CN104096040A - Preparation method of six-ingredient rehmannia capsules - Google Patents
Preparation method of six-ingredient rehmannia capsules Download PDFInfo
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Abstract
A preparation method of six-ingredient rehmannia capsules. The invention relates to a new method of preparation of a traditional Chinese medicine compound preparation. The six-ingredient rehmannia capsules comprise of six raw material medicines: prepared rehmannia roots, paeonia suffruticosa, Chinese yam, cornus officinalis, rhizoma alismatis and poria cocos. The preparation method includes preparation of poria cocos micropowder, the preparation of a water extract of the poria cocos, the preparation of an alcohol extract of the cornus officinalis, the preparation of a paeonol [beta]-cyclodextrine inclusion complex, the preparation of a water extract of the medicines, and the filling of the capsules. By means of an ultrasonic extraction method, active ingredients in cells of the medicines can be dissolved out rapidly and the active ingredients are free from being destroyed under violent conditions so that high extraction ratios of the active ingredients is high, an extraction time is short and energy resources are saved. By means of a jet mill for ultrasonic kinetic energy jet milling, granules of the medicines are easy to absorb by human bodies. By means of a paeonol [beta]-cyclodextrine including technology, influences caused by light, oxygen and hydrolysis conditions are effectively avoided and stabilities of volatile ingredients are improved. Not only are retaining indexes of the volatile ingredients in the preparation effectively increased, but also thick pungent odors are covered better and the capsules are more convenient to take.
Description
technical field
The present invention relates to new method prepared by a kind of compound Chinese medicinal preparation, be specifically related to a kind of preparation method of famous Chinese patent medicine LIUWEIDIHUANG JIAONANG.
background technology
LIUWEIDIHUANG JIAONANG is the Traditional Chinese medicine historical preparation that < < Pharmacopoeia of People's Republic of China > > records.Prescription is comprised of Radix Rehmanniae Preparata, Cortex Moutan, Rhizoma Dioscoreae, Fructus Corni, Rhizoma Alismatis, Poria 6 taste medicines, has enriching yin and nourishing kidney effect.For damage of kidney-YIN, dizziness and tinnitus, soreness of the waist and knees, osteopyrexia and fever, the diseases such as night sweat.
The existing preparation method of LIUWEIDIHUANG JIAONANG is in above-mentioned 6 tastes, to get part Poria (1/5) to be ground into fine powder, tails over part and decocts with water three times with residue Poria, and each 30 minutes, filter, merging filtrate, is concentrated into thick paste shape; Fructus Corni adds alcohol reflux secondary, and each 1 hour, filter, medicinal residues are standby, and filtrate recycling ethanol is concentrated into thick paste shape; Cortex Moutan vapor distillation, and add l mol/L hydrochloric acid solution to make crystallization in the distillate of collecting, filtering, crystallization washes with water, and cold drying is ground into fine powder; Three tastes such as the aqueous solution after distillation and Cortex Moutan medicinal residues, Fructus Corni medicinal residues and all the other Radix Rehmanniae Preparata decoct with water three times; Each 1 hour, filter merging filtrate, by macroporous adsorptive resins, use 70% ethanol elution, collect eluent, reclaim ethanol, be concentrated into thick paste shape, add above-mentioned Poria thick paste, Fructus Corni thick paste and Poria fine powder, mix, drying under reduced pressure, is ground into fine powder, add above-mentioned Paeonia suffruticosa to answer extract fine powder and appropriate amount of auxiliary materials, mix, incapsulate, make 1000 (0.3mg/ grains), obtain.
Publication number is CN1456233A, application number is that 03118618.1 Chinese invention patent application discloses a kind of LIUWEIDIHUANG JIAONANG preparation method, this method has adopted cyclodextrin inclusion paeonol, the spray-dired method of extraction concentrated solution, other preparation process are basic and said method is basically identical.Another publication number is CN101313972A, and the Chinese invention patent application that application number is 200710111732.8 discloses a kind of production technology of new preparation of six ingredients with rehmannia, and this method has adopted supercritical C0
2efficacy component in abstracting tree peony skin, Cortex Lycii; Other medical materials are through ethanol or water extraction, and aqueous extract is first collected macromole active substance by the method for ultrafilter membrane separation, and effluent adopts macroporous resin separated again, collects ethanol elution thing.The prescription of this patent is slightly different from pharmacopeia prescription in addition, is to substitute the Rhizoma Alismatis in original prescription with Cortex Lycii.
In above-described preparation method, majority is all the crude drug of part Poria to be done to Ordinary pulverization mode join in preparation, the shortcoming such as make that preparation exists that medical material granule is large, absorption difference, effect are slow; In the extraction of these preparation method active ingredients from traditional Chinese medicinals, that what adopt is reflux, extract, or decocting cooking method and common concentrated, baking seasoning is more, because of extract long through decocting, dry heated time, some thermally labile active ingredients easily go to pot, effective component extraction rate is not high, the medium-term and long-term heating of process in addition, expends the energy, again contaminated environment, waste time and energy, be unfavorable for realizing the modernization of Chinese medicine and produce.Though the useful supercritical C0 of document
2the modern crafts of paeonol in abstracting tree peony skin, but its treating capacity is little, in the high production of cost, is difficult for adopting.
Summary of the invention
The object of the invention is the defect for above preparation method, provide that a kind of effective component extraction rate is high, extraction time is short, the preparation method of the LIUWEIDIHUANG JIAONANG of energy savings.
The object of the invention is to be achieved by the following technical programs.A preparation method for LIUWEIDIHUANG JIAONANG, consists of the raw medicinal material of the following weight portion of Six-element: Radix Rehmanniae Preparata 1408g, Cortex Moutan 528g, Rhizoma Dioscoreae 704g, Fructus Corni 704g, Rhizoma Alismatis 528g, Poria 528g; Preparation method in turn includes the following steps: 1. first the Poria of 1/5th dosage (110g) is ground into 80 order coarse powder, vacuum drying is to moisture below 3%, then with jet mill, doing supersonic speed kinetic energy airflow pulverizes, obtain 75 μ m, micropowder below 200 orders is standby, and a small amount of thick slag merges with residue Poria; 2. residue Poria coarse powder being crossed to 80 orders, to take 10-12 water be doubly solvent, with ultrasonic extractor, extracts 2 times, and each 30-40 minute, obtains water extract filtrate and be concentrated in vacuo to paste; 3. the 8-10 of Fructus Corni being take ethanol is doubly solvent, with ultrasonic extractor, extracts secondary, and each 25-30 minute, filters, and medicinal residues are standby; Filtrate recycling ethanol, vacuum concentration is to thick paste shape, standby; 4. Cortex Moutan extraction by steam distillation paeonol adds cycloheptaamylose to make it be saturated solution with inclusion paeonol in distillate, and then K cryogenic treatment reactant liquor filters and collect paeonol cycloheptaamylose inclusion complex, and cold drying is standby; After extracting paeonol, residual liquid and the Cortex Moutan medicinal residues of distillating still gave over to rear use; 5. distillation the aqueous solution after paeonol and Cortex Moutan medicinal residues, Fructus Corni medicinal residues and all the other Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis three taste coarse powder to take the water of 10-12 times be solvent, with ultrasonic extractor, extract secondary, each 30-40 minute, filter, merging filtrate, passes through macroporous adsorptive resins, after use 70% ethanol elution, collect eluent, reclaim ethanol, and vacuum concentration is standby to thick paste shape; 6. above-mentioned water extract thick paste and Poria water extract mastic, Fructus Corni ethanol extraction mastic, Poria comminution by gas stream micropowder are merged, mix, drying under reduced pressure, be ground into fine powder, add above-mentioned paeonol cycloheptaamylose inclusion complex and adjuvant, mix, incapsulate, make 1000, every 0.3g, obtains.
1. described step refer to the Poria of 1/5th dosage (110g) in prescription be above crushed to 80 order coarse powder, and at vacuum 0.85～0.95Mpa, 60～70 ℃ of drying under reduced pressure to moisture are less than 4%; Then under 100,000 grades of environment of air cleaning, use comminution by gas stream crusher machine, feeding quantity span 14.8～29.6kg/h, air-flow operating pressure 8.61kg/cm
2; Obtain granule and be less than 75 μ m micropowders, standby.
Step 2. described ultrasonic extraction refers to the coarse pulverization of residue Poria crossed to 80 orders, with 10-12 times, and W/W, water is solvent, first in water, soak 1.5～2 hours, then, bathing at warm 60～70 ℃, with ultrasonic extractor, at 35～40kHz, extract 2 times, each 30～40min, filter afterwards, filtrate is at vacuum 0.85～0.95Mpa, and 60～70 ℃ are evaporated to relative density is 1.30～1.35, the equivalent extract of 50 ℃, standby.
3. described step is that Fructus Corni was pulverized to 80 orders, with 8-10 doubly, W/V, 70% ethanol is solvent, first soaks 1-1.5 hour, with ultrasonic extractor, at room temperature extracts secondary, and each 25-30 minute, filters, and medicinal residues are standby; Reclaim the ethanol in filtrate, then at vacuum 0.85～0.95Mpa, 60～70 ℃ are evaporated to relative density is the thick paste shape of 1.30～1.35,50 ℃, standby.
4. described step refers to shreds Cortex Moutan to distilling paeonol wherein with steam distillation below 10mm; In still-process, the cooling water outlet temperature of condenser remains on 60～70 ℃, is distilled to effluent no longer containing till paeonol; In distillate, add cycloheptaamylose to make it be saturated solution, 50～60 ℃ of stirring reactions 30～50 minutes; Cool, set to 0～4 ℃ of cold rooms are put 24 hours, then filter, and collect inclusion complex, standby after 60～70 ℃ of cold drying; Extraction after water liquid in distillating still and Cortex Moutan medicinal residues give over to is used.
Described step 4. in cycloheptaamylose consumption be 4～6 times of paeonol total amount in Cortex Moutan medical material, W/W.
The liquor ferri trichloridi that a little distillate adds one 5% if get when 4. described step distills to a certain extent presents viride nitens or aeruginous, represents that distillation not yet completes, if complete without the distillation of change color explanation paeonol.
5. described step refers to take 10-12 times of water as solvent soaking 1～1.5 hour the aqueous solution in distillating still and Cortex Moutan medicinal residues, Fructus Corni medicinal residues and all the other Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis three taste coarse powder after distillation paeonol, then with ultrasonic extractor, bathing at warm 60～70 ℃, at 35～40kHz, extract 2 times, each 30～40min, filter afterwards, filtrate is passed through D101 macroporous adsorptive resins with the flow velocity of 3.5BV/h; Use afterwards 70% ethanol with the flow velocity eluting desorbing of 2.5BV/h, collect eluent, reclaim ethanol, and at vacuum 0.85～0.95Mpa, 60～70 ℃ are evaporated to relative density is that the thick paste shape of 1.30～1.35,50 ℃ is standby.
Described step 5. in resin column pretreatment routinely.
6. described step refers to above Chinese medicine water extract thick paste, Poria water extract mastic, Fructus Corni ethanol extraction mastic and Poria comminution by gas stream thing micropowder is merged, mix, at vacuum 0.85～0.95Mpa, 60～70 ℃ of drying under reduced pressure, are ground into fine powder, add above-mentioned paeonol cycloheptaamylose inclusion complex and adjuvant, mix, incapsulate, make 1000, every 0.3g, obtains.
The invention has the beneficial effects as follows: the present invention adopts supersonic extracting method, can make the rapid stripping of active ingredient in crude drug cell, and remove from and under violent condition, make the efficacy component of medical material destroy, reach that active ingredient extraction ratio is high, extraction time is short, energy savings; The Poria of 1/5th dosage is done to supersonic speed kinetic energy airflow with jet mill at low temperatures and pulverize, obtain the micropowder below 75 μ m, drug particles is narrower than mechanical flour method far away.Granule is thinner, is also just more easily absorbed by the body, and the difference that just can eliminate to greatest extent because absorbing causes the ill effect of human body to drug absorption; Paeonol cycloheptaamylose inclusion technique, effectively prevent the impact of light, oxygen and hydrolysising condition, increased the stability of volatile component, not only effectively improved the retention index in preparation of volatile ingredient, and hidden preferably dense penetrating odor, be more convenient for taking.With former technique with contrast file comparison new technology and overcome deficiency wherein, product quality meets or is better than the quality standard of former process stipulation completely, and the while is beneficial to again realizes low-carbon environment-friendly and energy-conservation requirement, for realizing Chinese medicine preparation modernization, has strided forward major step.
The specific embodiment
embodiment:prescription is Radix Rehmanniae Preparata 14.08Kg, Cortex Moutan 5.28Kg, Rhizoma Dioscoreae 7.04Kg, Fructus Corni 7.04Kg, Rhizoma Alismatis 2.28Kg, Poria 5.29Kg.
the preparation of Poria micropowder:get part Poria 1.06Kg in prescription and be crushed to the coarse powder below 80 orders, at vacuum 0.85～0.95Mpa, 60～70 ℃ of decompression drying to moisture are less than 4%.Then with jet mill, pulverize 100,000 grades of air cleaning environment, feeding quantity span 14.8～29.6kg/h, air-flow operating pressure 8.61kg/cm
2.Receive to obtain micropowder 0.92Kg, yield 84%, micro powder granule is less than 75 μ m(200 orders).A small amount of residual thick Poria merges stand-by with residue Poria medical material.
the preparation of Poria water extract:to remain Poria 4.19Kg coarse pulverization (crossing 80 orders), take 50.3Kg water as solvent, first in water, soak 1.5 hours, then bathing at warm 60～70 ℃, with ultrasonic extractor, at 35kHz, extract 2 times each 30min, filter afterwards, filtrate is used in vacuum 0.85～0.95Mpa, and 60～70 ℃ are evaporated to relative density is 1.30～1.35(50 ℃) dense thick extractum, standby.
the preparation of Fructus Corni ethanol extraction:7.04Kg Fructus Corni is pulverized to (crossing 80 orders), with 56.32L
,70% ethanol is solvent, first soaks 1 hour, with ultrasonic extractor, at room temperature extracts secondary, each 25 minutes, filter, and medicinal residues are standby.Reclaim the ethanol in filtrate, then at vacuum 0.85～0.95Mpa, 60～70 ℃ are evaporated to relative density is 1.30～1.35(50 ℃) thick paste, standby.
the preparation of paeonol β-CD inclusion complex:5.28Kg Cortex Moutan chopping (10mm is following) is extracted to paeonol with volatile oil distillator.The cooling water outlet temperature of condenser remains on 60～70 ℃, is distilled to effluent no longer containing till paeonol.In distillate, add cycloheptaamylose to make it be saturated solution (cycloheptaamylose consumption is approximately 0.42kg), 50～60 ℃ of stirring reactions 30 minutes.Cool, set to 0～4 ℃ of cold rooms are put 24 hours, then filter, and collect inclusion complex, standby after 60～70 ℃ of cold drying.Extraction after water liquid in distillating still and Cortex Moutan medicinal residues give over to is used.
the preparation of medical material water extract:aqueous solution in distillating still and Cortex Moutan medicinal residues, Fructus Corni medicinal residues and all the other Radix Rehmanniae Preparata 14.08Kg, Rhizoma Dioscoreae 7.04Kg, Rhizoma Alismatis 5.28Kg tri-taste coarse powder after distillation paeonol be take to 316Kg water (comprise and distill the aqueous solution in distillating still after paeonol) as solvent soaking 1 hour, then with ultrasonic extractor, bathing at warm 60～70 ℃, at 40kHz, extract 2 times, each 40min, filter afterwards, filtrate is passed through D101 macroporous adsorptive resins (resin pretreatment routinely) with the flow velocity of 3.5BV/h.Use afterwards 70% ethanol with the flow velocity desorbing of 2.5BV/h, collect eluent, reclaim ethanol, and at vacuum 0.85～0.95Mpa, 60～70 ℃ are evaporated to relative density is 1.30～1.35(50 ℃) thick paste shape standby.
recording of capsule:above Chinese medicine water extract thick paste, Poria water extract mastic, Fructus Corni ethanol extraction mastic and Poria comminution by gas stream thing micropowder are merged, mix, at vacuum 0.85～0.95Mpa, 60～70 ℃ of drying under reduced pressure, are ground into fine powder, add above-mentioned paeonol cycloheptaamylose inclusion complex and appropriate amount of auxiliary materials, mix, pour into capsule, make 10000 (0.3g/ grains), obtain LIUWEIDIHUANG JIAONANG finished product.
Finished product requires to test according to the quality standard of former technology establishment, and result is as follows.
[character]this product is capsule, and content is that light brown is to brown powder or granule; Bitter in the mouth, micro-acid.Up to specification.
[discriminating](1) get this product, put micro-Microscopic observation: irregular branched agglomerate is colourless, meet chloral hydrate liquid and dissolve; Hyphae colorless or light brown, diameter 4～6 μ m.
Result: up to specification.
(2) get this product content 0.6g (0.3g/ grain), add kieselguhr 2g, grind well, the 40ml that adds diethyl ether, reflux 1 hour, filters, and filtrate is reclaimed ether, and residue adds acetone 0.5ml to be made to dissolve, as need testing solution.Separately get paeonol reference substance, add acetone and make every 1ml containing the solution of 1mg, in contrast product solution.According to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2000), test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, thiacyclohexane-the ethyl acetate (3:1) of take is developing solvent, launch, take out, dry, spray is with 5% acid ferric chloride alcoholic solution (5% ferric chloride alcoholic solution 10ml, adds hydrochloric acid 2ml, mixes), it is clear that hot blast blows to speckle colour developing, in test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle of aobvious same color.
Result: up to specification.
[inspection] checks according to appendix I L of Chinese Pharmacopoeia version in 2000, should meet every regulation relevant under capsule item.
Result: up to specification.
[assay] Cortex Moutan: get the content 0.15g (0.3g/ grain) under content uniformity item, accurately weighed, with vapor distillation, collect the about 450ml of distillate, put in 500ml measuring bottle, be diluted with water to scale, according to spectrophotography (appendix VA of Chinese Pharmacopoeia version in 2000), at 274nm wavelength place, measure trap, by paeonol (C
9h
10o
3) absorptance (E1%cm) be 862 calculating, obtain.
Result: every contains Cortex Moutan with paeonol (C
9h
10o
3) meter, be 6.35mg/ grain.
Fructus Corni: the content of getting under content uniformity item is appropriate, porphyrize mixes, get the about 0.6g of fine powder (0.3g/ grain) accurately weighed, put in apparatus,Soxhlet's, add diethyl ether appropriate, reflux 4 hours, extracting solution evaporate to dryness, residue adds appropriate dehydrated alcohol-chloroform (3:2) mixed liquor, and slight fever makes to dissolve, quantitatively be transferred in 5ml measuring bottle, and be diluted to scale, shake up, as need testing solution.Separately get ursolic acid reference substance, add dehydrated alcohol and make every 1ml containing the solution of 0.5mg, product solution in contrast, according to thin layer chromatography (appendix VI B of Chinese Pharmacopoeia version in 2000), test, draw above-mentioned need testing solution 10 μ l, reference substance solution 4 μ l and 8 μ l, put respectively on same silica gel g thin-layer plate, thiacyclohexane-chloroform-ethyl acetate-the methanol (25:15:5:2) of take is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, at 110 ℃, be dried to speckle colour developing clear, take out, on lamellae, cover onesize glass plate, use immobilization with adhesive tape around, according to thin layer chromatography (appendix VIB thin slice scan of Chinese Pharmacopoeia version in 2000), scan, wavelength: λ s=520nm, λ R=700nm, measure test sample trap integrated value and reference substance trap integrated value, calculate, obtain.
Result: every contains Fructus Corni with ursolic acid (C
10h
48o
3) meter, be 0.73mg/ grain.
The former handicraft product quality of this technique comparison sheet.
From upper table result, learn, product prepared by the present invention is compared every test item with former handicraft product and is all reached requirement, and index components paeonol, ursolic acid content are higher than former technique.
Claims (9)
1. a preparation method for LIUWEIDIHUANG JIAONANG, consists of the raw medicinal material of the following weight portion of Six-element: Radix Rehmanniae Preparata 1408g, Cortex Moutan 528g, Rhizoma Dioscoreae 704g, Fructus Corni 704g, Rhizoma Alismatis 528g, Poria 528g; It is characterized in that, preparation method in turn includes the following steps: 1. first the Poria of 1/5th dosage (110g) is ground into 80 order coarse powder, vacuum drying is to moisture below 3%, then with jet mill, doing supersonic speed kinetic energy airflow pulverizes, obtain 75 μ m, micropowder below 200 orders is standby, and a small amount of thick slag merges with residue Poria; 2. residue Poria coarse powder being crossed to 80 orders, to take 10-12 water be doubly solvent, with ultrasonic extractor, extracts 2 times, and each 30-40 minute, obtains water extract filtrate and be concentrated in vacuo to paste; 3. the 8-10 of Fructus Corni being take ethanol is doubly solvent, with ultrasonic extractor, extracts secondary, and each 25-30 minute, filters, and medicinal residues are standby; Filtrate recycling ethanol, vacuum concentration is to thick paste shape, standby; 4. Cortex Moutan extraction by steam distillation paeonol adds cycloheptaamylose to make it be saturated solution with inclusion paeonol in distillate, and then K cryogenic treatment reactant liquor filters and collect paeonol cycloheptaamylose inclusion complex, and cold drying is standby; After extracting paeonol, residual liquid and the Cortex Moutan medicinal residues of distillating still gave over to rear use; 5. distillation the aqueous solution after paeonol and Cortex Moutan medicinal residues, Fructus Corni medicinal residues and all the other Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis three taste coarse powder to take the water of 10-12 times be solvent, with ultrasonic extractor, extract secondary, each 30-40 minute, filter, merging filtrate, passes through macroporous adsorptive resins, after use 70% ethanol elution, collect eluent, reclaim ethanol, and vacuum concentration is standby to thick paste shape; 6. above-mentioned water extract thick paste and Poria water extract mastic, Fructus Corni ethanol extraction mastic, Poria comminution by gas stream micropowder are merged, mix, drying under reduced pressure, be ground into fine powder, add above-mentioned paeonol cycloheptaamylose inclusion complex and adjuvant, mix, incapsulate, make 1000, every 0.3g, obtains.
2. the preparation method of a kind of LIUWEIDIHUANG JIAONANG according to claim 1, it is characterized in that: 1. described step refers to the Poria of 1/5th dosage (110g) in writing out a prescription is above crushed to 80 order coarse powder, at vacuum 0.85～0.95Mpa, 60～70 ℃ of drying under reduced pressure to moisture are less than 4%; Then under 100,000 grades of environment of air cleaning, use comminution by gas stream crusher machine, feeding quantity span 14.8～29.6kg/h, air-flow operating pressure 8.61kg/cm
2; Obtain granule and be less than 75 μ m micropowders, standby.
3. the preparation method of a kind of LIUWEIDIHUANG JIAONANG according to claim 1, it is characterized in that: step 2. described ultrasonic extraction refers to the coarse pulverization of residue Poria is crossed to 80 orders, with 10-12 doubly, W/W, water is solvent, first in water, soak 1.5～2 hours, then bathing at warm 60～70 ℃, with ultrasonic extractor, at 35～40kHz, extract 2 times, each 30～40min, filters afterwards, filtrate is at vacuum 0.85～0.95Mpa, 60～70 ℃ are evaporated to relative density is the equivalent extract of 1.30～1.35,50 ℃, standby.
4. the preparation method of a kind of LIUWEIDIHUANG JIAONANG according to claim 1, it is characterized in that: 3. described step is that Fructus Corni was pulverized to 80 orders, with 8-10 doubly, W/V, 70% ethanol is solvent, first soaks 1-1.5 hour, with ultrasonic extractor, at room temperature extract secondary, each 25-30 minute, filters, and medicinal residues are standby; Reclaim the ethanol in filtrate, then at vacuum 0.85～0.95Mpa, 60～70 ℃ are evaporated to relative density is the thick paste shape of 1.30～1.35,50 ℃, standby.
5. the preparation method of a kind of LIUWEIDIHUANG JIAONANG according to claim 1, is characterized in that: 4. described step refers to shreds Cortex Moutan to distilling paeonol wherein with steam distillation below 10mm; In still-process, the cooling water outlet temperature of condenser remains on 60～70 ℃, is distilled to effluent no longer containing till paeonol; In distillate, add cycloheptaamylose to make it be saturated solution, 50～60 ℃ of stirring reactions 30～50 minutes; Cool, set to 0～4 ℃ of cold rooms are put 24 hours, then filter, and collect inclusion complex, standby after 60～70 ℃ of cold drying; Extraction after water liquid in distillating still and Cortex Moutan medicinal residues give over to is used.
6. a kind of preparation method of LIUWEIDIHUANG JIAONANG according to claim 1 or 5, is characterized in that: described step 4. in cycloheptaamylose consumption be 4～6 times of paeonol total amount in Cortex Moutan medical material, W/W.
7. the preparation method of a kind of LIUWEIDIHUANG JIAONANG according to claim 5, it is characterized in that: the liquor ferri trichloridi that a little distillate adds one 5% if get when 4. described step distills to a certain extent presents viride nitens or aeruginous, represent that distillation not yet completes, if complete without the distillation of change color explanation paeonol.
8. the preparation method of a kind of LIUWEIDIHUANG JIAONANG according to claim 1, it is characterized in that: 5. described step refers to take 10-12 times of water as solvent soaking 1～1.5 hour the aqueous solution in distillating still and Cortex Moutan medicinal residues, Fructus Corni medicinal residues and all the other Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis three taste coarse powder after distillation paeonol, then with ultrasonic extractor, bathing at warm 60～70 ℃, at 35～40kHz, extract 2 times, each 30～40min, filter afterwards, filtrate is passed through D101 macroporous adsorptive resins with the flow velocity of 3.5BV/h; Use afterwards 70% ethanol with the flow velocity eluting desorbing of 2.5BV/h, collect eluent, reclaim ethanol, and at vacuum 0.85～0.95Mpa, 60～70 ℃ are evaporated to relative density is that the thick paste shape of 1.30～1.35,50 ℃ is standby.
9. the preparation method of a kind of LIUWEIDIHUANG JIAONANG according to claim 1, it is characterized in that: 6. described step refers to above Chinese medicine water extract thick paste, Poria water extract mastic, Fructus Corni ethanol extraction mastic and Poria comminution by gas stream thing micropowder are merged, mix, at vacuum 0.85～0.95Mpa, 60～70 ℃ of drying under reduced pressure, be ground into fine powder, add above-mentioned paeonol cycloheptaamylose inclusion complex and adjuvant, mix, incapsulate, make 1000, every 0.3g, obtains.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111700921A (en) * | 2020-06-24 | 2020-09-25 | 鲁南新时代生物技术有限公司 | Method for producing anti-depression medicine by using micro powder technology |
| CN115137786A (en) * | 2022-07-29 | 2022-10-04 | 吉林省民泰制药股份有限公司 | A capsule containing six ingredients with rehmanniae radix and its preparation method |
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| CN115137786A (en) * | 2022-07-29 | 2022-10-04 | 吉林省民泰制药股份有限公司 | A capsule containing six ingredients with rehmanniae radix and its preparation method |
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Application publication date: 20141015 |