CN100500686C - Method for extraction and preparation of astragaloside - Google Patents
Method for extraction and preparation of astragaloside Download PDFInfo
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- CN100500686C CN100500686C CNB2006100126876A CN200610012687A CN100500686C CN 100500686 C CN100500686 C CN 100500686C CN B2006100126876 A CNB2006100126876 A CN B2006100126876A CN 200610012687 A CN200610012687 A CN 200610012687A CN 100500686 C CN100500686 C CN 100500686C
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Abstract
This invention publisizes an extraction procedure for Astragalus membranaceous as followings: a.The raw astragalus roots would be soaked in water, refluxing extracted. The extract is condensed to dense concrete; b. precipitates the dense concrete with ethanol, recover the supernatant and adjust PH value to no more than 7, hydrolyze at 60-120deg C for 0.5-3 hours; c. filter the hydrolysate, precipitate ,wash to colorless with alkali, then add water to PH 7; d. Dry the sediment. The purity of Astragalus membranaceous with this invention is up to 90-98%. The recovery ratio reaches to 1.13-0.18%. The manipulation time is reduced by 30-50%.
Description
Technical field
The present invention relates to from plant, extract the method for effective ingredient, specifically from the Radix Astragali, extract the method for preparing Cyclosiversioside F.
Technical background
Cyclosiversioside F is the major ingredient of more than ten kind of saponin in the Radix Astragali, has the effect of anti-inflammatory, anti-ageing, antiviral, enhancing body immunizing power.Modern pharmacological research shows that also it has the white corpuscle of improvement deformability, improves myocardial contraction and pharmacological actions such as diastolic function, promotion insulin secretion and removing free radical.The content of Cyclosiversioside F in the Radix Astragali is very low.The method of extracting Cyclosiversioside F at present mainly is to adopt decoction water to carry or decoct water extraction and alcohol precipitation method.The problem that this method exists is that extract purity is low, yield is low.For addressing this problem, present many research staff are locked in research direction and adopt on organic solvent extraction, the crystallization method.As the disclosed Cyclosiversioside F preparation method of CN1172677C, utilize organic solvents such as propyl carbinol, chloroform, methyl alcohol to extract exactly.The problem that this type of technology exists is the production cost height, also can cause certain environmental pollution simultaneously.
Summary of the invention
Purpose of the present invention just provides a kind of novel method of extracting high-purity astragaloside, and this method extraction process cycle is short, cost is low and extract purity is high, yield is high, also can reduce the pollution to ecotope simultaneously.
The object of the present invention is achieved like this:
The method that extraction provided by the present invention prepares Cyclosiversioside F includes following steps:
A, Radix Astragali crude drug are added water to submerge, thermal backflow is extracted, and extracting solution is concentrated into thick medicinal extract;
Amount of water in this step generally gets final product according to conventional amount used.As adding the water of submergence medicinal material amount.Thermal backflow extraction time also can carry out according to the parameter in the common process.
B, thick medicinal extract add ethanol and carry out alcohol precipitation, after supernatant liquor reclaims ethanol, add alkaline solution and transfer pH value 〉=7; At 60～120 ℃, hydrolysis 0.5～3 hour;
Its concentration selection of used ethanol is a principle can reach the alcohol precipitation purpose in this step.General control ethanol content is 50-75%, to adapt to the stripping of Radix Astragali saponin class material.After supernatant liquor reclaims ethanol, adding alkaline solution (as sodium hydroxide solution, sodium hydrogen carbonate solution etc.) again transfers pH value to meta-alkalescence, and 60～120 ℃, hydrolysis 0.5～3 hour, its objective is make Radix Astragali saponin fully hydrolysis be converted into Cyclosiversioside F, to improve the purity and the yield of extract Cyclosiversioside F.
C, hydrolyzed solution filter, throw out with alkaline solution be washed till colourless after, add and be washed to neutrality;
D, taking precipitate oven dry.
Throw out in this step is high-purity astragaloside of the present invention.
In order further to improve the purity and the yield of extract Cyclosiversioside F, be preferably in the C step in the hydrolyzed solution, add the gac of crude drug amount 1～10%, after adsorbing fully, refilter, filtering medium adds ethanol and resolves, filters, reclaim ethanol, filtered liquid concentrates, and concentrated solution filters, filtering medium is washed till colourless with alkali lye, be washed to neutrality.
The addition preferable range of the gac in this step is 3～8% (in the crude drug weight).
Filtering medium adds ethanol and resolves in this step, wherein the preferable range 60～98% of alcohol concn.
The Cyclosiversioside F that the inventive method is extracted preparation and the medicinal adjuvant of routine such as vehicle, disintegrating agent, tamanori, lubricant, antioxidant, Drug coating, tinting material, perfume compound, tensio-active agent etc. mix, can be made into granule, capsule, tablet etc. oral preparations.Also can be according to adopting the conventional formulation technology to be prepared into preparations such as injection liquid, infusion solution.
But the present invention extracts the Cyclosiversioside F oral administration of preparation or without oral administration, dosage is had nothing in common with each other because of formulation is different, and concerning the grownup, 100～200mg every day is more suitable for oral medication.5～100mg every day is more suitable in the intravenous injection medication.
Its purity of Cyclosiversioside F that the inventive method is extracted preparation can reach 90～98%, and its yield can reach 0.13～0.18%, and extraction comparable general extraction preparation method of total time saves for 30%～50% time.Because the inventive method is not used other organic solvent, so low cost of manufacture has also reduced the environmental pollution that is caused in the production process simultaneously.
The inventive method is extracted the medicine that the Cyclosiversioside F for preparing can be used for preparing known clinical application, also can prepare the medicine that is used for the treatment of cerebrovascular disease.
Embodiment
The following examples and example of formulations can illustrate in greater detail the present invention, but do not limit the present invention in any form.
Embodiment 1
The Cyclosiversioside F preparation can be used for treating the beneficial effect of cerebral infarction disease, has obtained checking by following experiment:
Laboratory apparatus
Automatic clinical chemistry analyzer (TBA-120FR, Japan), liquid flashing counting device (Wallac, Pharmacia).Experiment reagent and medicine
Experiment reagent and medicine
Endothelin (ET), thromboxane B2 (TxB2), 6-ketone-prostaglandin F l α (6-KetoPGF1 α) are put and are exempted from medicine box (Beijing Fu Rui bio-engineering corporation), TCC (Tianjin couple stars biotech company).Superoxide-dismutase (SOD), mda (MDA) test kit (biological reagent company is built up in Nanjing).
Astragaloside injection: 10ml/ props up.Cyclosiversioside F raw material wherein adopts the method for the invention preparation, and it is 40g that the content of Cyclosiversioside F is amounted to into Radix Astragali crude drug amount
Compound injection of red sage root: Shanghai Zhongxi Pharmaceutical Co., Ltd.'s (lot number: 0412105).
Laboratory animal
Wistar rat (Beijing dimension tonneau China company provides), the SPF level, male, body weight 240～260g.Conformity certification number: SCX (capital) 2002-0003.
The experiment grouping
The basic, normal, high dosage group of astragaloside injection, compound injection of red sage root group, model group, sham operated rats and normal group.Every group 10.
The multiple infraction property of rat brain replication of Model
Reference literature method (Mei Jianxun, Zhang Yunling, Zhang Baili. the improvement of multi-infarct dementia rat model and the Chinese combination of Chinese tradiational and Western medicine magazine 2000 of application, 20 (2): 113-115.) method, duplicate the multiple infraction property of brain model model, blood sampling in the Wistar rat left ventricle of the same race, in 37 ℃ of incubator inner dryings, grind the back and sieve, get Thromboembolus 1mg during application and add physiological saline 0.3ml, shake up into suspension with the 200Lm sieve aperture.10% Chloral Hydrate is pressed the intraperitoneal anesthesia of 3.5ml/kg body weight, neck medisection skin, peel off sternohyoideus, omohyoid and breastbone Papillary muscle, expose arteria carotis communis, external carotid artery and internal carotid artery, temporary transient folder closes arteria carotis communis, and pterygoid process arteria palatina, inject embolus solution 0.3ml in the external carotid artery retrograde catheterization, inject open simultaneously arteria carotis communis, make embolus enter encephalic to each artery of brain, cause multiple cerebral infarction, open pterygoid process arteria palatina by internal carotid artery, the ligation external carotid artery, skin suture.
Drug intervention
Through the sublingual vein administration, later every 24h's each treated animal is administered once in immediate postoperative, and in continuous 1 week, 1h gets blood and cerebral tissue after the last administration.Normal group and sham operated rats injecting normal saline, astragaloside injection low dose group injection astragaloside injection 0.9ml/kg amounts to Radix Astragali extract and is respectively 3.15mg/kg; Dosage group injection astragaloside injection 1.8ml/kg amounts to Radix Astragali extract and is respectively 6.3mg/kg in the astragaloside injection; Astragaloside injection high dose group injection astragaloside injection 3.6ml/kg amounts to Radix Astragali extract and is respectively 12.6mg/kg; Compound injection of red sage root group injection compound injection of red sage root 1.8ml/kg.Each is organized the administration volume and is adjusted to 3.6ml/kg with physiological saline.
Index detects:
The serum biochemistry index detects
1h after reconstructed model 1 all last administrations, each experimental group rat ball rear vein beard is got blood, and automatic clinical chemistry analyzer reference reagent box specification sheets detects serum superoxide dismutases (SOD) activity, mda (MDA) content; Liquid flashing counting device reference reagent box specification sheets detects endothelin (ET), thromboxane B2 (TxB2), 6-ketone-prostaglandin F l α (6-KetoPGF1 α).
Morphological examination
1h after reconstructed model 1 all last administrations, each experimental group rat ball rear vein beard is got blood, 10% Chloral Hydrate is pressed the intraperitoneal anesthesia of 3.5ml/kg body weight subsequently, through left ventricle perfusion 0.01M phosphate buffered saline buffer, pH value 7.4 treats that perfusion liquid is limpid, pours into 4% Paraformaldehyde 96 phosphate buffer 1 0min, get brain, put into 4% Paraformaldehyde 96 phosphate buffered saline buffer external fixation.Paraffin embedding, section, row HE dyeing, om observation.
Experimental result
1 astragaloside injection is to the influence of the multiple infraction property of rat brain model forms
The HE coloration result shows, model group cortex brain mantle oedema and small part hyperemia, and seeing in the part lumen of vessels has particulate state or silk floss, and the little lumen of vessels of cortex is also seen above-mentioned change, with fashion visible brain essence oedema and multiple softening necrosis region.Neurone swelling and degeneration, parts of fine karyon are cavity sample or granular sex change, and chromatin is sparse or lose, and the microglia hyperplasia is arranged.Thalamus, hippocampus position observations are the same.Embolus obviously reduces or loses in astragaloside injection group cortex pia mater and the essence lumen of vessels, and seeing in the tube chamber that has has residual fine particle or filament shape remains, and encephalomalacia and oedema are not obvious, and neuronal degeneration is also not obvious, and spongiocyte does not have obvious hyperplasia.Thalamus and hippocampus observations are the same substantially.The above-mentioned three position neuronal degenerations of compound injection of red sage root group are not obvious, the slight hyperplasia of spongiocyte, and softening kitchen range obviously reduces.
2 astragaloside injections are to the influence (seeing Table 1) of the multiple infraction property of rat brain model oxidative damage
Table 1: astragaloside injection is to the influence of the multiple infraction property of rat brain model SOD in serum, MDA
Compare with model group,
*: P＜0.05
*: P＜0.01
By table 1 as seen, astragaloside injection height, middle dosage group all can obviously increase the multiple infraction property of brain rat blood serum SOD activity, and reduction MDA content (P＜0.05-0.01).
3 astragaloside injections pour into the influence (seeing Table 2) of rat inner skin cell function again to experimental cerebral ischemia
Table 2: astragaloside injection is to the influence of the multiple infraction property of rat brain model E T, TxB2,6-KetoPGF1 α
Compare with model group,
*: P＜0.05
*: P＜0.01
By table 2 as seen, astragaloside injection height, middle dosage group can obviously reduce Serum ET, TxB2 concentration, and increase 6-KetoPGF1 α concentration (P＜0.05-0.01).
Experiment shows: astragaloside injection can obviously improve the multiple infraction property of rat brain model cerebral tissue pathomorphism, increases activity of SOD in serum, reduces MDA content, obviously reduces Serum ET, TxB2 concentration, increases 6-KetoPGF1 α concentration.This shows that astragaloside injection has significant protective effect to the multiple infraction property of rat brain model.Therefore can be used for preparing the pharmaceutical preparation of treatment cerebral infarction disease.
Embodiment 2:
The Cyclosiversioside F preparation can be used for treating the beneficial effect of ischemia apoplexy disease, has obtained checking by following experiment:
Laboratory apparatus
Automatic clinical chemistry analyzer (TBA-120FR, Japan), liquid flashing counting device (Wallac, Pharmacia).
Experiment reagent and medicine
Endothelin (ET), thromboxane B2 (TxB2), 6-ketone-PGF1 (6-KetoPGF1 α) are put and are exempted from medicine box (Beijing Fu Rui bio-engineering corporation), TCC (Tianjin couple stars biotech company).Superoxide-dismutase (SOD), mda (MDA) test kit (biological reagent company is built up in Nanjing).
Astragaloside injection: 10ml/ props up.Cyclosiversioside F raw material wherein adopts the method for the invention preparation, and it is 40g that the content of Cyclosiversioside F is amounted to into Radix Astragali crude drug amount
Compound injection of red sage root: Shanghai Zhongxi Pharmaceutical Co., Ltd.'s (lot number: 0412105).
Laboratory animal
Wistar rat (Beijing dimension tonneau China company provides), the SPF level, male, body weight 240-260g.Conformity certification number: SCX (capital) 2002-0003.
The experiment grouping
The basic, normal, high dosage group of astragaloside injection, compound injection of red sage root group, model group, sham operated rats and normal group.Every group 20.
The cerebral ischemic reperfusion in rats replication of Model
The reference literature method is duplicated cerebrum ischemia re-perfusion model (reference Yuji Kuge, KazuoMinematsu, Takenori Yamaguchi, et al..Nylon Monofilament for IntraluminalMiddle Cerebral Artery Occlusion in Rats.Stroke 1995 26:1655-1658), rat 10% Chloral Hydrate 3ml/kg intraperitoneal injection of anesthesia, lie on the back and be fixed on the operating table, neck median incision, tell left carotid (CCA) and external carotid artery (ECA), electricity cuts off last arteria thyreoidea and the occipital artery branch of ECA with fixed attention, with 6-0 silk thread ligation ECA distal end, close the section start of ECA then with the micro vessel clamp folder, use 6-0 silk thread to pass ECA pine loose ground again and beat half hitch, cut off ECA near far-end ligation place.Get 4-0 the filament nylon line of long a 5-6cm., diameter 0.23mm, silk thread are coated with poly-lysine outward, and at bolt line insertion end 5mm place coating paraffin, waxing end diameter 0.3mm.Silk thread is inserted ECA, and the silk thread of tightening on the ECA avoids hemorrhage, removes blood vessel clip, and silk thread is imported internal carotid artery (ICA) by ECA, and silk thread is injected cranial cavity, when feeling resistance, counts from the ICA section start, and generally inserting length is 19～20mm.The MCA section start promptly is blocked, and ligation ECA stump is sewed up the incision, and draws nylon wire outside skin incision, uses so that extract when recovering blood flow.1.5h after, reopen otch, extract silk thread, to have finished blood flow and poured into again, ligation ECA stump is sewed up the incision.Possess homonymy HomerShi after the ischemia model animal is clear-headed and levy, the interior receipts person side of left fore flexing classifies research object as when carrying tail, and getting rid of has subarachnoid hemorrhage person.
Drug intervention
Through the sublingual vein administration, later every 24h's each treated animal is administered once in immediate postoperative, continuous 72h, and 1h gets blood and cerebral tissue after the last administration.Normal group and sham operated rats injecting normal saline, astragaloside injection low dose group injection astragaloside injection 0.9ml/kg amounts to Radix Astragali extract and is respectively 3.15mg/kg; Dosage group injection Cyclosiversioside F injection stoste 1.8ml/kg amounts to Radix Astragali extract and is respectively 6.3mg/kg in the astragaloside injection; Astragaloside injection high dose group injection astragaloside injection 3.6ml/kg amounts to Radix Astragali extract and is respectively 12.6mg/kg; Compound injection of red sage root group injection compound injection of red sage root stoste 1.8ml/kg.Each is organized the administration volume and is adjusted to 3.6ml/kg with physiological saline.
Index detects
The evaluation of neurological deficit sign:
1h after secondary administration behind the reconstructed model carries out the evaluation [2] of neurological deficit sign: adopt clinical neural function standards of grading to observe the influence of medicine to ischemic rat neurological deficit sign.Standards of grading: 0 grade: the impassivity functional impairment, limb activity is normal; 1 grade: the slight focal lesion of neural function, not tensible left fore; 2 grades: neural function moderate focal lesion, draw circle to the left; 3 grades: neural function severe focal lesion, topple over to the left; 4 grades: neural function utmost point severe focal lesion, there are not the autonomous walking and the disturbance of consciousness.
The cerebral infarction scope
1h after four administrations of reconstructed model, each experimental group part rat (n=10) broken end is rapidly got brain, after cutting antinion, weigh, 2mm does 6 crown sections of brain continuously at interval, put stripping and slicing lucifuge constant temperature in 37 ℃ of 1%TTC phosphate buffered saline buffers immediately and hatch 5-10min, visible healthy tissues dyeing takes on a red color, and necrotic tissue is white in color.The careful separation white area is weighed, and is infarcted region weight, calculates the per-cent that infarcted region accounts for left brain and full brain.
Cerebral index and brain water content
1h after four administrations of reconstructed model, each experimental group part rat (n=10) rapidly broken end is got brain, cut antinion after, weigh, place then and weigh again after drying in the baking box (110 ℃).Calculate cerebral index and brain water content at last.Cerebral index=brain weight in wet base * 100/ body weight, brain water content=(brain weight in wet base-brain stem is heavy) * 100%.
The serum biochemistry index detects
1h after four administrations of reconstructed model, each experimental group rat ball rear vein beard is got blood, and automatic clinical chemistry analyzer reference reagent box specification sheets detects serum superoxide dismutases (SOD) activity, mda (MDA) content; Liquid flashing counting device reference reagent box specification sheets detects endothelin (ET), thromboxane B2 (TxB2), 6-ketone-PGF1 (6-KetoPGF1 α).
Statistical procedures
Experimental data is represented with x ± s, carries out variance analysis, the F check, and relatively, q checks between group.
Experimental result
1, astragaloside injection pours into the influence of rat neurological deficit sign again to experimental cerebral ischemia
Sham operated rats rat limb activity freely, the impassivity afunction.Simple ischemia group ischemic 90min irritates in the 24h group again, draws circle during 5 mouse walkings to the left; Topple over to the left during 4 walkings; 1 the disturbance of consciousness occurs.The astragaloside injection high dose group has only 3 not tensible of mouse left fores in identical time point, and all the other rats do not have obvious neurologic impairment.The dosage group is drawn circle to the left in the astragaloside injection when 1 walking of identical time point, 3 not tensible of mouse left fores, and all the other rats do not have obvious neurologic impairment.Show that astragaloside injection can obviously alleviate the neurologic impairment due to cerebral ischemia re-pouring injured, has cerebral protection.
2, astragaloside injection pours into the influence of rat cerebral infarction scope again to experimental cerebral ischemia
(seeing Table 3)
Table 3: astragaloside injection pours into the influence of rat cerebral infarction scope again to experimental cerebral ischemia
Compare with model group,
*: P＜0.05
*: P＜0.01
By table 3 as seen, astragaloside injection height, middle dosage group can obviously reduce experimental cerebral ischemia and pour into the rat cerebral infarction scope again, compare with model group, and significant difference (P＜0.05) is arranged.
3, astragaloside injection pours into the influence of rat index and brain water content again to experimental cerebral ischemia
(seeing Table 4)
Table 4: astragaloside injection pours into the influence of rat brain index and brain water content again to experimental cerebral ischemia
Compare with model group,
*: P＜0.05
*: P＜0.01
By table 4 as seen, astragaloside injection height, middle dosage group can obviously reduce experimental cerebral ischemia and pour into rat brain exponential sum brain water content again, compare with model group, and significant difference (P＜0.05) is arranged.
4, astragaloside injection pours into the influence of rat oxidative damage again to experimental cerebral ischemia
(seeing Table 5)
Table 5: astragaloside injection pours into the influence of rat SOD, MDA again to experimental cerebral ischemia
Compare with model group,
*: P＜0.05
*: P＜0.01
By table 5 as seen, astragaloside injection height, middle dosage group can obviously increase experimental cerebral ischemia and pour into rat blood serum SOD activity again, reduce MDA content, compare with model group, and significant difference (P＜0.05～0.01) is arranged.
5 astragaloside injections pour into the influence of rat inner skin cell function again to experimental cerebral ischemia
(seeing Table 6)
Table 6: astragaloside injection pours into the influence of rat ET, TxB2,6-KetoPGF1 α again to experimental cerebral ischemia
Compare with model group,
*: P＜0.05
*: P＜0.01
By table 6 as seen, the high, medium and low dosage group of astragaloside injection can obviously reduce Serum ET, TxB2 concentration, and increase 6-KetoPGF1 α concentration (P＜0.05-0.01).
Conclusion
Astragaloside injection can obviously alleviate the neurologic impairment due to cerebral ischemia re-pouring injured, reduces the cerebral infarction scope, reduces cerebral index and brain water content, increase activity of SOD in serum, reduce MDA content, reduce Serum ET, TxB2 concentration, increase 6-KetoPGF1 α concentration.This shows that astragaloside injection has significant protective effect to cerebral ischemia.Therefore can be used for preparing the pharmaceutical preparation of treatment ischemia apoplexy disease.
Embodiment 3: the extraction preparation of Cyclosiversioside F
Get Radix Astragali thin slice 10kg, twice of boiling, each amount of water was not advisable to have powder, merge decocting liquid twice, filter to get filtrate 1, be condensed into proportion and be 1.35 thick medicinal extract, adding concentration again and be 80% ethanol, to make alcohol precipitation concentration be 75%, get supernatant liquor, reclaim ethanol, add the gac of crude drug 3% to crude drug amount volume, filter, continuing, it is closely colourless to be filtered to filtrate with 75% ethanol, and filtered liquid concentrates, and adds NaOH solution and transfers to concentrated solution pH value 8, in 90 ℃ of hydrolysis 0.5 hour, filter, throw out is washed till colourless with 0.5%NaOH solution, be washed to neutrality, get and be deposited in 80 ℃ of oven dry down.Promptly.Adopt HPLC-ELSD method (with reference to content measuring standard under Milkvetch Root item of version Chinese Pharmacopoeia in 2005) to measure its purity, purity is 98%.Yield is 0.135%.
Embodiment 4: the extraction preparation of Cyclosiversioside F
Get Radix Astragali thin slice 10kg, extracting in water 2 times, extracting solution is condensed into 1/2 thick medicinal extract of raw medicinal herbs amount, and adding ethanol, to make alcohol precipitation concentration be 60%, and supernatant liquor reclaims ethanol to medicinal material amount volume, add NaOH solution and transfer to concentrated solution pH value 7, in 110 ℃ of hydrolysis 2 hours, filter, that 0.5%NaOH solution is washed till is colourless, be washed to neutrality, get and be deposited in 80 ℃ of oven dry down, promptly.Adopt HPLC-ELSD method (with reference to content measuring standard under Milkvetch Root item of version Chinese Pharmacopoeia in 2005) to measure its purity, purity is 95%.
Embodiment 5:
Get Radix Astragali thin slice 10kg, extracting in water 2 times, extracting solution is recycled to 1/2 thick paste of raw medicinal herbs amount, adding ethanol, to make alcohol precipitation concentration be 75%, supernatant liquor reclaims ethanol to medicinal material amount volume, adds NaOH solution, transfers concentrated solution pH value to 9, in 60 ℃ of hydrolysis 3 hours, the gac that adds raw medicinal herbs amount 5% filters, and filters with 25% ethanol, continue and be filtered to colourless with 95% ethanol, filtered liquid concentrates, and concentrated solution filters, and that 0.5%NaOH solution is washed till is colourless, be washed to neutrality, get and be deposited in 60 ℃ of oven dry down, promptly get Cyclosiversioside F.Adopt HPLC-ELSD method (with reference to content measuring standard under Milkvetch Root item of version Chinese Pharmacopoeia in 2005) to measure its purity, purity is 98%.Yield is 0.15%
Embodiment 6:
Get and produce Radix Astragali injection (standard No. is: filter last gac during ministerial standard the 17 256 pages (WS3-B-3335-98), adding 80% ethanol stirs, filter carbon removal, filtrate is about 9 with the NaOH adjust pH, reclaim ethanol and in 90 ℃ of following hydrolysis 2 hours, soup cooled, filter, be filtered to colourless and wash with water to neutrality with 0.1%NaOH, taking precipitate is drying to obtain Cyclosiversioside F.
Present embodiment can come out Cyclosiversioside F extraction separation contained in the discarded gac in the Radix Astragali injection production technique, so also fully reclaim the Cyclosiversioside F of being wasted in the Radix Astragali injection production process in the prior art, thereby saved starting material, also reduced the manufacturing cost of Cyclosiversioside F.
Example of formulations 7
The granule preparation of medicine of the present invention:
Take by weighing the prepared Cyclosiversioside F bulk drug of embodiment 3--6.It is ground into powder, adds ethanol and make tamanori, add starch and make weighting agent, be pressed into particle.
Example of formulations 8
Prepare tablet according to methods known in the art, every contains following compositions:
Take by weighing the prepared Cyclosiversioside F bulk drug 50mg of embodiment 3～6
Lactose 70mg
Magnesium Stearate 3mg
Example of formulations 9
Prepare capsule according to methods known in the art, contain following compositions in each capsule:
Cyclosiversioside F raw material 100mg
Lactose 70mg
W-Gum 25mg
Magnesium Stearate 1mg
Example of formulations 10
Prepare injection according to methods known in the art, contain Cyclosiversioside F raw material 200mg among the 100ml.
Claims (4)
1, a kind of method for preparing Cyclosiversioside F of extracting is characterized in that it may further comprise the steps:
A, Radix Astragali raw medicinal herbs add water, and refluxing extraction is concentrated into thick medicinal extract;
B, thick medicinal extract add ethanol and carry out alcohol precipitation, after supernatant liquor reclaims ethanol, add alkaline solution and transfer pH value 〉=7; At 60～120 ℃, hydrolysis 0.5～3 hour;
C, hydrolyzed solution filter, precipitation with alkaline solution be washed till colourless after, add and be washed to neutrality;
D, taking precipitate oven dry.
2, extraction according to claim 1 prepares the method for Cyclosiversioside F, it is characterized in that in the C step be in the hydrolyzed solution, the gac that adds raw medicinal herbs 1～10%, filter, filtering medium adds ethanol to be resolved, filters, and filtered liquid concentrates, and concentrated solution filters, filtering medium is washed till colourless with alkali lye, be washed to neutrality.
3, extraction according to claim 2 prepares the method for Cyclosiversioside F, it is characterized in that the consumption that adds of said gac is 3～8% of a raw medicinal herbs amount.
4, extraction according to claim 3 prepares the method for Cyclosiversioside F, it is characterized in that said filtering medium adds ethanol and resolves, and wherein alcohol concn is 60～98%.
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| CN103073614B (en) * | 2013-01-22 | 2016-04-20 | 西安岳达植物科技有限公司 | A kind of method extracting Cyclosiversioside F from the Radix Astragali |
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