CN101129482B - Composition extracted from tubiflorae cistanche salsa, use thereof and method of extracting the same - Google Patents
Composition extracted from tubiflorae cistanche salsa, use thereof and method of extracting the same Download PDFInfo
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- CN101129482B CN101129482B CN2007101493881A CN200710149388A CN101129482B CN 101129482 B CN101129482 B CN 101129482B CN 2007101493881 A CN2007101493881 A CN 2007101493881A CN 200710149388 A CN200710149388 A CN 200710149388A CN 101129482 B CN101129482 B CN 101129482B
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Abstract
The invention discloses a composition extracted from Cistanche deserticola and application of drug composition and extracting method, which comprises the following steps: preparing raw material; lixiviating through alcohol; condensing; extracting; doing water sedimentation; drying; dehydrating; filtering through macropore resin. The invention increases the content of pineal glycoside and ergosterin steroid glycoside to 56. 3% and 9. 78% respectively, which can treat hypertension obviously.
Description
Technical field:
The present invention relates to a kind of compositions of from Cistanche Tubulosa, extracting and contain the purposes and the extracting method of said composition, especially a kind of from Cistanche Tubulosa, extract the compositions that contains echinacoside and acteoside and mainly by said composition constitute in order to treat hypertensive medicinal usage and said composition extracting method.
Background technology:
Cistanche Tubulosa [Cistanche tubulosa (Schenk) Wight.] belongs to perennial parasitic plant for the Orobanchaceae Herba Cistanches, generally be to use as nourishing class medicine, its main active ingredient is the phenethyl alcohol glycoside compounds, it is made up of caffeic acid, phenethanol aglycon, sugared three parts, comprises materials such as echinacoside, acteoside, boschnaloside.
Known pharmacological action at present has kidney-replenishing, benefiting essence-blood, the function of loosening bowel to relieve constipation, be used for sexual impotence, infertile, soreness of the waist and knees, muscles and bones is unable, hot-tempered constipation of intestinal and senile dementia, and Japanese scholar helps rattan investigation and studies carefully proof phenethyl alcohol glycosides material and also have the effect of obvious enhancing learning memory.
But mainly be to adopt traditional concocting method when being used as medicine at present, as immersion, infusion etc., the utilization of its effective ingredient is very limited.What particularly traditional process of preparing Chinese medicine was extracted is a kind of mixture, in use can not be separately with wherein each kind of effective ingredient, and use respectively at concrete object, caused the waste of effective ingredient, on the other hand owing to be the mixing of various compositions, thereby wherein a certainly having the component content of specific function lower, its usefulness also is difficult to be brought into play well.
Summary of the invention:
A main purpose of the present invention provides that a kind of method is simple, extraction effect good, be easy to the compositions of extracting from Cistanche Tubulosa that industry is applied, especially a kind of pharmaceutical composition that contains echinacoside and acteoside that from Cistanche Tubulosa, extracts and this pharmaceutical composition is applied to treat hypertensive medicinal usage, simultaneously, the present invention also provides the process of extracting described compositions in the aforementioned tube flower herba cistanches.
The compositions of extracting from Cistanche Tubulosa of the present invention, its characteristics are that the content of echinacoside is 30%～60% in containing, and the content of acteoside is 5～15%.
The purposes of the above-mentioned compositions of extracting from Cistanche Tubulosa is characterized in order to conduct treatment high blood pressure disease.
The above-mentioned method for compositions that contains middle echinacoside and acteoside of extracting from Cistanche Tubulosa is characterized in mainly being made up of following technical process:
Raw material is prepared: get the Cistanche Tubulosa medical material, pulverize, be beneficial to extract.
Lixiviate: with 4～10 times of Cistanche Tubulosa medical material weight, concentration is 80%～100% ethanol lixiviate 2～5 times, each lixiviate 2～7 days, after each lixiviate with 250～149 Ц m strainer filterings, gained filtrate is decompressed to boiling under temperature≤60 ℃ be concentrated into≤crude drug weight, get extractum, described extractum is preferably moisture and is no more than 30%.
Water precipitating: it is the macroporous resin capital of 0.1～1.0mm that gained extractum is added 5～60 times, granularity, with the alcoholic solution of concentration 5%～50% wash to macroporous resin column to colourless, use respectively, collect and wash thing
Drying and dehydrating: under 40～70 ℃ of negative pressure of temperature, be dried to moisture be no more than 30% Cistanche Tubulosa extract.
As further improvement, in the above-mentioned water precipitating operation, be preferably gradient flushing when alcoholic solution washes 2～5 times, during the gradient flushing after an alcoholic solution concentration be higher than before once.
As further improvement, before the above-mentioned water precipitating operation, preferably lixiviate gained extractum is extracted: use ethyl acetate extraction 1～5 time, each extraction is 1～4 times of crude drug weight with the amount of ethyl acetate, after the layering, cast out the ethyl acetate part, be decompressed to the extractum of boiling simmer down to weight≤crude drug weight under temperature≤60 ℃, described extractum is preferably moisture and is no more than 30%.
After the above-mentioned water precipitating operation, can adopt the alcoholic solution of concentration＞50% to wash resin column 1～2 time, make resin column reusable in the next round operation.
Method of the present invention adopts alcohol extraction, water precipitating, also filters through macroporous resin column, method is simple, extraction effect good, be easy to industry applies, and the content of echinacoside and acteoside obviously increases in the extract, can reach 56.3% and 9.78% respectively after testing, total amount reaches 66.1%, and described extract has obvious effect to treatment hypertension simultaneously.
Below be by of the influence of animal experiment test Cistanche Tubulosa extract to hypertension, erythrocyte membrane fluidity:
Material: Cistanche Tubulosa extract, the content of echinacoside, acteoside are 60%;
Reagent: 5-NS, lot number: 29545-48-0; U.S. Sigma company;
Subjects: animal SD rat (SPF level), ♂, body weight (180 ± 20) g;
Instrument: the BP-6 animal non-invasive blood pressure of Chengdu TME Technology Co., Ltd. is measured system; Electron paramagnetic resonance instrument ESP one 300 types of Germany Bruker company; The freezing high-capacity and high-speed centrifuge XL-8 type of U.S. Beckman company;
The foundation of the hypertension model of laboratory animal and the extraction of erythrocyte membrane, EPR measure
The hypertension model of laboratory animal:
With the rat random packet, 5 every group.Except that normal group, other all gives the high salt feedstuff of saliferous 4%; Through 40 days raising, measured blood pressure in the 40th day, three group blood pressures that give high salt feedstuff see Table 1 apparently higher than normal group, and the film success is made in prompting; When continuing to give high salt feedstuff, give the of the present invention Cistanche Tubulosa extract of large, medium and small three dosage 1 every day; Blank group is all to normal saline.After the administration 18 days, measure blood pressure, see Table 2, whole blood viscosity sees Table 3, shows that Cistanche Tubulosa extract has more significantly effect for the reduction of blood pressure, and the erythrocyte whole blood viscosity is also had in various degree influence.
Each treated animal systolic pressure value before table 1 administration
Compare * P＞0.05 * * P≤0.05 * * * P≤0.01 with the blank group
Table 2 Herba Cistanches extract is to the influence of each treated animal systolic pressure value
Compare * P＞0.05 * * P≤0.05 * * * P≤0.01 with model group
Table 3 Herba Cistanches extract is to the influence of each treated animal whole blood viscosity
Compare * P＞0.05 * * P≤0.05 * * * P≤0.01 with the blank group
The extraction of erythrocyte membrane, EPR measure:
Rat heart is got blood, and getting blood is left standstill layering in 12 hours under 4 ℃ of environment, inhales with dropper and removes the upper strata leukocyte, merges phase erythrocyte on the same group, adds 40 times 4 ℃ 0.05molL
-1(pH=8.0) PBS stirs evenly, and leaves standstill 1 minute in 4 ℃ of environment, with low-temperature and high-speed centrifuge (4 ℃, 12000rmin
-1) centrifugal 10 times, each 10min gets erythrocyte membrane.Get film, add a little 0.05molL
-1(pH=7.4) PBS shakes up, in a plurality of microcentrifugal tubes of packing into.Freezing (20 ℃), to be measured.
Refrigerated erythrocyte membrane is thawed, and with vortex suspendible device jolting mixing, sucking-off 250 μ L solution are put in the microcentrifugation, add 25 μ L1.3mmolL
-15-DS uses 0.05molL
-1(pH=7.4) PBS is diluted to about 1.0ml, and microcentrifugal tube stirs 3min gently in frozen water, put 4 ℃ spend the night after, take out centrifugal (3000rmin
-1, 3min), draw upper strata liquid and measure, if having absorption signal, erythrocyte membrane 0.05molL
-1(pH=7.4) PBS is centrifugal not to have the EPR absorption signal to supernatant, the erythrocyte membrane tubulature, puts in the resonator cavity of people EPR spectrometer and measures.
EPR location parameter and computing formula:
EPR test parameter: central magnetic field (CF): 3500G, sweep length (SW): 150G, sweep time (sT): 50S, modulation amplitude (MA): 3.2E+0G, modulating frequency (MF): 100KHz, microwave frequency (MF): 9.802GHz. microwave power (MP) .20mW, probe temperature (T): room temperature
Computing formula: S=0.568 * 3 (A
//-A
⊥)/(A
//+ 2A
⊥), target component S and erythrocyte membrane fluidity are inversely proportional to, and it is worth, and the microcyte membrane fluidity is good more more.
Table 4 Herba Cistanches extract is to the influence of each treated animal erythrocyte membrane fluidity
Compare * P＞0.05 * * P≤0.05 * * * P≤0.01 with model group
After making the rat hypertension model success, its hypertension, whole blood viscosity raise, erythrocyte membrane fluidity is relatively poor relatively, by giving significantly to bring high blood pressure down with Cistanche Tubulosa extract (P≤0.01), this explanation Cistanche Tubulosa extract has hypotensive activity preferably, and dosage and heavy dose of erythrocyte membrane fluidity also are significantly increased (P≤0.01) with respect to model group in the Cistanche Tubulosa extract simultaneously.
Membrane fluidity is one of key property of cell membrane, be the kinestate to film fat, memebrane protein, the dynamic change of film fat constituent and the combined reaction that the memebrane protein configuration changes, cell can cause that all cell membrane fluidity changes under damage or exogenous influence factor effect.From erythrocyte whole blood viscosity data analysis, all there is different influences in Herba Cistanches extract to Hypertensive Rats low shear rate, high shear rate, make its parameter more near normal value: hypertension model group rat performance low shear rate, high shear rate raise, the erythrocyte aggregation height is described, blood is in hypercoagulability, red cell deformability is poor, the fragility height, rat erythrocyte aggregation through administration reduces, red cell deformability is good, fragility is good, illustrates that Herba Cistanches extract has certain influence to hypertension animal's whole blood viscosity.
Numerical value from whole blood viscosity, low cut to cut with height can reflect erythrocytic aggregation and erythrocytic morphotropism, the height of mobility of erythrocyte membrance also reflects the state of erythrocyte membrane, from the measured value of blood pressure determination value, whole blood viscosity and the measured value of red cell membrane, Herba Cistanches extract has the effect of the blood pressure that reduces Hypertensive Rats, and the prompting Herba Cistanches extract has the pharmacological action of blood pressure lowering.
Description of drawings:
Fig. 1 is the sketch map of extracting method technical process of the present invention.
Fig. 2 is an echinacoside reference substance high-efficient liquid phase chromatogram in the described extract.
Fig. 3 is an acteoside reference substance high-efficient liquid phase chromatogram in the described extract.
Fig. 4 is described Cistanche Tubulosa extract high-efficient liquid phase chromatogram.
The specific embodiment:
Embodiment 1:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤0.3mm standby;
Lixiviate: with 10 times of Cistanche Tubulosa medical material weight, concentration is 90% ethanol lixiviate 4 times, and each lixiviate 5 days with 149 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 55 ℃ of temperature, being concentrated into gross weight is 80Kg;
Extraction: with ethyl acetate extraction 5 times, each extraction after the layering, is cast out the ethyl acetate part with the amount 120Kg of ethyl acetate, under 55 ℃ of temperature, be decompressed to boiling be concentrated into water content 30% extractum;
Water precipitating: with gained extractum add 5000Kg, granularity is the macroporous resin capital of 0.5mm, respectively washes 4 times with the alcoholic solution of concentration 10%, 20%, 30%, 40% respectively sequentially, and is extremely colourless to macroporous resin column
,Collect the flushing thing;
Drying and dehydrating: under 40 ℃ of temperature, be decompressed to boiling, drying be concentrated into water content 30% Cistanche Tubulosa extract.
Resin column behind the above-mentioned water precipitating, the alcoholic solution flushing of reuse concentration 55% 2 times is produced repeated use in order to next round.
Experiment detects:
Instrument, reagent and medical material:
Highly effective liquid phase chromatographic system: Tianjin, island 2010CHT, LC-solution chromatographic work station; Mettler-AE163 electronic balance (German Mettler company), KQ3200 type ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.), methanol, acetonitrile are Fisher reagent; Acetic acid: analytical pure (Xi'an chemical reagents corporation), ultra-pure water (self-control), echinacoside (Nat'l Pharmaceutical ﹠ Biological Products Control Institute, 111670-200502), acteoside (Nat'l Pharmaceutical ﹠ Biological Products Control Institute, 11530-200505).
Method and result:
Chromatographic condition Waters symmetry Cl8 chromatographic column (4.6 * 250mm, 5 μ m), mobile phase methanol-acetonitrile-1% acetic acid (15: 10: 75), flow velocity 0.6mLmin
-130 ℃ of column temperatures detect wavelength 334nm.
Test sample: Cistanche Tubulosa extract of the present invention is dried to water content≤10% before the detection.
Result: see that reference substance and sample chromatogram separation graph see Fig. 2～Fig. 4.
The content of echinacoside is 56.3%, and the content of acteoside is 9.78%.Total content reaches 66.08%.
Embodiment 2:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤3.0mm standby;
Lixiviate: with 4 times of Cistanche Tubulosa medical material weight, concentration is 80% ethanol lixiviate 3 times, and each lixiviate 6 days with 250 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 55 ℃ of temperature, is concentrated into total amount and is lower than 90Kg;
Extraction: with ethyl acetate extraction 2 times, each extraction after the layering, is cast out the ethyl acetate part with the amount 350Kg of ethyl acetate, under 55 ℃ of temperature, be decompressed to boiling be concentrated into water content 28% extractum;
Water precipitating: with gained extractum add 800Kg, granularity is the macroporous resin capital of 0.5mm, respectively wash 1 time with the alcoholic solution of concentration 15%, 20%, 25%, 30%, 35% respectively sequentially, to macroporous resin column to colourless, collect and wash thing;
Drying and dehydrating: under 30 ℃ of temperature, be decompressed to boiling, drying be concentrated into water content 28% Cistanche Tubulosa extract.
Embodiment 3:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤1mm standby;
Lixiviate: with Cistanche Tubulosa medical material weight be 85% ethanol lixiviate 5 times in 6 times, concentration, each lixiviate 4 days with 149 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 50 ℃ of temperature, being concentrated into gross weight is 80Kg;
Extraction: with ethyl acetate extraction 4 times, ethyl acetate 100Kg use in each extraction, after the layering, casts out the ethyl acetate part, is decompressed to boiling and is concentrated into water content 25% and gets extractum under 45 ℃ of temperature;
Water precipitating: with gained extractum add 3000Kg, granularity is the macroporous resin capital of 0.3mm, respectively washes 1 time with the alcoholic solution of concentration 15%, 25%, 35% respectively sequentially, and is extremely colourless to macroporous resin column
,Collect the flushing thing;
Drying and dehydrating: under 65 ℃ of temperature, be decompressed to boiling, drying be concentrated into water content 20% Cistanche Tubulosa extract.
Resin column behind the above-mentioned water precipitating, the alcoholic solution flushing of reuse concentration 60% 2 times is produced repeated use in order to next round.
Embodiment 4:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤1.5mm standby;
Lixiviate: with Cistanche Tubulosa medical material weight be 89% ethanol lixiviate 2 times in 10 times, concentration, each lixiviate 6 days with 210 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 40 ℃ of temperature, being concentrated into water content 20% gross weight is 60Kg;
Extraction: with ethyl acetate extraction 2 times, ethyl acetate 360Kg use in each extraction, after the layering, casts out the ethyl acetate part, is decompressed to seethe with excitement to be concentrated into gross weight≤60Kg under 50 ℃ of temperature;
Water precipitating: with gained extractum add 4000Kg, granularity is the macroporous resin capital of 0.7mm, respectively washes 1 time with the alcoholic solution of concentration 20%, 30% respectively sequentially, and is extremely colourless to macroporous resin column
,Collect the flushing thing;
Drying and dehydrating: under 50 ℃ of temperature, be decompressed to boiling, with gained wash the thing drying be concentrated into water content be lower than 20% Cistanche Tubulosa extract.
Embodiment 5:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤1.5mm standby;
Lixiviate: with Cistanche Tubulosa medical material weight be 92% ethanol lixiviate 4 times in 5 times, concentration, each lixiviate 7 days with 149 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 55 ℃ of temperature, being concentrated into gross weight is 100Kg;
Extraction: with ethyl acetate extraction 4 times, ethyl acetate 150Kg use in each extraction, after the layering, casts out the ethyl acetate part, is decompressed to boiling and is concentrated into water content 20% and gets extractum under 50 ℃ of temperature;
Water precipitating: with gained extractum add 1000Kg, granularity is the macroporous resin capital of 0.4mm, respectively washes 1 time with the alcoholic solution of concentration 10%, 15%, 25%, 30% respectively sequentially, and is extremely colourless to macroporous resin column
,Collect the flushing thing;
Drying and dehydrating: under 70 ℃ of temperature, be decompressed to boiling, drying be concentrated into water content be lower than 10% Cistanche Tubulosa extract.
Embodiment 6:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤2.5mm standby;
Lixiviate: with Cistanche Tubulosa medical material weight be 94% ethanol lixiviate 3 times in 9 times, concentration, each lixiviate 4 days with 210 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 45 ℃ of temperature, being concentrated into gross weight is 75Kg;
Extraction: with ethyl acetate extraction 4 times, ethyl acetate 250Kg use in each extraction, after the layering, casts out the ethyl acetate part, is decompressed to boiling and is concentrated into water content 26% and gets extractum under 55 ℃ of temperature;
Water precipitating: with gained extractum add 2000Kg, granularity is the macroporous resin capital of 0.2mm, respectively washes 1 time with the alcoholic solution of concentration 10%, 15%, 20%, 25%, 30% respectively sequentially, and is extremely colourless to macroporous resin column
,Collect the flushing thing;
Drying and dehydrating: under 40 ℃ of temperature, be decompressed to boiling, drying be concentrated into water content be lower than 25% Cistanche Tubulosa extract.
Embodiment 7:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤0.5mm standby;
Lixiviate: with Cistanche Tubulosa medical material weight be 95% ethanol lixiviate 5 times in 8 times, concentration, each lixiviate 5 days with 150 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 45 ℃ of temperature, being concentrated into gross weight is 75Kg;
Extraction: with ethyl acetate extraction 2 times, ethyl acetate 380Kg use in each extraction, after the layering, casts out the ethyl acetate part, is decompressed to seethe with excitement to be concentrated into gross weight≤50Kg under 50 ℃ of temperature;
Water precipitating: with gained extractum add 3000Kg, granularity is the macroporous resin capital of 0.6mm, respectively washes 1 time with the alcoholic solution of concentration 10%, 20%, 30%, 40% respectively sequentially, and is extremely colourless to macroporous resin column
,Collect the flushing thing;
Drying and dehydrating: under 65 ℃ of temperature, be decompressed to boiling, with gained wash the thing drying be concentrated into water content be lower than 10% Cistanche Tubulosa extract.
Embodiment 8:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤1.5mm standby;
Lixiviate: with Cistanche Tubulosa medical material weight be 97% ethanol lixiviate 4 times in 6 times, concentration, each lixiviate 7 days with 180 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 50 ℃ of temperature, being concentrated into gross weight is 50Kg;
Extraction: with ethyl acetate extraction 3 times, ethyl acetate 280Kg use in each extraction, after the layering, casts out the ethyl acetate part, is decompressed to boiling and is concentrated into water content 35% and gets extractum under 50 ℃ of temperature;
Water precipitating: with gained extractum add 3000Kg, granularity is the macroporous resin capital of 0.8mm, respectively washes 1 time with the alcoholic solution of concentration 15%, 25%, 35%, 40% respectively sequentially, and is extremely colourless to macroporous resin column
,Collect the flushing thing;
Drying and dehydrating: under 60 ℃ of temperature, be decompressed to boiling, with gained wash the thing drying be concentrated into water content be lower than 10% Cistanche Tubulosa extract.
Embodiment 9:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤1.8mm standby;
Lixiviate: with Cistanche Tubulosa medical material weight be 98% ethanol lixiviate 3 times in 7 times, concentration, each lixiviate 7 days with 150 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 40 ℃ of temperature, being concentrated into gross weight is that 70Kg gets extractum;
Water precipitating: with gained extractum add 3000Kg, granularity is the macroporous resin capital of 0.8mm, respectively washes 1 time with the alcoholic solution of concentration 15%, 25%, 35% respectively sequentially, and is extremely colourless to macroporous resin column
,Collect the flushing thing;
Drying and dehydrating: under 40 ℃ of temperature, be decompressed to boiling, with gained wash the thing drying be concentrated into water content be lower than 25% Cistanche Tubulosa extract.
Embodiment 10:
Raw material is prepared: get Cistanche Tubulosa medical material dry product 100Kg and pulverize as for the granule of≤1.2mm standby;
Lixiviate: with Cistanche Tubulosa medical material weight be 94% ethanol lixiviate 3 times in 7 times, concentration, each lixiviate 7 days with 150 Ц m strainer filterings, is got filtrate after each lixiviate;
Concentrate: lixiviate gained filtrate is decompressed to boiling under 40 ℃ of temperature, be concentrated into water content 35% extractum;
Water precipitating: with gained extractum add 3000Kg, granularity is the macroporous resin capital of 0.8mm, respectively washes 1 time with the alcoholic solution of concentration 10%, 20%, 30%, 40% respectively sequentially, and is extremely colourless to macroporous resin column
,Collect the flushing thing;
Drying and dehydrating: under 40 ℃ of temperature, be decompressed to boiling, with gained wash the thing drying be concentrated into water content be lower than 15% Cistanche Tubulosa extract.
Claims (6)
1. a compositions of extracting from the Cistanche Tubulosa application in preparation treatment high blood pressure disease medicine is characterized in that described compositions mainly produced by following technical process:
Raw material is prepared: get the Cistanche Tubulosa medical material, pulverize, be beneficial to extract;
Lixiviate: with 4～10 times of Cistanche Tubulosa medical material weight, concentration is 80%～100% ethanol lixiviate 2～5 times, each lixiviate 2～7 days, after each lixiviate with 250～149 ц m strainer filterings, gained filtrate is decompressed to boiling under temperature≤60 ℃, be concentrated into≤crude drug weight, get extractum;
Water precipitating: it is the macroporous resin capital of 0.1～1.0mm that above-mentioned gained extractum is added 5～60 times, granularity, washes macroporous resin column to colourless with the alcoholic solution of concentration 5%～50%, uses respectively, collects and washes thing;
Drying and dehydrating: under 40～70 ℃ of negative pressure of temperature, be dried to moisture be no more than 30% Cistanche Tubulosa extract, wherein contain echinacoside 30%～60%, acteoside is 5～15%.
2. described composition manufacturing method of extracting from Cistanche Tubulosa of claim 1 is characterized in that mainly being made up of following technical process:
Raw material is prepared: get the Cistanche Tubulosa medical material, pulverize, be beneficial to extract;
Lixiviate: with 4～10 times of Cistanche Tubulosa medical material weight, concentration is 80%～100% ethanol lixiviate 2～5 times, each lixiviate 2～7 days, after each lixiviate with 250～149 ц m strainer filterings, gained filtrate is decompressed to boiling under temperature≤60 ℃, be concentrated into≤crude drug weight, get extractum;
Water precipitating: it is the macroporous resin capital of 0.1～1.0mm that above-mentioned gained extractum is added 5～60 times, granularity, with the alcoholic solution of concentration 5%～50% wash to macroporous resin column to colourless, use respectively, collect and wash thing;
Drying and dehydrating: under 40～70 ℃ of negative pressure of temperature, be dried to moisture be no more than 30% Cistanche Tubulosa extract.
3. the composition manufacturing method of from Cistanche Tubulosa, extracting according to claim 2, before it is characterized in that described water precipitating operation, lixiviate gained extractum is extracted: use ethyl acetate extraction 1～5 time, each extraction is 1～4 times of crude drug weight with the amount of ethyl acetate, after the layering, cast out the ethyl acetate part, under temperature≤60 ℃, be decompressed to boiling, the extractum of simmer down to weight≤crude drug weight.
4. according to claim 2 or the 3 described composition manufacturing method of from Cistanche Tubulosa, extracting, it is characterized in that described extractum is that moisture is no more than 30%.
5. according to claim 2 or the 3 described composition manufacturing method of from Cistanche Tubulosa, extracting, it is characterized in that in the described water precipitating operation, be gradient flushing 2～5 times when alcoholic solution washes, during the gradient flushing after an alcoholic solution concentration be higher than before once.
6. the composition manufacturing method of from Cistanche Tubulosa, extracting according to claim 4, it is characterized in that in the described water precipitating operation, be gradient flushing 2～5 times when alcoholic solution washes, during the gradient flushing after an alcoholic solution concentration be higher than before once.
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Cited By (1)
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|---|---|---|---|---|
| WO2014190936A1 (en) * | 2013-05-30 | 2014-12-04 | 杏辉天力（杭州）药业有限公司 | Medicament for regulating blood sugar |
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| CN1526400A (en) * | 2003-03-04 | 2004-09-08 | 杭州天力药业有限公司 | Tubiflorous desert cistanche prepn containing phenethyl alcohol glycoside and its prepn process and use |
| CN1733885A (en) * | 2005-08-31 | 2006-02-15 | 王茂祥 | Broomrape dry red wine and its preparation method |
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