CN104447901B - A kind of method that network match dimension is prepared in the rhodiola root from rose - Google Patents
A kind of method that network match dimension is prepared in the rhodiola root from rose Download PDFInfo
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- CN104447901B CN104447901B CN201410638395.8A CN201410638395A CN104447901B CN 104447901 B CN104447901 B CN 104447901B CN 201410638395 A CN201410638395 A CN 201410638395A CN 104447901 B CN104447901 B CN 104447901B
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- Prior art keywords
- concentrated
- resin
- rhodiola root
- alcohol
- rose
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/18—Acyclic radicals, substituted by carbocyclic rings
-
- 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
Abstract
A kind of method the invention discloses network match dimension is prepared in rhodiola root from rose, it includes raw material pre-treatment, extractions, once filtering, macroreticular resin, again concentration, mistake resin, UF membrane, the step such as spray drying excessively.Compared with other method, present invention employs column chromatography method twice, the method for UF membrane, the present invention is more suitable for industrialized production.Product Safety that the inventive method is obtained is high, purity is high, and quality is high, high income.
Description
Technical field
The present invention relates to health products, the method that network match dimension is prepared in a kind of rhodiola root from rose of field of medicaments, specifically
Relate to a kind of utilization crush, extract, purified by macroporous resin enrichment, again purifying resin, UF membrane obtains network match and ties up product
The method of product.
Background technology
Rose rhodiola root is perennial herb, high 10-20 centimetres.Root is sturdy, and cone, meat is isabelline, root neck tool
Most fibrous roots.Rhizome is short, thick shape, cylinder, the leaf of the flakey arranged by most imbricates.Extracted out from the axil on stem top
There is fleshy leaf several scape, scape top and the bottom, and blade is oval, and edge tool sawtooth, tip is sharp, base portion wedge shape, several stockless.
Cyme basidixed, premium color.Rose rhodiola root is a kind of famous traditional medicinal plant, great Liang Yan in China and the East European countries
Study carefully and show to be slept with antifatigue, enhancing learning and memory, stimulating central nervous system system, raising operating efficiency, resist oxygen lack, improvement
Sleep, prevent the different physiological roles such as altitude sickness, anticancer, be currently a kind of medicine-food two-purpose " adapting to former " plant being popular.Its
Main active component includes rhodioside (salidroside) and its tyrosol, network match dimension etc..Wherein network match dimension hplc reaches
More than 0.7%.But the network match dimension extracted from rose rhodiola root using prior art haves the shortcomings that purity is low, yield is low,
Cause healthcare function unstable, it is impossible to meet the market demand.
The content of the invention
A kind of method it is an object of the invention to provide network match dimension is prepared in rhodiola root from rose, the method high income,
Product content is high, functional component stabilization, is adapted to industrialized production,
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of method that network match dimension is prepared in rhodiola root from rose, comprises the following steps：
（1）Raw material pre-treatment：Take and dry rose rhodiola root raw material and be crushed to 20-40 mesh；
（2）Extract：Rhodiola root after will be broken, plus mass ratio is that 50-80% ethanol waters extract refluxing extraction three times,
Extraction solvent material ratio is respectively 8：1；6：1；4：1；Extraction time is 2-3 hours.
（3）Extract solution is concentrated；It is concentrated in vacuo to without alcohol taste.
（4）Centrifugation：Concentrate is carried out into centrifugal filtration；
（5）Cross post：Adsorbed using the macroporous absorbent resin anticipated；Again with purifying washing post；Finally with washing
The network match dimension desorption that de- liquid will be enriched on resin gets off to collect eluent；
（6）Concentration：Eluent is concentrated in vacuo to without alcohol state；
（7）Post is crossed again：By last time concentrate PRP resin adsorption, parsed with alcohol；
（8）Film is concentrated：Cross 40-60 nano-precisions；
（9）Spray drying is obtained final product.
Described step（3）Middle utilization temperature concentrated in vacuo is less than 60 DEG C, and vacuum is 0.08pma, and concentration time is
No more than 2 hours, it is concentrated into without alcohol state.
Described step（4）Middle to carry out enriching and purifying using D101, HPD-100 macroreticular resin, concentrate is in adsorption rate
It is 1.0-1.5bv/h, washing speed is 2-3 bv/h, it is colourless to be washed to lower column liquid, and wash-out concentration of alcohol is 50-70%, wash-out
Speed is 1.0-1.2bv/h.
Described step（7）Middle resin prepares resin for a kind of PRP, and adsorption rate is 0.5-1.0bv/h, and adsorbance is
0.2-0.4BV, eluent is 10-30% ethanol solution 3-5bv, and pressure is 0.2-0.4Mpa, TCL monitoring.
Described step（10）Middle spray drying EAT is 170-180 DEG C, and leaving air temp is 70-80 DEG C.
Beneficial effects of the present invention：
（1）Compared with other method, the obtained product network match dimension hplc of the present invention is 90%, and Determination of Salidroside 5% keeps
The big active ingredient of rhodiola root two, is more suitable for medicines and health protection application；
（2）The inventive method concentration process uses vacuum concentration mode, keeps product performance to have effect well；
（3）The inventive method is simple using equipment needed for preparing resin methods purifying, and impurity-eliminating effect is good, is more suitable for producing
Industry metaplasia is produced；
（4）The effect of concentration and purifying is act as in the present invention using UF membrane, the purity of product is further improved；
（5）The high income of product in the present invention, yield is 1.2%, and step is simply more suitable for industrialized production.
Specific embodiment
With reference to example, the present invention will be further described.
Embodiment
（1）Title dries rhodiola root 200kg, and network matches dimension hplc 1.38%, Determination of Salidroside 0.92%, by being crushed to
20 mesh；Plus mass ratio is that 60% ethanol water extracts refluxing extraction three times, Extraction solvent material ratio is respectively 8：1；6：1；4：
1；Extraction time is 2 hours；
（3）By extract solution mix concentrate, vacuum be temperature concentrated in vacuo be less than 60 DEG C, vacuum be not less than be
0.08pma, concentration time is, no more than 2 hours, to be concentrated into without alcohol state, and density is in 1.05-1.10；
（4）Concentrate filter cloth is centrifuged for 500 mesh；
（5）Processed good D101 macroreticular resins 200L dress posts, centrifugate is 1.0-1.5bv/h, washing in adsorption rate
Speed is 2-3 bv/h, and it is colourless to be washed to lower column liquid, and wash-out concentration of alcohol is 50-70%, and elution speed is 1.0-1.2bv/h.
Eluent is collected to be concentrated into without alcohol taste；
（6）Concentrate prepares resin through PRP, and adsorption rate is 0.5-1.0bv/h, and adsorbance is 0.2-0.4BV, wash-out
Liquid is 10-30% ethanol solution 3-5bv, and pressure is 0.2-0.4Mpa, and TCL monitoring, collection has the partially liq of content, and film is dense
It is reduced to density 1.05；
（7）Spray drying：The spray-dried EAT of concentrate is 170-180 DEG C, and leaving air temp is 70-80 DEG C.Receive
Collection xeraphium：2.38kg, yield is：1.19%, network match dimension hplc is 92%, and rhodioside is 4.8%.
Claims (1)
1. a kind of method that network match dimension is prepared in rhodiola root from rose, it is characterised in that comprise the following steps：
（1）Raw material pre-treatment：Take and dry rose rhodiola root raw material and be crushed to 20-40 mesh；
（2）Extract：Rhodiola root after will be broken, plus mass ratio is that 50-80% ethanol waters extract refluxing extraction three times, is extracted
Solvent material ratio is respectively 8：1；6：1；4：1；Extraction time is 2-3 hours；
（3）Extract solution is concentrated；It is concentrated in vacuo to without alcohol taste；
（4）Centrifugation：Concentrate is carried out into centrifugal filtration；
（5）Cross post：Adsorbed using the macroporous absorbent resin anticipated；Again with purifying washing post；Finally use eluent
The network match dimension desorption that will be enriched on resin gets off to collect eluent；
（6）Concentration：Eluent is concentrated in vacuo to without alcohol state；
（7）Post is crossed again：By last time concentrate PRP resin adsorption, parsed with alcohol；
（8）Film is concentrated：Cross 40-60 nano-precisions；
（9）Spray drying is obtained final product；Described step（3）Middle utilization temperature concentrated in vacuo is less than 60 DEG C, and vacuum is
0.08MPa, concentration time is, no more than 2 hours, to be concentrated into without alcohol state；
Described step（5）Middle to carry out enriching and purifying using D101, HPD-100 macroreticular resin, concentrate adsorption rate is 1.0-
1.5bv/h, washing speed is 2-3 bv/h, and it is colourless to be washed to lower column liquid, and wash-out concentration of alcohol is 50-70%, and elution speed is
1.0-1.2bv/h；
Described step（7）Middle resin is a kind of PRP resins, and adsorption rate is 0.5-1.0 bv/h, and adsorbance is 0.2-
0.4BV, eluent is 10-30% ethanol solution 3-5bv, and pressure is 0.2-0.4MPa, TLC monitoring；
Described step（10）Middle spray drying EAT is 170-180 DEG C, and leaving air temp is 70-80 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410638395.8A CN104447901B (en) | 2014-11-13 | 2014-11-13 | A kind of method that network match dimension is prepared in the rhodiola root from rose |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410638395.8A CN104447901B (en) | 2014-11-13 | 2014-11-13 | A kind of method that network match dimension is prepared in the rhodiola root from rose |
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| Publication Number | Publication Date |
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| CN104447901A CN104447901A (en) | 2015-03-25 |
| CN104447901B true CN104447901B (en) | 2017-06-06 |
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| CN201410638395.8A Active CN104447901B (en) | 2014-11-13 | 2014-11-13 | A kind of method that network match dimension is prepared in the rhodiola root from rose |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1091957A (en) * | 1993-03-05 | 1994-09-14 | 西藏自治区藏医院 | A kind of is the medicinal granule and preparation method thereof of main component with the Radix Rhodiolae extract |
| CN103535730A (en) * | 2013-11-01 | 2014-01-29 | 王颖 | Extraction method for rhodiola rosea essence substance |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1246325C (en) * | 2003-03-28 | 2006-03-22 | 上海纳贝生物技术有限责任公司 | Preparation method of hongjintian effective component extract |
| CN101095690A (en) * | 2006-06-30 | 2008-01-02 | 成都华高药业有限公司 | Rhodiola sacra extractive, medicinal composition containing the same, method for preparing the same and the use thereof |
| CN101863871B (en) * | 2010-05-20 | 2012-01-18 | 于非 | Total glycosides of Rhodiola rosea, medical application and preparation method thereof |
| 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 |
| CN103819516A (en) * | 2012-11-16 | 2014-05-28 | 安徽尚善生物科技有限公司 | Intermediate-pressure preparation method for rosavin monomers |
| CN103505492B (en) * | 2013-09-27 | 2015-09-30 | 宁波市北仑玉健医药科技有限公司 | A kind of method using ultrafiltration to prepare high anti-oxidation value Radix Rhodiolae extract |
| 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 |
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- 2014-11-13 CN CN201410638395.8A patent/CN104447901B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1091957A (en) * | 1993-03-05 | 1994-09-14 | 西藏自治区藏医院 | A kind of is the medicinal granule and preparation method thereof of main component with the Radix Rhodiolae extract |
| CN103535730A (en) * | 2013-11-01 | 2014-01-29 | 王颖 | Extraction method for rhodiola rosea essence substance |
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