CN101580525A - Method for extracting salidroside, polysaccharose and tannin-type substances from rhodiola root crude drugs - Google Patents
Method for extracting salidroside, polysaccharose and tannin-type substances from rhodiola root crude drugs Download PDFInfo
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Abstract
The invention relates to a method for extracting salidroside, polysaccharose and tannin-type substances from rhodiola root crude drugs. The method comprises the following steps of: firstly, drying and crashing rootstalks of the rhodiola root crude drugs; then, adopting the supercritical carbon dioxide technology to extract oil type substances from the rhodiola root crude drugs, and carrying out microwave extraction, deposition in alcohol and filtration so as to obtain sediment and supernatant fluid; and then, drying the sediment to obtain a rough polysaccharose powder product of the rhodiola, and carrying out absorption by macroporous resin, elution and drying to the supernatant fluid so as to obtain a salidroside powder product; and finally, using acetone for extracting microwave extraction residue, and obtaining the rhodiola root tannin extract after centrifugation and drying. The method can simultaneously extract three active ingredients, namely, salidroside, polysaccharose and tannin in the rhodiola root, thus improving the utilization rate of the rhodiola root and increasing the utilization value of the rhodiola root.
Description
Technical field
The present invention relates to the deep processing of Root of Kirilow Rhodiola medicinal material, relate in particular to a kind of method of from the Root of Kirilow Rhodiola medicinal material, extracting rhodioside, polysaccharide and tannin class material.
Background technology
Root of Kirilow Rhodiola is Crassulaceae, draft or semishrub plant, grows on limestone, grouan mountain region, ground, glacier and ridge meadow or the mountain valley rock about height above sea level 3500~5000m, and Tibetan language claims " Suluomabu ".Because Root of Kirilow Rhodiola is grown under the extremely abominable and changeable natural environmental condition, stood the tolerance of hypoxemia, low temperature, drying, blast, strong ultraviolet radiation, day and night temperature great disparity, make it adapt to high and cold changeable severe environment from heredity, therefore be pregnant with the unexistent adaptitude material of other plant, thereby have anticancer, anti-oxidant, anti-hypoxia, antifatigue, effect such as delay senility; Simultaneously, it to short period of time memory, the blood oxygen pressure level that improves the people, the front and back load that reduces heart that improve the people, improve heart function etc. remarkable effect arranged.
Why Root of Kirilow Rhodiola can have unique pharmacological action, and its basic substance is the bioactive ingredients that it contains---rhodioside.Rhodioside belongs to phenylethanol; be considered to one of main active ingredient of Root of Kirilow Rhodiola; have antifatigue, anti-ageing, immunoregulation effect; cardiovascular and cerebrovascular, neurocyte had provide protection; can anti-hepatic fibrosis, antitumor, radioprotective; effectively nervous system regulation, improve learning memory, also have simultaneously sleep peacefully, effect such as calmness.
In addition, the tannin that also contains Radix Rhodiolae polysaccharide and large amount of complex in the Root of Kirilow Rhodiola.Wherein Radix Rhodiolae polysaccharide is made up of pectinose, glucose, semi-lactosi, seminose, rhamnosyl, wood sugar and galacturonic acid, have multiple pharmacological effect such as anti-radiation, antiviral, hypoglycemic, immunomodulatory, and similar genseng, the strengthening by means of tonics of Radix Et Caulis Acanthopanacis Senticosi, the effect of strengthening the body resistance to consolidate the constitution.And tannin belongs to the Polyphenols composition, and its existence can influence the clarity and the taste of Root of Kirilow Rhodiola solution, therefore in order to correct its astringent taste, improves clarity, usually how it is removed as impurity; But studies show that at present vegetable tannin not only has very strong antioxygenation, but also have significantly antibacterial, anticancer and suppress effect such as cholesterol rising, wherein its resistance of oxidation makes it can remove the intravital superfluous free radical of people effectively, thus the aging of reducing human histoorgan.
Because Root of Kirilow Rhodiola is a kind of material with multiple biological effect, contains the amino acid and the trace element of needed by human body, no matter be therefore as dietary supplements, still all have the widespread use DEVELOPMENT PROSPECT as the medicine rhodiola rosea formulated product.And at present Root of Kirilow Rhodiola mainly uses is rhodioside, less to polysaccharide, tannin isoreactivity components utilising; The residue that extracts simultaneously behind the rhodioside generally abandons as refuse, causes the waste of medicine resource.Therefore how fully utilizing Root of Kirilow Rhodiola, improve the comprehensive utilization of resources rate, is that one of problem to be solved is arranged at present.
Summary of the invention
Technical problem to be solved by this invention provide a kind of effective raising Root of Kirilow Rhodiola comprehensive utilization ratio from from the Root of Kirilow Rhodiola medicinal material, extracting the method for rhodioside, polysaccharide and tannin class material.
For addressing the above problem, a kind of method of extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material of the present invention may further comprise the steps:
(1) Root of Kirilow Rhodiola medicinal material rhizome is carried out drying, and be ground into 20~80 purpose powder;
(2), and get residue with the oil substances in the powder employing super critical CO 2 technology extraction Root of Kirilow Rhodiola medicinal material of described step (1) gained;
(3) in residue, add aqueous solvent, centrifugal extracting solution and the extraction residue of getting after carrying out microwave extraction or heating direct refluxing extraction; Wherein the feed liquid weightmeasurement ratio is 1: 10~1: 30;
(4) extracting solution in the described step (3) after filtering, concentrated, alcohol precipitation is got throw out and supernatant liquor;
(5) drying precipitate with described step (4) gained gets Root of Kirilow Rhodiola Crude polysaccharides powdery product;
(6) with the supernatant concentration of described step (4) gained after after the macroporous resin adsorption, wash-out, drying the rhodioside powder-like product;
(7) with the extraction residue in the described step (3) with acetone extraction after, through centrifugal, after reclaiming solvent, drying Root of Kirilow Rhodiola tannin extract; Wherein the feed liquid weightmeasurement ratio is 1: 10~1: 40.
The extraction conditions that CO 2 supercritical technology in the described step (2) is adopted is meant that pressure is that 20~30Mpa, temperature are that 30~55 ℃, time are 60~120min.
Microwave extraction condition in the described step (3) is meant that extracting temperature is that 40~80 ℃, extraction power are that 150~320W, extraction time are 1~5min.
The direct refluxing extraction condition of heating in the described step (3) is meant that Heating temperature is 80~100 ℃, and reflux extracting time is 1~4h.
Alcohol precipitation concentration in the described step (4) is 50~85%.
Root of Kirilow Rhodiola Crude polysaccharides powdery product in the described step (5) contains 30~60% Radix Rhodiolae polysaccharide.
Rhodioside powder-like product in the described step (6) contains 10~20% rhodioside.
Macroporous resin in the described step (6) is the polar macroporous adsorption resin tower.
Acetone concentration of volume percent in the described step (7) is 30~90%.
Root of Kirilow Rhodiola tannin extract in the described step (7) contains 20~50% tannin class material.
The present invention compared with prior art has the following advantages:
1, because the present invention mainly adopts water as solvent, therefore safe and reliable.
2, because the extraction among the present invention is to carry out under relatively low temperature, has therefore saved the energy, lowered energy consumption.
3, because the present invention can extract rhodioside in the Root of Kirilow Rhodiola, polysaccharide and three kinds of activeconstituentss of tannin simultaneously, and the rhodioside yield is 25~50% after tested, polysaccharide yield is 10~20%, the tannin yield is 15~25%, therefore improve the utilization ratio of Root of Kirilow Rhodiola, increased the utility value of Root of Kirilow Rhodiola.
4, because operation steps of the present invention is simple, extraction time is short, has therefore improved working efficiency effectively, is a kind of quick, efficient, energy-conservation, is easy to form the extraction process of industrialization, green safety.
Embodiment
Embodiment 1 extracts the method for rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material, may further comprise the steps:
(1) getting 10kg Root of Kirilow Rhodiola medicinal material rhizome, to put into the KMZ-2006 type microwave vacuum dryer that Wenzhou City health board pharmaceutical machine company limited produces dry, puts into the Jiangyin City then and cross over the ZFJ-200 type herbal medicine pulverizing machine that mechanical company limited produces and be ground into 20~80 purpose powder.
(2) powder of step (1) gained is put into the HA221-40-12 type supercritical CO that Huaan, Nantong supercritical extraction equipment company limited produces
2In the extraction plant, after extracting 60~120min under 20~30Mpa pressure, 30~55 ℃ of temperature, the oil substances 0.84kg (grease yield 1.0%~2.0%) in the Root of Kirilow Rhodiola medicinal material, and residue.
(3) in residue, added aqueous solvent in 1: 10~1: 30 by the feed liquid weightmeasurement ratio, the WCD10S-01 type microwave extracting equipment that places Sanle Microwave Technology Development Co., Ltd, Nanjing to produce then, at 40~80 ℃, extraction power is 150~320W, each extraction time to be under 1~5min condition after the microwave extraction three times, the GQ75 type high speed tubular-bowl centrifuge of producing with sky, PVG this centrifugal machine company limited with the speed of 10000r/min respectively to the feed liquid of three microwave extraction centrifugal extracting solution and extract residue.
(4) with after the merging of the extracting solution in the step (3), the R5002K type Rotary Evaporators of producing with Wuxi Xing Hai king's biochemical equipment company limited concentrates, and gets concentrated solution; The edible ethanol that in this concentrated solution, adds volumetric concentration 95%, make that ethanol concn is after alcohol precipitation concentration reaches 50~85% in the solution, standing over night, the GQ75 type high speed tubular-bowl centrifuge of using the production of sky, PVG this centrifugal machine company limited is with centrifugal throw out and the supernatant liquor of getting of the speed of 10000r/min;
(5) it is dry the throw out of step (4) gained to be put into microwave vacuum dryer, 1.59kg scarlet, content reach the Root of Kirilow Rhodiola Crude polysaccharides powdery product of 30~60% Radix Rhodiolae polysaccharides.
(6) supernatant liquor with step (4) gained adopts the Rotary Evaporators evaporate to dryness to get 2.14kg Root of Kirilow Rhodiola medicinal extract, and adopting the U.S. Agilent of Agilent company 1100 type high-efficient liquid phase chromatogram HPLCs to measure rhodioside content is 1.0~3.0%; After this medicinal extract added water and dissolve fully, polarity HPD600 type macroporous adsorbent resin tower absorption 4~12h that the precious grace chemical industry in Cangzhou, Hebei after treatment company limited produces, water is eluted to colourless or light brown with the flow velocity of 0.5~2.0BV/h then; Be eluted to the flow velocity of 0.5~2.0BV/h with 30~70% ethanol again and stop wash-out when the colourless specification 100 * 100mm silica gel G plate promptly produced with Haiyang Chemical Plant, Qingdao of elutriant is checked in the elutriant no rhodioside spot, collect elutriant at this moment.
Elutriant is put into the Rotary Evaporators evaporation reclaim etoh solvent, get the rhodioside concentrated solution; This concentrated solution is put after refrigerator-18 a ℃ precooling is frozen into ice cube, use the FDU-1100 of Tokyo Physico-chemical Apparatus Co., Ltd. type freeze drier lyophilize 24h again, pulverize with Wenjiang city hundred happy pulverizer instrument factory FZ-10 type high speed medicinal herb grinders then and obtain 0.535kg rhodioside powder-like product.Measuring rhodioside content through HPLC is 10~20%.
(7) the extraction residue in the step (3) is put into the CTXNW-100B type built-up type circulating ultrasonic extracting machine that the Beijing Hongxianglong Biotechnology Development Co., Ltd produces, in the feed liquid weightmeasurement ratio is that to add volumetric concentration be 30~90% acetone for 1: 10~1: 40 ratio, at ultrasonic power 200~600W, extract three times under the condition that each extraction time is 20~60min; Centrifugal to the feed liquid of three extractions respectively with the high speed tubular-bowl centrifuge then with the speed of 10000r/min, merge supernatant liquor; This supernatant liquor is reclaimed solvent with Rotary Evaporators, after the microwave vacuum dryer drying, get 0.9kg Root of Kirilow Rhodiola tannin extract again.Through casein food grade spectrophotometry Root of Kirilow Rhodiola tannin tannin class substances content is 30~50%.
Wherein: the treatment process of polarity HPD600 type macroporous adsorbent resin tower is: the NaOH solution with mass concentration 2% steeps 120min with the macroporous adsorbent resin tower leaching earlier, be washed till neutrality with deionized water then, after using 95% alcohol immersion 60min again, it is as clear as crystal to wash elutriant with 95% ethanol.Be washed till no ethanol flavor with deionized water before the last sample.
Embodiment 2 extracts the method for rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material, may further comprise the steps:
(1) gets 10kg Root of Kirilow Rhodiola medicinal material rhizome and put into the microwave vacuum dryer drying, put into herbal medicine pulverizing machine then and be ground into 20~80 purpose powder.
(2) powder of step (1) gained is put into supercritical CO
2In the extraction plant, after extracting 60~120min under 20~30Mpa pressure, 30~55 ℃ of temperature, the oil substances 0.84kg (grease yield 1.0%~2.0%) in the Root of Kirilow Rhodiola medicinal material, and residue.
(3) in residue, added aqueous solvent in 1: 10~1: 30 by the feed liquid weightmeasurement ratio, the TQ-300 type multipotency thickner that places Wuhan sunshine roc pharmaceutical machine equipment company limited to produce then, under the condition of 80~100 ℃ of Heating temperatures, extract 1~3 time, behind each 1~4h that refluxes, centrifugal to the feed liquid of three refluxing extraction respectively by the high speed tubular-bowl centrifuge again with the speed of 10000r/min, get extracting solution and extract residue.
(4) with after the merging of the extracting solution in the step (3), concentrate, get concentrated solution with Rotary Evaporators; The edible ethanol that adds volumetric concentration 95% in this concentrated solution makes that ethanol concn is after alcohol precipitation concentration reaches 50~85% in the solution, standing over night, with the high speed tubular-bowl centrifuge with the speed of 10000r/min centrifugal throw out and supernatant liquor;
(5) it is dry the throw out of step (4) gained to be put into microwave vacuum dryer, 1.59kg scarlet, content reach the Root of Kirilow Rhodiola Crude polysaccharides powdery product of 30~60% Radix Rhodiolae polysaccharides.
(6) supernatant liquor with step (4) gained adopts the Rotary Evaporators evaporate to dryness to get 2.14kg Root of Kirilow Rhodiola medicinal extract, and adopting HPLC to measure rhodioside content is 1.0~3.0%; After this medicinal extract added water and dissolve fully, polarity HPD600 type macroporous adsorbent resin tower absorption 4~12h after treatment, water is eluted to colourless or light brown with the flow velocity of 0.5~2.0BV/h then; Be eluted to the flow velocity of 0.5~2.0BV/h with 30~70% ethanol again and stop wash-out when elutriant is colourless promptly uses specification 100 * 100mm silica gel G plate to check in the elutriant no rhodioside spot, collect elutriant at this moment.
Elutriant is put into the Rotary Evaporators evaporation reclaim etoh solvent, get the rhodioside concentrated solution; This concentrated solution is put after refrigerator-18 a ℃ precooling is frozen into ice cube, used freeze drier lyophilize 24h again, pulverize with the high speed medicinal herb grinder then and obtain 0.535kg rhodioside powder-like product.Measuring rhodioside content through HPLC is 10~20%.
(7) the extraction residue in the step (3) is put into built-up type circulating ultrasonic extracting machine, in the feed liquid weightmeasurement ratio is that to add volumetric concentration be 30~90% acetone for 1: 10~1: 40 ratio, at ultrasonic power 200~600W, extract three times under the condition that each extraction time is 20~60min; Centrifugal to the feed liquid of three extractions respectively with the high speed tubular-bowl centrifuge then with the speed of 10000r/min, merge supernatant liquor; This supernatant liquor is reclaimed solvent with Rotary Evaporators, after the microwave vacuum dryer drying, get 0.9kg Root of Kirilow Rhodiola tannin extract again.Through casein food grade spectrophotometry Root of Kirilow Rhodiola tannin tannin class substances content is 30~50%.
The treatment process of its Semi-polarity HPD600 type macroporous adsorbent resin tower is with embodiment 1.
Claims (10)
1, a kind of method of extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material may further comprise the steps:
(1) Root of Kirilow Rhodiola medicinal material rhizome is carried out drying, and be ground into 20~80 purpose powder;
(2), and get residue with the oil substances in the powder employing super critical CO 2 technology extraction Root of Kirilow Rhodiola medicinal material of described step (1) gained;
(3) in residue, add aqueous solvent, centrifugal extracting solution and the extraction residue of getting after carrying out microwave extraction or heating direct refluxing extraction; Wherein the feed liquid weightmeasurement ratio is 1: 10~1: 30;
(4) extracting solution in the described step (3) after filtering, concentrated, alcohol precipitation is got throw out and supernatant liquor;
(5) drying precipitate with described step (4) gained gets Root of Kirilow Rhodiola Crude polysaccharides powdery product;
(6) with the supernatant concentration of described step (4) gained after after the macroporous resin adsorption, wash-out, drying the rhodioside powder-like product;
(7) with the extraction residue in the described step (3) with acetone extraction after, through centrifugal, after reclaiming solvent, drying Root of Kirilow Rhodiola tannin extract; Wherein the feed liquid weightmeasurement ratio is 1: 10~1: 40.
2, the method for extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material as claimed in claim 1 is characterized in that: the extraction conditions that the CO 2 supercritical technology in the described step (2) is adopted is meant that pressure is that 20~30Mpa, temperature are that 30~55 ℃, time are 60~120min.
3, the method for extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material as claimed in claim 1 is characterized in that: the microwave extraction condition in the described step (3) is meant that extracting temperature is that 40~80 ℃, extraction power are that 150~320W, extraction time are 1~5min.
4, the method for from the Root of Kirilow Rhodiola medicinal material, extracting rhodioside, polysaccharide and tannin class material as claimed in claim 1, it is characterized in that: the direct refluxing extraction condition of the heating in the described step (3) is meant that Heating temperature is 80~100 ℃, and reflux extracting time is 1~4h.
5, the method for extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material as claimed in claim 1, it is characterized in that: the alcohol precipitation concentration in the described step (4) is 50~85%.
6, the method for extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material as claimed in claim 1 is characterized in that: the Root of Kirilow Rhodiola Crude polysaccharides powdery product in the described step (5) contains 30~60% Radix Rhodiolae polysaccharide.
7, the method for extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material as claimed in claim 1, it is characterized in that: the rhodioside powder-like product in the described step (6) contains 10~20% rhodioside.
8, the method for extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material as claimed in claim 1, it is characterized in that: the macroporous resin in the described step (6) is the polar macroporous adsorption resin tower.
9, the method for extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material as claimed in claim 1, it is characterized in that: the acetone concentration of volume percent in the described step (7) is 30~90%.
10, the method for extracting rhodioside, polysaccharide and tannin class material from the Root of Kirilow Rhodiola medicinal material as claimed in claim 1, it is characterized in that: the Root of Kirilow Rhodiola tannin extract in the described step (7) contains 20~50% tannin class material.
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