CN101428128A - Process for producing Anzhongsan formulation - Google Patents
Process for producing Anzhongsan formulation Download PDFInfo
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- CN101428128A CN101428128A CNA2007101662907A CN200710166290A CN101428128A CN 101428128 A CN101428128 A CN 101428128A CN A2007101662907 A CNA2007101662907 A CN A2007101662907A CN 200710166290 A CN200710166290 A CN 200710166290A CN 101428128 A CN101428128 A CN 101428128A
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Abstract
The invention belongs to the technical field of traditional Chinese medicine, in particular to a preparation method of an Anzhong San preparation. In order to return to the essence of the traditional medicine for treating diseases, the invention proposes the guideline that the classic formula of the Anzhong San is in line with the ancient way, medicine is extracted by water, and the preparation method combines the modern concentration and granulation processes, thereby summing up preparation process parameters and applicable excipients which are most matched with the Anzhong San preparation. The accumulated experiences of the traditional medicine are retained to the maximum extent, and the preparation method can also meet the needs of preparation forms which are applicable to the rapid pace of modern society, such as granules, tablets, capsules, powder, dropping pills, etc.
Description
[technical field]
The invention belongs to technical field of Chinese medicines, be specifically related to a kind of regulating the spleen and stomach powder preparation and preparation method thereof.
[background technology]
Regulating the spleen and stomach sheds from " prescription of peaceful benevolent dispensary ".It is the agent of controlling pricking caused by the stagnation of QI and blood.The chronicity spasmic pain that is used to control weak body constitution is main.Can treat after deficiency and coldness anemia, vomiting, the food or on an empty stomach, heart bottom can hypodynia or dull pain, the time acid regurgitation water or hypogastric region are arranged to the target of diseases such as waist generation dragging pain for using.Its indication is: gastric ulcer, duodenal ulcer, gastroptosis, chronic gastritis, hyperchlorhydria, nerve stomachache, hysteria.Use utilization clinically with reference to often being: the malignant histocytosis vomiting adds the Rhizoma Pinelliae, Poria.Women's blood stasis adds rhizoma sparganic, Rhizoma Curcumae.Flatulence adds Pingwei San.
The scientific research group of Frankfurt University medical science institute of viruses finds that the glycyrrhizin that refines from the Radix Glycyrrhizae root has good inhibition effect to SARS virus laboratory research.Compare with the antiviral drugs virazole that generally adopts at present, its curative effect is more obvious.Scientist believes, utilizes glycyrrhizin to be expected to develop than the present used more effective new drug of antiviral.The physician develops medicine with glycyrrhizin as effective ingredient before this, treatment hepatitis C and acquired immune deficiency syndrome (AIDS) etc., and obtained certain effect.
Thereby the diarrhoea that the glycyrrhizin content of conclusive evidence regulating the spleen and stomach in the loosing digestive tract disease, the especially virus that cause for increasing virus at present cause has the Chinese medicine meaning.
In recent decades, the production of Chinese herbal medicine has realized mechanization and semi-mechanization to a certain degree.Chinese medicine often is considered to that active constituent content is low, impurity is many, quality is unstable, so medication is based upon on the empirical basis more, can not integrate with modern medicine.For addressing this problem, Chinese medicine must be walked the road of extraction and purification.The extraction of Chinese medicine comprises many unit operationss such as leaching, clarification, filtration and evaporation.
[summary of the invention]
The preparation method that the purpose of this invention is to provide a kind of new regulating the spleen and stomach powder preparation.Basis of the present invention prescription derives from regulating the spleen and stomach and looses.
Regulating the spleen and stomach powder preparation prescription of the present invention is: Cortex cinnamomi japonici (Ramulus Cinnamomi) 40 weight portions, Rhizoma Corydalis, each 30 weight portion of Concha Ostreae, Fructus Foeniculi 15 weight portions, Radix Glycyrrhizae, each 10 weight portions and Rhizoma Alpiniae Officinarum 5 weight portion of sand that contract, its preparation method is: Cortex cinnamomi japonici (Ramulus Cinnamomi), Rhizoma Corydalis, Concha Ostreae, Fructus Foeniculi, Radix Glycyrrhizae, contract sand and Rhizoma Alpiniae Officinarum are decocted with water 0.5-3 hour at every turn 2-4 time, merge decocting liquid, filter the back concentrate fluid extract, add behind the adjuvant with behind the fluidized bed granulation useful in preparing drug formulations.
The proportion of above-mentioned fluid extract is 1.10-1.30, preferred 1.15-1.30.
Above-mentioned decocting liquid can carry out centrifugation earlier, gets clarifying decocting liquid, and centrifugal rotation speed is 1500-20000 rev/min, and preferred 1500-10000 rev/min, more preferably 2000-8000 rev/min, most preferably 3000-5000 rev/min.
Above-mentioned decocting liquid can adopt the method for membrane filtration to filter.
Above-mentioned membrane filtration comprises one of filter method of employing ultrafiltration and nanofiltration or ultrafiltration and nanofiltration is used in combination.
Above-mentioned ultrafilter membrane is selected from cellulose diacetate film, three cellulose acetate membrane, cyanoethyl cellulose film, polysulfone membrane, sulfonated polysulfone membrane, poly (ether sulfone) film, sulfonated polyether sulfone film, polysulfonamides film, phenolphthalein side group polyarylsulfone (PAS) film, polyvinylidene fluoride film, polyacrylonitrile film, polyimide film, cellulose membrane, methyl methacrylate-acrylonitrile copolymer film, polyacrylonitrile-cellulose diacetate blend film, the dynamic ultrafilter membrane that forms, one of and the Modified Membrane of above-mentioned film, its molecular retention amount is below the 6000-10000.
The filter membrane aperture of above-mentioned ultrafiltration is: the 0.22-0.45 micron.
The membrane ultrafiltration device that above-mentioned ultrafiltration is adopted can be commercial doughnut or plate ultrafilter membrane separator.
Above-mentioned NF membrane molecular retention amount is 500-2000, preferred 500-1000, more preferably 700-1000.
The process of above-mentioned membrane filtration preferably with the process ultrafiltration earlier of decocting liquid, is carried out nanofiltration again.
Above-mentioned adjuvant is selected from microcrystalline Cellulose, powdery cellulose, mannitol, starch, lactose, gelatin, methylcellulose, dextrin, pregelatinized Starch, micropowder silica gel, hydroxypropyl methylcellulose, cross-linking sodium carboxymethyl cellulose, carboxymethyl starch sodium, Polyethylene Glycol, xylitol, lactose, glucose, glycine, mannitol, tartaric acid, silicon dioxide, one or more in calcium stearate and the magnesium stearate.
The said medicine preparation comprises granule, tablet, capsule, powder, drop pill.
In the above-mentioned fluidized bed granulation process, the optimization technique parameter of fluid bed fluidized granulating is: atomisation pressure 0.15-0.45 MPa; Temperature of charge 50-65 ℃; Inlet temperature 68-100 ℃; Leaving air temp 35-65 ℃; Preferably, atomisation pressure 0.15-0.45 MPa; Temperature of charge 55-60 ℃; Inlet temperature 80-100 ℃; Leaving air temp 60-65 ℃.
The technical study of fluid bed boiling patent of the present invention comprises:
1. dosage form selection: according to the clinical application needs, square taste of Chinese medicine character and active ingredient physicochemical property thereof and a day clothes crude drug amount in conjunction with factors such as the market demands, are selected dosage form.The present invention should be developed into dosage forms such as granule, capsule, tablet, drop pill, soft capsule, powder, syrup preparation or dispersible tablet, and they can satisfy the clinical day big needs of clothes dosage, and preserve, transport, carry and taking convenience.
But when granulating, find the water extraction after-filtration, put boiling granulating in the fluid bed again.The process route of drafting had both shortened production technology, had reduced supplementary product consumption again, was beneficial to molding.
2. isolation and purification technical study: the former prescription of this product day clothes crude drug amount is big, therefore should discard the dross and select the essential as far as possible, and it is more that water is carried the part impurities, as macromolecular substances and solid particles such as protein, phlegmatic temperaments.Also can adopt centrifugal (2000-20000 rev/min) method, reach impurity-eliminating effect.
3. concentration technology research: method for concentration is selected, and controls and avoid loss of effective components, water to carry medicinal liquid for the ease of production operation to concentrate, and getting relative density is the clear paste of 1.10-1.30.
4. granulating process research: (1) method of granulating is investigated: method of granulating once adopted wet granulation, selected for use Different concentrations of alcohol and PVP to granulate, and easily bonding is softening because of extractum, and operating difficulties is so abandon this kind method.Boiling method in the fluid bed is adopted in the back, for mix homogeneously, after the merging of water extract, adds an amount of adjuvant, mixing, and boiling granulating in fluid bed, promptly.
The investigation of fluidized granulating important technological parameters is screened the fluidized granulating important technological parameters, and concrete outcome sees Table 1.
Table 1 fluidized granulating important technological parameters is investigated
The important technological parameters of fluid bed fluidized granulating is as seen from the above table: atomisation pressure 0.15-0.45 MPa; Temperature of charge 50-65 ℃; Inlet temperature 68-100 ℃; Leaving air temp 35-65 ℃.
The at present used extracting technique of Chinese medicine compound recipes that adopt certain density ethanol extraction Chinese medicine more, help reclaiming solvent like this and reduce impurity, but the method that adopts alcohol extraction has deviated from the experience accumulation of the treatment disease of Chinese medicine since 3000, has ignored for the purpose that can arrive " quality controllable " comparatively simply under the guiding theory of " modernization of Chinese medicine " " effectiveness " even " safety ".
In sum, the hysteresis of Chinese medicine extraction separating technology development becomes the bottleneck of traditional Chinese medicine development and existence, must be optimized, reform and strengthen original technology.The reinforcement technique of chemical separating and mass transfer will provide strong assurance for this reason, and realization Chinese medicine subject intersects with Chemical Engineering, will help realizing the modernization of Chinese medicine production equipment.With the Chinese medicine extraction separation process that induces one of notion, the theory of Chemical Engineering.Utilize available research achievements,,, technological process, production equipment, operating condition are done modernization overlay and careful groping, provided feasible scheme from basic influence factor's research staff in conjunction with the concrete condition that Chinese medicine is produced.
In order to return the marrow of traditional medicine treatment disease, the present invention proposes the guiding theory according to " abiding by Gu " with the diffusing classics side of regulating the spleen and stomach, use the water extraction medicine, concentrated, granulating process in conjunction with modern have summed up the preparation process parameter and the suitable adjuvant that mate the most with the regulating the spleen and stomach powder preparation.Kept the experience accumulation of traditional medicine to greatest extent, and it is allegro as dosage forms such as tablet, capsule, granule, powder, drop pills to adapt to modern society.
[specific embodiment]
Following embodiment further describes the present invention, but described embodiment only is used to illustrate the present invention rather than restriction the present invention.Various medical materials feed intake and are among the embodiment: Cortex cinnamomi japonici (Ramulus Cinnamomi) 400 grams, and Rhizoma Corydalis, each 300 gram of Concha Ostreae, Fructus Foeniculi 150 grams, Radix Glycyrrhizae, the sand that contracts are 100 grams and Rhizoma Alpiniae Officinarum 50 grams respectively.
Embodiment 1
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times with water extraction, each 2 hours, amount of water was 12 times of medical material, merge the water extract, filter decompression and solvent recovery, get fluid extract (proportion is 1.13-1.18), add adjuvant boiling granulating in fluid bed, promptly get granular preparation of the present invention.
Embodiment 2
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 3 times with water extraction, each 2 hours, amount of water was 8 times of medical material, merge the water extract, filter, decompression and solvent recovery gets fluid extract (proportion is 1.15-1.21), add adjuvant boiling granulating in fluid bed, encapsulated, promptly obtain capsule preparations of the present invention.
Embodiment 3
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 3 times with water extraction, each 2 hours, amount of water was 10 times of medical material, merged the water extract, filter, decompression and solvent recovery gets fluid extract (proportion is 1.10-1.19), adds adjuvant boiling granulating in fluid bed, add the adjuvant tabletting, promptly obtain tablet of the present invention.
Embodiment 4
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times with water extraction, each 3 hours, amount of water was 10 times of medical material, merge the water extract, filter, decompression and solvent recovery gets fluid extract (proportion is 1.20-1.26), add adjuvant boiling granulating in fluid bed, add vegetable oil substrate, pill promptly obtains drop pill of the present invention.
Embodiment 5
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times with water extraction, each 2.5 hours, amount of water was 10 times of medical material, merge the water extract, filter, decompression and solvent recovery gets fluid extract (proportion is 1.19-1.25), add adjuvant boiling granulating in fluid bed, add 800 gram vegetable oil, mix homogeneously promptly obtains soft capsule of the present invention with being pressed into soft capsule after the colloid mill grinding.
Embodiment 6
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 3 times with water extraction, each 1.5 hours, amount of water was 10 times of medical material, merge the water extract, filter, decompression and solvent recovery gets fluid extract (proportion is 1.20-1.24), add adjuvant boiling granulating in fluid bed, pulverize, promptly obtain powder of the present invention.
Embodiment 7
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times with water extraction, each 2 hours, amount of water was 6 times of medical material, merged the water extract, filtered, and filtrate is 8000 three cellulose acetate membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.It is to handle in 500 the rolling nanofiltration device that ultrafiltration gained filtrate is selected molecular cut off for use through system, wherein the nanofiltration amount of water can be controlled in about 0.85 times of former ultrafiltrate, get fluid extract (proportion is 1.18-1.27), add adjuvant boiling granulating in fluid bed, promptly get granular preparation of the present invention.
Embodiment 8
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 3 times with water extraction, each 2 hours, amount of water was 8 times of medical material, merged the water extract, filtered, and filtrate is 6000 cyanoethyl cellulose membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.It is to handle in 500 the rolling nanofiltration device that ultrafiltration gained filtrate is selected molecular cut off for use through system, wherein the nanofiltration amount of water can be controlled in about 0.8 times of former ultrafiltrate, get fluid extract (proportion is 1.25-1.30), add adjuvant boiling granulating in fluid bed, encapsulated, promptly obtain capsule preparations of the present invention.
Embodiment 9
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 3 times with water extraction, each 2 hours, amount of water was 6 times of medical material, merged the water extract, filtered, and filtrate is 10000 polysulfone membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.It is to handle in 500 the rolling nanofiltration device that ultrafiltration gained filtrate is selected molecular cut off for use through system, wherein the nanofiltration amount of water can be controlled in about 0.75 times of former ultrafiltrate, get fluid extract (proportion is 1.28-1.30), add adjuvant boiling granulating in fluid bed, add the adjuvant tabletting, promptly obtain tablet of the present invention.
Embodiment 10
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times with water extraction, each 3 hours, amount of water was 10 times of medical material, merged the water extract, filtered, and filtrate is 6000 SPSF membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.It is to handle in 1000 the rolling nanofiltration device that ultrafiltration gained filtrate is selected molecular cut off for use through system, wherein the nanofiltration amount of water can be controlled in about 0.7 times of former ultrafiltrate, get fluid extract (proportion is 1.26-1.30), add adjuvant boiling granulating in fluid bed, add vegetable oil substrate, pill promptly obtains drop pill of the present invention.
Embodiment 11
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times with water extraction, each 2.5 hours, amount of water was 10 times of medical material, merged the water extract, filtered, and filtrate is 8000 poly (ether sulfone) film ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.It is to handle in 2000 the rolling nanofiltration device that ultrafiltration gained filtrate is selected molecular cut off for use through system, wherein the nanofiltration amount of water can be controlled in about 0.75 times of former ultrafiltrate, get fluid extract (proportion is 1.21-1.30), add adjuvant boiling granulating in fluid bed, add 200 gram vegetable oil, mix homogeneously promptly obtains soft capsule of the present invention with being pressed into soft capsule after the colloid mill grinding.
Embodiment 12
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 3 times with water extraction, each 1.5 hours, amount of water was 10 times of medical material, merged the water extract, filtered, and filtrate is 6000 sulfonated polyether sulfone membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.It is to handle in 500 the rolling nanofiltration device that ultrafiltration gained filtrate is selected molecular cut off for use through system, wherein the nanofiltration amount of water can be controlled in about 0.65 times of former ultrafiltrate, get fluid extract (proportion is 1.28-1.30), add adjuvant boiling granulating in fluid bed, pulverize, promptly obtain powder of the present invention.
Embodiment 13
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times each 2 hours with water extraction, amount of water is 8 times of medical material, merges the water extract, centrifugal (rotating speed is 2000 rev/mins), filter, filtrate is 6000 three cellulose acetate membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.Ultrafiltration gained filtrate decompression reclaims solvent, gets fluid extract (proportion is 1.15-1.25), adds adjuvant boiling granulating in fluid bed, promptly gets granular preparation of the present invention.
Embodiment 14
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 3 times each 2 hours with water extraction, amount of water is 8 times of medical material, merges the water extract, centrifugal (rotating speed is 2500 rev/mins), filter, filtrate is 8000 cyanoethyl cellulose membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.Ultrafiltration gained filtrate decompression reclaims solvent, gets fluid extract (proportion is 1.17-1.24), adds adjuvant boiling granulating in fluid bed, and is encapsulated, promptly obtains capsule preparations of the present invention.
Embodiment 15
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times each 2 hours with water extraction, amount of water is 8 times of medical material, merges the water extract, centrifugal (rotating speed is 5000 rev/mins), filter, filtrate is 6000 polysulfone membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.Ultrafiltration gained filtrate decompression reclaims solvent, gets fluid extract (proportion is 1.18-1.30), adds adjuvant boiling granulating in fluid bed, adds the adjuvant tabletting, promptly obtains tablet of the present invention.
Embodiment 16
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times each 3 hours with water extraction, amount of water is 8 times of medical material, merges the water extract, centrifugal (rotating speed is 3000 rev/mins), filter, filtrate is 6000 SPSF membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.Ultrafiltration gained filtrate decompression reclaims solvent, gets fluid extract (proportion is 1.24-1.29), adds adjuvant boiling granulating in fluid bed, adds vegetable oil substrate, and pill promptly obtains drop pill of the present invention.
Embodiment 17
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 2 times each 2.5 hours with water extraction, amount of water is 8 times of medical material, merges the water extract, centrifugal (rotating speed is 8000 rev/mins), filter, filtrate is 6000 poly (ether sulfone) film ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.Ultrafiltration gained filtrate decompression recovery solvent gets fluid extract (proportion is 1.21-1.29), adds adjuvant boiling granulating in fluid bed, adds 200 gram vegetable oil, and mix homogeneously promptly obtains soft capsule of the present invention with being pressed into soft capsule after the colloid mill grinding.
Embodiment 18
Take by weighing the pulverizing medicinal materials of recipe quantity, decoct 3 times each 1.5 hours with water extraction, amount of water is 8 times of medical material, merges the water extract, centrifugal (rotating speed is 10000 rev/mins), filter, filtrate is 6000 sulfonated polyether sulfone membrane ultrafiltration with molecular cut off, filter type employing cross flow filter.The operating condition of ultrafiltration technology is: the inlet pressure of ultrafiltration is 0.1 MPa, and low 0.5 kPa of the liquid outlet pressure ratio inlet pressure of ultrafiltration progressively boosts during ultrafiltration.In ultra-filtration process, adopt the periodic pressure fluctuation, the pressure wave moment is 0.1 MPa.Ultrafiltration gained filtrate decompression reclaims solvent, gets fluid extract (proportion is 1.29-1.30), adds adjuvant boiling granulating in fluid bed, pulverizes, and promptly obtains powder of the present invention.
Determining of the amount of experimental example 1-dry extract of the present invention
Embodiment 1-18 fluid extract with among the present invention does not add adjuvant, and directly lyophilization obtains dry extract, data such as following table 1:
The data of the amount of table 1 dry extract of the present invention
By realization of the present invention, can be under the prerequisite that the effective ingredient in the Chinese medicine preparation of the present invention is extracted to greatest extent, reducing in the extract macromolecular substances such as impurity such as tannin, polyphenol, resin, protein, phlegmatic temperament and solid particle effectively removes, the active ingredient that keeps medicine is for the preparation of oral drug preparation is provided convenience.
Glycyrrhizin assay in the experimental example 2-dry extract of the present invention
1 material and instrument
1.1 material
Embodiment 1-18 fluid extract (not adding adjuvant) is lyophilization gained dry extract directly.Methanol is chromatographic grade; Other reagent is analytical pure.
1.2 instrument
SPD-10AVP type high performance liquid chromatograph (day island proper Tianjin company); LibrorAEG-200 electronic balance (day island proper Tianjin company).
2 assays
2.1 chromatographic condition
With methanol-water-acetic acid (88: 11: 1) is mobile phase, and ODS-3 post (150mm * 4.6mm, 5 μ m) is an immobile phase, and detecting flow velocity at ultraviolet 250nm is 1.0 ml/min.
2.2 reagent
Methanol (chromatographically pure), glacial acetic acid (analytical pure), distilled water, glycyrrhizin reference substance
2.3 the investigation of the range of linearity
The preparation precision of reference substance stock solution takes by weighing 25 milligrams of glycyrrhizin reference substances, puts in 50 milliliters of measuring bottles, adds dissolve with methanol and is diluted to scale, shakes up, and makes per 1 milliliter of solution that contains 1 milligram, in contrast the product stock solution.Accurate above-mentioned reference substance stock solution (1 milligram/1 milliliter) 0.1,0.5,1.0,2.0,5.0,8.0,10.0 milliliters of drawing is put in 10 milliliters of measuring bottles, adds methanol and is diluted to scale, shakes up.The therefrom accurate respectively 10 μ l that draw inject chromatograph of liquid, the record peak area.The range of linearity of glycyrrhizin is 0.2884-1.4420 μ g (r=0.9998).
2.4 the preparation of reference substance solution: precision takes by weighing 25 milligrams of glycyrrhizin reference substances, put in 50 milliliters of measuring bottles, add dissolve with methanol and be diluted to scale, shake up, accurate again absorption is put in 50 milliliters of measuring bottles for 10 milliliters, adds dissolve with methanol and is diluted to scale, shakes up, make per 1 milliliter of solution that contains 0.1 milligram, in contrast product solution.
2.5. the preparation of need testing solution: get the about 0.25g of sample of the present invention (embodiment 1-18), porphyrize.Precision takes by weighing, and puts in 50 milliliters of measuring bottles, adds about 45 milliliters of methanol, and supersound extraction is 30 minutes respectively, the cooling back is diluted to scale with methanol, shakes up, and leaves standstill, and gets supernatant and filters with microporous filter membrane (0.45 μ m), discard filtrate just, get subsequent filtrate 10 μ l, inject chromatograph of liquid, the results are shown in Table 1.
The table 1 sample ultrasonic time is investigated
3. conclusion: guaranteed the stable content of glycyrrhizin among the present invention, for the standardization production of preparation is laid a good foundation.By realization of the present invention, under the prerequisite that can extract to greatest extent at the effective ingredient during regulating the spleen and stomach is loose, reducing in the extract macromolecular substances such as impurity such as tannin, polyphenol, resin, protein, phlegmatic temperament and solid particle effectively removes, keep the active ingredient in the medical material, for the preparation of oral drug preparation is provided convenience.
Claims (7)
1. the preparation method of a regulating the spleen and stomach powder preparation, its prescription consists of Cortex cinnamomi japonici (Ramulus Cinnamomi) 40 weight portions, Rhizoma Corydalis, each 30 weight portion of Concha Ostreae, Fructus Foeniculi 15 weight portions, Radix Glycyrrhizae, each 10 weight portion of sand that contract, Rhizoma Alpiniae Officinarum 5 weight portions is characterized in that, Cortex cinnamomi japonici (Ramulus Cinnamomi), Rhizoma Corydalis, Concha Ostreae, Fructus Foeniculi, Radix Glycyrrhizae, contract sand and Rhizoma Alpiniae Officinarum are decocted with water 2-4 time, each 0.5-3 hour, merge decocting liquid, filter the back concentrate fluid extract, add behind the adjuvant with behind the fluidized bed granulation useful in preparing drug formulations.
2. preparation method according to claim 1, the proportion that it is characterized in that described fluid extract is 1.10-1.30.
3. preparation method according to claim 2, the proportion that it is characterized in that described fluid extract is 1.15-1.30.
4.. preparation method according to claim 1 is characterized in that described decocting liquid can carry out centrifugation earlier, gets clarifying decocting liquid, centrifugal rotation speed is 1500-20000 rev/min.
5. according to the arbitrary described preparation method of claim 1-4, it is characterized in that described decocting liquid can adopt the method for membrane filtration to filter.
6. preparation method according to claim 5 is characterized in that described membrane filtration comprises ultrafiltration and nanofiltration.
7. preparation method according to claim 6, the process that it is characterized in that described membrane filtration is carried out nanofiltration again for the process ultrafiltration earlier of decocting liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101662907A CN101428128A (en) | 2007-11-09 | 2007-11-09 | Process for producing Anzhongsan formulation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101662907A CN101428128A (en) | 2007-11-09 | 2007-11-09 | Process for producing Anzhongsan formulation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101428128A true CN101428128A (en) | 2009-05-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101662907A Pending CN101428128A (en) | 2007-11-09 | 2007-11-09 | Process for producing Anzhongsan formulation |
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| Country | Link |
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| CN (1) | CN101428128A (en) |
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2007
- 2007-11-09 CN CNA2007101662907A patent/CN101428128A/en active Pending
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Open date: 20090513 |