CN103467540B - A kind of method extracting rhodioside from Root of Kirilow Rhodiola - Google Patents
A kind of method extracting rhodioside from Root of Kirilow Rhodiola Download PDFInfo
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Abstract
The invention discloses a kind of method extracting rhodioside from Root of Kirilow Rhodiola, comprise the following steps: by Root of Kirilow Rhodiola pulverizing medicinal materials, using water as solvent, adopt ultrasonic-assisted extraction 1 ~ 4 time, united extraction liquid filters and obtains filtrate A; Through macroporous resin column, collect the elutriant B of rhodioside, concentrating under reduced pressure elutriant B obtains dry thing C; After anhydrous alcohol solution, be separated by simulated moving bed chromatography, obtain the component D being rich in rhodioside; Rhodioside product is obtained through concentrated, crystallization, centrifugal, drying; The extracting method of rhodioside of the present invention is easy and simple to handle, and in industry, application prospect is good, productive rate and product purity higher, the rhodioside yield obtained with technical scheme of the present invention reaches more than 70%, and products obtained therefrom is containing rhodioside more than 98%.
Description
Technical field
The present invention relates to a kind of method extracting rhodioside from Root of Kirilow Rhodiola.
Background technology
Root of Kirilow Rhodiola (Rhodiola) is Crassulaceae rhodiola perennial herb or semishrub plant, is one of rare medicinal plant, is described as " plateau ginseng ".This platymiscium about 90 kinds altogether in the whole world, to distribute kind more than 70 in China, main product in North China, northeast, southwest, the area such as northwest and Central China.Its chemical composition mainly contains flavonoid, tyrosol, rhodioside (Salidroside), Sitosterol, organic acid, volatile oil, polysaccharide, fat, protein etc.Wherein, rhodioside and tyrosol thereof are that Root of Kirilow Rhodiola mainly contains effective constituent, are also the most important indexs evaluating Root of Kirilow Rhodiola and extract thereof.Modern pharmacology research confirms, Radix Rhodiolae extract has anti-ageing, antitumor, antiviral, antibacterial, anti-hypoxia, antifatigue, radioprotective, anti-oxidant, analgesia, to various active such as nervus centralis and endocrine system two-ways regulation, and has very little side effect.
In neutral red red-spotted stonecrop, the Extraction and separation method of rhodioside mainly contains chromatography, ultrafiltration purification method, alcohol precipitation method of purification, macroreticular resin absorbing method etc.Column chromatography can obtain the rhodioside of higher degree, but loss of effective components is serious, and yield is too low, is only applicable to the preparation of microstandard product; In the use procedure of ultrafiltration purification method ultra-filtration membrane, fouling membrane easily causes membrane flux to fall sharply, and membrane cleaning process will use a large amount of alkali and acid, and separation selectivity is poor, unstable product quality; Ethanol precipitation is going deimpurity while, and gained dry extract viscosity is comparatively large, the easy moisture absorption, makes troubles to late stage process operation, and this method consumption alcohol amount is large, and cost is high, and the treatment time is longer; Macroreticular resin absorbing method uses comparatively general, but only relies on a kind of separation method of macroporous adsorbent resin, the rhodioside product purity obtained or on the low side.
Simulated moving bed chromatography technology introduces in liquid phantom preparing chromatogram by simulation moving-bed design philosophy, both the consumption having maintained liquid phantom preparing chromatogram is little, separation purity is high, and the advantage such as temperature-changeable operation, overcoming again usual liquid phantom preparing chromatogram can not the shortcoming of operate continuously, make it have separating power strong, equipment volume is little, and cost of investment is low, and is particularly conducive to the features such as the system of the high and difficult separation of heat of dissociation sensitivity.
Summary of the invention
In order to overcome the defect existed in above-mentioned prior art, the invention provides a kind of method of high efficiency extraction rhodioside from Root of Kirilow Rhodiola.Technical scheme of the present invention is:
From Root of Kirilow Rhodiola, extract a method for rhodioside, comprise the following steps:
pre-treatment: by Root of Kirilow Rhodiola pulverizing medicinal materials, is placed in water and soaks;
extract: using water as Extraction solvent, by step
pretreated medicinal material adopts ultrasonic-assisted extraction method, extracts 1 ~ 4 time, filters and obtain filtrate A after united extraction liquid;
macroporous resin purification: by step
the filtrate A obtained, through macroporous resin column, collects the elutriant B of rhodioside, and concentrating under reduced pressure elutriant B, to dry, obtains dry thing C;
simulation moving-bed purifying: by step
in dry thing C anhydrous alcohol solution after, be separated by simulated moving bed chromatography, obtain the component D being rich in rhodioside;
by step
in be rich in that the component D of rhodioside is concentrated, crystallization, centrifugal, drying obtain rhodioside product.
Described step
in, the Root of Kirilow Rhodiola medicinal material soak time after pulverizing is 1 ~ 2h.
Described step
in, supersound extraction temperature is 50 ~ 80 DEG C, and extraction time is 30 ~ 60min, extracts 1 ~ 4 time; Extracting for several times and consuming the cumulative volume of Extraction solvent is 5 ~ 20L/kg with the ratio of Root of Kirilow Rhodiola raw materials quality.
Step of the present invention
the macroporous resin of middle use is the nonpolar macroporous adsorption resins such as AB-8, D101, with 1 ~ 2 times of washing decon to column volume after absorption, then uses 2 ~ 3 times to 50 ~ 70% ethanol elution rhodiosides of column volume.
Step of the present invention
in, every gram of dry thing C 10ml anhydrous alcohol solution; The sorbent material that simulated moving bed chromatography is filled is silica gel, and eluent is the EtOH-EtOAc solution that volume ratio equals 1:9; Adsorption zone flow velocity 1 ~ 2BV/h; Elution zone flow velocity 1 ~ 3BV/h; Switching time is 600 ~ 800s; Temperature controls at 30 DEG C ~ 50 DEG C; Pressure-controlling is at 0.2MPa ~ 0.6MPa.
Step of the present invention
in, the component D being rich in rhodioside being concentrated into solid content is 30 ~ 50wt.%, crystallization, suction filtration, and 40 DEG C ~ 60 DEG C vacuum-dryings obtain rhodioside product.
Further, step of the present invention
in, filtrate A use after absorption with macroporous adsorbent resin, preferably uses 2 times to the washing decon of column volume, then uses 3 times to 70% ethanol elution rhodioside of column volume.
Further, step of the present invention
in, the preferred 2BV/h of simulated moving bed chromatography adsorption zone flow velocity; Elution zone flow velocity 2 is BV/h preferably; Switching time preferred 800s; Temperature preferably 40 DEG C; The preferred 0.4MPa of pressure.
The extracting method of rhodioside of the present invention is easy and simple to handle, and in industry, application prospect is good, productive rate and product purity higher, the rhodioside yield obtained with technical scheme of the present invention reaches more than 70%, and products obtained therefrom is containing rhodioside more than 98%.
Embodiment
embodiment 1
Take 5kg Radix Rhodiolae, add 30L water after pulverizing, 40 DEG C are soaked 1h, supersound extraction 60min at 65 DEG C, extract 2 times more afterwards, all add Extraction solvent water 30L at every turn.Filter after united extraction liquid, the filtrate A obtained does preliminary purification through macroporous adsorbent resin.Macroporous adsorbent resin take AB-8 as resin column, after the ion of 2 times of column volumes, with 70% ethanol elution rhodioside of 3 times of column volumes.The elutriant B obtained is evaporated to evaporate to dryness, obtains dry thing C and be about 109g.Dissolved by dry thing C with 1090ml dehydrated alcohol, gained solution enters simulated moving bed chromatography again.The sorbent material of simulation moving-bed filling is silica gel, and eluent is the EtOH-EtOAc solution that volume ratio equals 1:9; Adsorption zone flow velocity 2BV/h; Elution zone flow velocity 2BV/h; Switching time 800s; Temperature 40 DEG C; Pressure 0.4MPa.Through the component D being rich in rhodioside that simulation moving-bed separation obtains.Component D is concentrated into solid content 50wt.%, crystallization, obtains rhodioside product 39.5g, content 98.6% after suction filtration with 60 DEG C of vacuum-dryings, the yield of rhodioside is 72.0%.
embodiment 2
Take 8kg Radix Rhodiolae, add 80L water after pulverizing, 40 DEG C are soaked 1h, supersound extraction 60min at 70 DEG C, and extract 1 time more afterwards, the Extraction solvent water added is 80L.Filter after united extraction liquid, the filtrate A obtained does preliminary purification through macroporous adsorbent resin.Macroporous adsorbent resin take D101 as resin column, after the ion of 2 times of column volumes, with 70% ethanol elution rhodioside of 3 times of column volumes.The elutriant B obtained is evaporated to evaporate to dryness, obtains dry thing C and be about 162g.Dissolved by dry thing C with 1620ml dehydrated alcohol, gained solution enters simulated moving bed chromatography again.The sorbent material of simulation moving-bed filling is silica gel, and eluent is the EtOH-EtOAc solution that volume ratio equals 1:9; Adsorption zone flow velocity 2BV/h; Elution zone flow velocity 2BV/h; Switching time 800s; Temperature 40 DEG C; Pressure 0.4MPa.Through the component D being rich in rhodioside that simulation moving-bed separation obtains.Component D is concentrated into solid substance containing 50wt.%, crystallization, obtains rhodioside product 62.2g with 60 DEG C of vacuum-dryings after suction filtration, content 98.1%, and the yield of rhodioside is 76.3%.
embodiment 3
Take 5kg Hericiumerinaceus Pers, add 30L water after pulverizing, 40 DEG C are soaked 1h, supersound extraction 65min at 70 DEG C, extract 2 times more afterwards, all add Extraction solvent water 30L at every turn.Filter after united extraction liquid, the filtrate A obtained does preliminary purification through macroporous adsorbent resin.Macroporous adsorbent resin take D101 as resin column, after the ion of 2 times of column volumes, with 70% ethanol elution rhodioside of 3 times of column volumes.The elutriant B obtained is evaporated to evaporate to dryness, obtains dry thing C76.2g.Dissolved by dry thing C with 762ml dehydrated alcohol, gained solution enters simulated moving bed chromatography again.The sorbent material of simulation moving-bed filling is silica gel, and eluent is the EtOH-EtOAc solution that volume ratio equals 1:9; Adsorption zone flow velocity 2BV/h; Elution zone flow velocity 2BV/h; Switching time 800s; Temperature 40 DEG C; Pressure 0.4MPa.Through the component D being rich in rhodioside that simulation moving-bed separation obtains.Component D is concentrated into solid content 50 wt.%, crystallization, obtains rhodioside product 30.3g, content 98.9% after suction filtration with 60 DEG C of vacuum-dryings, the yield of rhodioside is 78.6%.
embodiment 4
The content of rhodioside is detected by high performance liquid chromatography
Chromatographic condition:
Chromatographic column: C
18post, (5.0 μm, 4.6mm × 150.0mm)
Moving phase: water-acetonitrile-phosphoric acid (volume ratio is 93.0:7.0:0.2)
Flow velocity: 1.0mL/min
Determined wavelength: 223nm
With rhodioside standard substance in contrast, utilize the content of peak area external standard method counting yield rhodioside.In standard substance HPLC spectrogram, the retention time of rhodioside is 14.521min, and in embodiment 1 product HPLC spectrogram, the retention time of rhodioside is 14.528min, and the two all has maximum absorption at 221nm and 275nm.
Claims (8)
1. from Root of Kirilow Rhodiola, extract a method for rhodioside, it is characterized in that comprising the following steps:
(1) pre-treatment: by Root of Kirilow Rhodiola pulverizing medicinal materials, is placed in water and soaks;
(2) extract: using water as Extraction solvent, pretreated for step (1) medicinal material is adopted ultrasonic-assisted extraction method, extracts 1 ~ 4 time, filter after united extraction liquid and obtain filtrate A;
(3) macroporous resin purification: filtrate A step (2) obtained is through macroporous resin column, macroporous resin column packed nonpolar macroporous adsorption resin, with 1 ~ 2 times of washing decon to column volume after absorption, use 2 ~ 3 times again to 50 ~ 70% ethanol elution rhodiosides of column volume, collect the elutriant B of rhodioside, concentrating under reduced pressure elutriant B, to dry, obtains dry thing C;
(4) simulation moving-bed purifying: after the dry thing C anhydrous alcohol solution in step (3), be separated by simulated moving bed chromatography, obtain the component D being rich in rhodioside; Wherein, every gram of dry thing C 10ml anhydrous alcohol solution; The sorbent material that simulated moving bed chromatography is filled is silica gel, and eluent is the EtOH-EtOAc solution that volume ratio equals 1:9; Adsorption zone flow velocity 1 ~ 2BV/h; Elution zone flow velocity 1 ~ 3BV/h; Switching time is 600 ~ 800s; Temperature controls at 30 DEG C ~ 50 DEG C; Pressure-controlling is at 0.2MPa ~ 0.6MPa;
(5) concentrated for the component D being rich in rhodioside in step (4), crystallization, centrifugal, drying are obtained rhodioside product.
2. a kind of method extracting rhodioside from Root of Kirilow Rhodiola as claimed in claim 1, it is characterized in that: in described step (1), the Root of Kirilow Rhodiola medicinal material soak time after pulverizing is 1 ~ 2h.
3. a kind of method extracting rhodioside from Root of Kirilow Rhodiola as claimed in claim 1 or 2, it is characterized in that: in described step (2), supersound extraction temperature is 50 ~ 80 DEG C, and extraction time is 30 ~ 60min, extracts 1 ~ 4 time; Extracting for several times and consuming the cumulative volume of Extraction solvent is 5 ~ 20L/kg with the ratio of Root of Kirilow Rhodiola raw materials quality.
4. a kind of method extracting rhodioside from Root of Kirilow Rhodiola as claimed in claim 3, is characterized in that: described nonpolar macroporous adsorption resin can be AB-8 or D101.
5. a kind of method extracting rhodioside from Root of Kirilow Rhodiola as claimed in claim 3, it is characterized in that: in described step (3), after macroporous resin adsorption, preferably use 2 times to the washing decon of column volume, then use 3 times to 70% ethanol elution rhodioside of column volume.
6. a kind of method extracting rhodioside from Root of Kirilow Rhodiola as described in claim 1,2,4 or 5, is characterized in that: in described step (4), the preferred 2BV/h of simulated moving bed chromatography adsorption zone flow velocity; The preferred 2BV/h of elution zone flow velocity; Switching time preferred 800s; Temperature preferably 40 DEG C; The preferred 0.4MPa of pressure.
7. a kind of method extracting rhodioside from Root of Kirilow Rhodiola as claimed in claim 6, it is characterized in that: in described step (5), the component D being rich in rhodioside being concentrated into solid content is 30 ~ 50wt.%, crystallization, suction filtration, 40 DEG C ~ 60 DEG C vacuum-dryings obtain rhodioside product.
8. a kind of method extracting rhodioside from Root of Kirilow Rhodiola as claimed in claim 6, is characterized in that: the kind of Root of Kirilow Rhodiola medicinal raw material can be Radix Rhodiolae, Radix Rhodiolae or Hericiumerinaceus Pers.
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| CN103923132B (en) * | 2014-04-16 | 2017-01-04 | 安徽博格生物科技有限公司 | The ultrasonic extraction process of rhodioloside in neutral red Herba hylotelephii erythrosticti |
| CN104017036A (en) * | 2014-06-11 | 2014-09-03 | 福建中医药大学 | Novel crystal form of rhodioloside and preparation method of novel crystal form |
| CN104672286B (en) * | 2015-03-09 | 2018-04-17 | 大兴安岭林格贝寒带生物科技股份有限公司 | The method of enriching and purifying α ursin from blueberry leaf |
| CN105924481B (en) * | 2016-06-29 | 2018-11-06 | 陈阿梅 | A kind of extracting method of rhodioside |
| CN106117281B (en) * | 2016-06-29 | 2018-11-06 | 陈阿梅 | The method that rhodioside is extracted from rhodiola root |
| CN106117280B (en) * | 2016-06-29 | 2018-11-06 | 陈阿梅 | The isolation and purification method of rhodioside |
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| CN101974045A (en) * | 2010-10-19 | 2011-02-16 | 康美药业股份有限公司 | Method for preparing salidroside |
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