detection and reference substance through HPLC compare, and analyze the relation of ratio extract, and the content that wherein contains rhodioside (Salidroside) is in the 5-95% interval, and the content of Rosavin (Rosavin) is in the 95-5% scope.
Because the crude drug place of production difference of Root of Kirilow Rhodiola, the kind difference is so the content of wherein contained rhodioside and Rosavin composition is also different.The selected raw material of content of the present invention is the Radix Rhodiolae kind.In the embodiment of research, consider the alcoholic acid gradient elution, may cause partial loss, last yield decreases.
The Root of Kirilow Rhodiola activeconstituents that the application of the invention preparation method obtains is the different activities component extract for preparing in the same extraction of Root of Kirilow Rhodiola position, and their content ratio is rhodioside (Salidroside) 5-95: Rosavin (Rosavin) 95-5.
Method technology of the present invention is simple, can once obtain plurality of active ingredients, and organic solvent residual is few, and can effectively improve the active component content in the Root of Kirilow Rhodiola, is applicable to large-scale production, does not see domestic and international any report so far.
Description of drawings
Fig. 1 designs the schema that preparation contains the Root of Kirilow Rhodiola activeconstituents
Rosavin in Fig. 2 Root of Kirilow Rhodiola (Rosavin) standard substance collection of illustrative plates
Provide for Na Bei company by Tianjin spike company
Fig. 3 is made collection of illustrative plates by the sample that obtains, and wherein contains Rosavin (Rosavin) about 8%
Provide for Na Bei company for testing the chamber by Tianjin spike company center, because it is less to contain composition in the sample, so assorted peak is more about 5 minutes
The formed mass spectrum of Rosavin in Fig. 4 sample, Rosavin molecular weight 428 in the mapping process, uses the sub-Na+ that pluses fifteen, molecular ion peak 451.07, meet contain in the sample activeconstituents Rosavin
Fig. 5 has further verified the Rosavin composition in the sample, and two molecule Rosavin combine with a part Na, obtain molecular ion peak 879.17, i.e. 428 * 2+23 * 1=879
Provide by Shanghai Institute of Pharmaceutical Industry's mass spectrum chamber
Embodiment
Embodiment one
Get the crude drug 200g of Radix Rhodiolae, grind, ethanolic soln with 65% extracts three times, each alcoholic acid amount that adds is respectively 1200ml, 1000ml, 800ml, obtain extracting solution, concentrate the back medicinal extract 19.4g that weighs, use ethyl acetate (1: 1) and propyl carbinol (1: 1) to extract respectively then three times, get butanol extraction liquid, concentrate weigh 5.3g, add 3 times water dissolution, 3.8g weighs behind activated carbon decolorizing, last D-101 type macroporous resin exchange column, first water carries out wash-out, uses 10% respectively then, 30%, 50%, 70%, 90% ethanol carries out gradient elution, collect the wash-out position of 50-70%, obtain the effective part extract 1.2g of Root of Kirilow Rhodiola, the about 1.03g of rhodioside wherein, Rosavin 0.011g.
Embodiment two
Get the crude drug 1kg of Radix Rhodiolae, grind, dissolve with ethanol with 75% extracts three times, obtain extracting solution, concentrate the back medicinal extract 118g that weighs, use ethyl acetate (1: 1) and propyl carbinol (1: 1) to extract respectively then three times, get butanol extraction liquid, concentrate 26.7g, after the water dissolution of 4 times of amounts, obtain 14.5g, last AB-8 type macroporous resin exchange column through activated carbon decolorizing, elder generation's water wash-out, use 30% again, 50%, 70%, 90% ethanol gradient elution, the wash-out position of collecting 50-70% obtains the effective part extract 4.9g of Root of Kirilow Rhodiola, rhodioside 2.79g wherein, Rosavin is 1.74g.
Embodiment three
Get the raw material 2kg of Root of Kirilow Rhodiola, grind, dissolve with ethanol with 85% extracts three times, obtain extracting solution, concentrate the back medicinal extract 237g that weighs, use ethyl acetate (1: 1) and propyl carbinol (1: 1) to extract respectively then three times, get butanol extraction liquid, concentrate 58.7g, after the water dissolution of 5 times of amounts, obtain 30.2g, last D-101 type macroporous resin exchange column through activated carbon decolorizing, elder generation's water wash-out, use 30% again, 50%, 70%, 90% ethanol carries out gradient elution, collects the wash-out position of 50-70%, obtains the effective part extract 11.4g of Root of Kirilow Rhodiola, rhodioside 2.39g wherein, Rosavin is 8.21g.
Testing conditions: (accompanying drawing spectrum)
1. rhodioside:
Moving phase: water: methyl alcohol: second eyeball=70: 25: 5
Detect wavelength: 273nm
Flow velocity: 0.6ml/min
Chromatographic column: ODS C
18250*4.6mm 5um
2. Rosavin:
Moving phase: water: second eyeball=75: 25
Detect wavelength: 252nm
Flow velocity: 0.8ml/min
Chromatographic column: ODS C
18250*4.6mm 5um
Claims (1)
1. a rhodiola active ingredient preparation method of extract is characterized in that this method comprises the following steps:
1) draw materials: choose an amount of Root of Kirilow Rhodiola raw material, the extraction using alcohol of adding 65-85% three times obtains extracting solution.Reclaim ethanol and obtain Root of Kirilow Rhodiola medicinal extract,, select the n-butanol extraction position with ethyl acetate, n-butanol extraction;
2) separation and purification: get n-butyl alcohol extract, add an amount of water-dispersion, activated carbon decolorizing gets filtrate and goes up D-101 type macroporous resin column, and the ethanol elution of water and different gradients is TLC and HPLC simultaneously and is followed the tracks of, and collects the ethanol eluate of 50-70%;
3) obtain finished product: with the ethanol eluate of collecting, reclaim ethanol, drying obtains the ratio extract;
4) check: content detection and reference substance through HPLC compare, and analyze the relation of ratio extract, and the content that wherein contains rhodioside is in the 5-95% interval, and the content of Rosavin is in the 95-5% scope.
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| CN 03116051 CN1246325C (en) | 2003-03-28 | 2003-03-28 | Preparation method of hongjintian effective component extract |
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| CN 03116051 CN1246325C (en) | 2003-03-28 | 2003-03-28 | Preparation method of hongjintian effective component extract |
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| CN1246325C true CN1246325C (en) | 2006-03-22 |
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| CN 03116051 Expired - Fee Related CN1246325C (en) | 2003-03-28 | 2003-03-28 | Preparation method of hongjintian effective component extract |
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Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1931214B (en) * | 2005-09-14 | 2011-07-20 | 山东轩竹医药科技有限公司 | Medicine composition of rhodiola root and puerarin |
| CN1990496B (en) * | 2005-12-29 | 2010-05-05 | 复旦大学 | Process for preparing high purity rhodiola root glycosides |
| CN101281175B (en) * | 2007-06-12 | 2011-08-17 | 上海谱尼测试技术有限公司 | Method for measuring salidroside in food |
| CN101928638B (en) * | 2009-06-23 | 2013-04-17 | 湖北中烟工业有限责任公司 | Rhodiola rosea extract and application thereof as tobacco product additive |
| GB2488303A (en) * | 2009-12-07 | 2012-08-22 | Univ Hong Kong Science & Techn | CDK5 inhibitors and therapeutic uses thereof |
| CN101766670B (en) * | 2010-02-23 | 2012-05-23 | 上海应用技术学院 | Rhodiola rosea polyphenol microcapsule and preparation method |
| CN102603819A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Preparation method of rosavin |
| CN102228501B (en) * | 2011-06-16 | 2012-11-21 | 中国人民解放军第四军医大学 | Chinese medicinal composition for resisting anoxia and fatigue and preparation method thereof |
| CN102875614A (en) * | 2012-10-05 | 2013-01-16 | 南通四海植物精华有限公司 | Method for preparing salidroside from rose roots |
| CN103012512B (en) * | 2013-01-16 | 2016-03-30 | 河北科技大学 | The separation purification method of rhodioloside in neutral red red-spotted stonecrop |
| CN103467539B (en) * | 2013-09-30 | 2015-10-07 | 桂林茗兴生物科技有限公司 | A kind of method extracting Rosavin from rose-red red-spotted stonecrop |
| CN104447901B (en) * | 2014-11-13 | 2017-06-06 | 安徽尚善生物科技股份有限公司 | A kind of method that network match dimension is prepared in the rhodiola root from rose |
| CN105962281A (en) * | 2016-05-03 | 2016-09-28 | 王胜 | Sea salt and rhodiolarosea extract containing plant salt and method for preparing plant salt by using preheating enrichment crystallization process |
| CN107312047B (en) * | 2017-08-06 | 2020-05-01 | 中国科学院兰州化学物理研究所 | Method for synchronously separating and preparing salidroside and rosavin from rhodiola rosea |
| CN109875110B (en) * | 2019-04-16 | 2022-03-25 | 吉林烟草工业有限责任公司 | Rhodiola rosea extract, preparation method and application thereof and prepared tobacco shreds |
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