CN101530590A - Pearl capsule with twenty-five components, preparation method and quality detection method thereof - Google Patents
Pearl capsule with twenty-five components, preparation method and quality detection method thereof Download PDFInfo
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Abstract
The invention provides pearl capsule with twenty-five components, a preparation method and a quality detection method thereof. The preparation method includes steps of dividing the twenty-five medicinal materials into four parts, namely mineral and precious medicine, precious and refine medicine, medicinal material containing volatile oil and medicinal material containing water-soluble components, crushing the mineral and precious medicine to 80 mesh, uniformly mixing; crushing the medicinal material containing high volatile oil to crude powder, extracting volatile oil, using beta-cyclodextrin for clathration; carrying out water extraction for the medicinal material containing water-soluble components, concentrating to relative density of 1.25-1.35 under reduction pressure, mixing the three parts, drying at 60-80 DEG C, crushing to 80 mesh; respectively grinding the precious and refine medicine, namely buffalo horn concentrated powder, cow-bezoar and musk into fine powder, mixing, adding beta-cyclodextrin and dextrin for mixing, and packaging into capsule. The high efficiency liquid chromatogram method is used for detecting content of piperine, and the thin layer chromatography method is used for discriminating nine objects.
Description
Technical field:
The present invention relates to new Chinese medicine technical field, particularly a kind of pearl capsule with twenty-five components and preparation method thereof and quality determining method.
Background technology:
Cerebrovascular disease is to become a main class important diseases with the cerebral arteries systemic disease, and anxious because of its morbidity, the state of an illness is heavy, classifies the emphasis problem clinically always as and studies.This disease traditional Chinese medical science is called apoplexy, often shows as hemiplegia, aphasia etc.Mainly be to cause clinical show as cerebral thrombosis and cerebral hemorrhages because vascular lesion, blood pressure and blood change three aspects more.
It is that tube wall is narrow because cerebrovascular wall sclerotic degeneration makes endarterium coarse that cerebral hemorrhage forms, slow blood flow, and blood formed element adheres to diseased region, impels thrombosis.Having under the hypertensive situation, can increase the weight of arteriosclerosis, impel the necrosis of arteriosclerotic tube wall generation internal hemorrhage, thereby form cerebral thrombosis.Cerebral hemorrhage is on hypertension and arteriosclerosis basis, because of overexert or too excitement blood pressure is raise suddenly, cause rupture of blood vessel in brain hemorrhage.
Because pathogeny is different with the cause of disease, Therapeutic Method also differs.To the treatment of cerebral embolism and cerebral hemorrhage, doctor trained in Western medicine is mainly used treatments such as low molecular dextran vasodilation anticoagulant.The traditional Chinese medical science is main to improve cerebral blood circulation, as FUFANG DANSHEN ZHUSHEYE, troxerutin, MAILUONING etc. with the promoting blood circulation to remove obstruction in the collateral.Though Chinese and western medicine has the multiple Drug therapy should disease, mostly the course of treatment long, medication inconvenience, curative effect is also not satisfactory, and Tibetan medicine and pharmacology has a long history in China, is China's national medicine treasure-house, is the important component part of Chinese medicine.
Former Tibetan medicine masterpiece " the Supreme Being's agate that is stated from the 17th century in Christian era of 25-component pearl ball.Pellet increases Peng and arranges the doctor to show selected works " in, the function that having calms the nerves has one's ideas straightened out through the ancient Chinese medicine doctor clinical verification, has very significant curative effect in diseases such as treatment apoplexy and hemiplegia, be the classics recipe in the Tibetanmedicine, so " Chinese pharmacopoeia nineteen ninety-five version version in 2000, all collections in succession of version in 2005.
Because the 25-component pearl ball is traditional water-honeyed pill dosage form, dose is big, difficult disintegrate, and bioavailability is low, is difficult for the due curative effect of performance.
Over nearly more than 20 years, along with the application and the development of modern biotechnology, cyclodextrin (CD) has been realized suitability for industrialized production, and cost descends significantly.Therefore, increasing about its research report, the application of beta-schardinger dextrin-in Chinese materia medica is increasingly extensive, and the beta-cyclodextrin inclusion compound Study on Technology especially becomes the focus that the Chinese medicine novel form is studied with exploitation.
Inclusion technique more and more widely applies in the Chinese medicine preparation, because of the limitation and the required particular technology condition of inclusion technique of beta-schardinger dextrin-self, cause many researchs to only limit to laboratory, and suitability for industrialized production is less.Along with science and technology development, and the development and application of cyclodextrin derivative, adopt inclusion technique developmental research Chinese medicine novel form, new varieties to hold out broad prospects.
Beta-schardinger dextrin-and medicine enclose are a kind of physical processes, chemical reaction does not take place, make medicine still keep original character and effect, after being prepared as clathrate, cut off contacting of drug molecule and surrounding to a certain extent, avoided being subjected to the influence of light, oxygen and hydrolysising condition, improved bioavailability of medicament, increase stability of drug, and can reduce the ease mistake of volatile medicine, prolonged drug effect and shelf-life.
Summary of the invention:
One of purpose of the present invention is the deficiency that overcomes prior art, and a kind of pearl capsule with twenty-five components is provided;
Of the present invention two provide a kind of preparation method of pearl capsule with twenty-five components;
Three of purpose of the present invention provides a kind of quality determining method of pearl capsule with twenty-five components.
Purpose of the present invention realizes according to following proposal:
Pearl capsule with twenty-five components, its prescription is:
Margarita 8.44g Semen Myristicae 16.89g Tufa 42.23g
Fructus Tsaoko 12.67g Flos Caryophylli 21.11g Lignum Dalbergiae Odoriferae 42.23g
Fructus Amomi Rotundus 16.89g Fructus Chebulae 54.89g Lignum Santali Albi 33.78g
Fructus Phyllanthi 42.23g Lignum Aquilariae Resinatum 33.78g Cortex cinnamomi japonici (Ramulus Cinnamomi) 16.89g
Fructus Terminaliae Billericae 42.23g Eriocheir sinensis 21.11g Radix Aucklandiae 33.78g
Fructus Malvae 33.78g Fructus Piperis Longi 16.89g seedling of Fructus Fragariae Ananssae 42.23g
Lapis Micae Aureus 16.89g Pulvis Cornus Bubali Concentratus 25.34g seed of Ajowan 16.89g.
Stigma Croci 8.44g Semen Nigellae 12.67g Calculus Bovis 0.42g
Moschus 0.42g;
25-component medical material in the prescription is divided into mineral substance and valuable medicine, expensive thin medicine, contains the volatile oil medical material, contains water soluble ingredient medical material four parts, mineral medicine and valuable medicinal were crushed to 80 mesh sieves, mix homogeneously; The pulverizing medicinal materials that will contain the innage that volatilizees becomes coarse powder, extracts volatile oil, uses beta-cyclodextrin inclusion compound; After will containing water soluble ingredient medical material water and carrying, be evaporated to relative density 1.25～1.35, with above three partially mixed, 60 ℃～80 ℃ dryings, pulverized 80 mesh sieves; With expensive thin medicine: Pulvis Cornus Bubali Concentratus, Calculus Bovis, Moschus grind to form fine powder respectively, behind the facing-up, add beta-schardinger dextrin-and dextrin and mix, and be encapsulated;
Described mineral substance and valuable medicine are meant Eriocheir sinensis, Lapis Micae Aureus, Tufa, Stigma Croci, Fructus Piperis Longi, Margarita;
The described medical material that contains the innage that volatilizees is meant Semen Myristicae, Fructus Tsaoko, Lignum Santali Albi, Cortex cinnamomi japonici (Ramulus Cinnamomi), Lignum Aquilariae Resinatum, Flos Caryophylli, Fructus Amomi Rotundus, the Radix Aucklandiae, Lignum Dalbergiae Odoriferae, Semen Nigellae, seed of Ajowan;
The described water soluble ingredient medical material that contains is meant Fructus Chebulae, Fructus Phyllanthi, Fructus Terminaliae Billericae, Fructus Malvae, seedling of Fructus Fragariae Ananssae.
The preparation method of pearl capsule with twenty-five components, its raw material is: Margarita, Semen Myristicae, Tufa, Fructus Tsaoko, Flos Caryophylli, Lignum Dalbergiae Odoriferae, Fructus Amomi Rotundus, the Fructus Chebulae, Lignum Santali Albi, Fructus Phyllanthi, Lignum Aquilariae Resinatum, Cortex cinnamomi japonici (Ramulus Cinnamomi), Fructus Terminaliae Billericae, Eriocheir sinensis, the Radix Aucklandiae, Fructus Malvae, Fructus Piperis Longi, seedling of Fructus Fragariae Ananssae, Lapis Micae Aureus, Pulvis Cornus Bubali Concentratus, seed of Ajowan, Stigma Croci, Semen Nigellae, Calculus Bovis, Moschus, 25-component medical material in the prescription is divided into mineral substance and valuable medicine, expensive thin medicine, contain the volatile oil medical material, contain water soluble ingredient medical material four parts, mineral medicine and valuable medicinal were crushed to 80 mesh sieves, mix homogeneously; The pulverizing medicinal materials that will contain the innage that volatilizees becomes coarse powder, extracts volatile oil, uses beta-cyclodextrin inclusion compound; After will containing water soluble ingredient medical material water and carrying, be evaporated to relative density 1.25～1.35, with above three partially mixed, 60 ℃～80 ℃ dryings, pulverized 80 mesh sieves; With expensive thin medicine: Pulvis Cornus Bubali Concentratus, Calculus Bovis, Moschus grind to form fine powder respectively, behind the facing-up, add beta-schardinger dextrin-and dextrin and mix, and be encapsulated;
The technology of described extraction volatile oil is, raw material adds 8 times of water gagings, volatile oil is collected in ultrasonic distillation 6 hours, uses beta-cyclodextrin inclusion compound volatile oil, beta-schardinger dextrin-and volatile oil ratio are 6-8:1,40 ℃ of dry 4h, clathrate, carry the medical material filtering liquid medicine behind the volatile oil, add 6 times of water gaging supersound extraction 1 hour again, 2 times extracting solution merges;
The described water soluble ingredient medical material extraction process by water that contains is that raw material adds 8 times of water gagings, supersound extraction 3 times, each one hour, 3 extracting solution merging.
The pearl capsule with twenty-five components assay adopts high performance liquid chromatography, measures the content of piperine in the preparation, and its chromatographic condition is: with octadecyl silane is filler, and methanol-water: 77:33 is a mobile phase; Detect wavelength 343nm, number of theoretical plate calculates by the piperine peak and is not less than 1500.
The pearl capsule with twenty-five components composition differentiates that selecting Lignum Aquilariae Resinatum, Flos Caryophylli, Margarita, Calculus Bovis, the Radix Aucklandiae, Lignum Dalbergiae Odoriferae, Fructus Piperis Longi, Cortex cinnamomi japonici (Ramulus Cinnamomi), Stigma Croci is detected object, adopt thin layer chromatography, prepare sample solution and reference substance solution earlier, two kinds of solution put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, comparison colour developing situation;
The discrimination method of described Lignum Aquilariae Resinatum composition is: get capsule 's content 6g, and the 40ml that adds diethyl ether, supersound process 30 minutes filters, and filtrate volatilizes, and residue adds methanol 1ml as need testing solution; Other gets Lignum Aquilariae Resinatum control medicinal material 0.8g, shine medical material solution in pairs with legal system, according to draw each 10 μ l of above-mentioned two kinds of solution according to thin layer chromatography, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with normal hexane-ethyl acetate-formic acid 9:1:0.2, be developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, be heated to clear spot at 105 ℃, on test agent and the corresponding position of control medicinal material chromatograph, as showing the speckle of same color, then composition exists;
The discrimination method of described Flos Caryophylli composition is: get capsule 's content 4g, and the 20ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and residue adds dehydrated alcohol 1ml dissolving, as need testing solution; It is an amount of that other gets the eugenol reference substance, adds dehydrated alcohol and make the solution that every 1ml contains 1 μ l, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with petroleum ether (60-90 ℃)-ethyl acetate 9:1, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, it is clear to developing the color to be heated to speckle at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists;
The discrimination method of described pearl composition is: get capsule 's content 3g, add acetone 20ml, supersound process 20 minutes, filter, 0.2g is got in the medicinal residues oven dry, put in the peace bottle, add dilute hydrochloric acid test solution 5ml, seal, put in the baking oven, 105 ℃ were heated 20 hours, took out, and supernatant is as need testing solution, other gets Margarita control medicinal material 0.02g, shine medical material solution in pairs with legal system,, draw above-mentioned two kinds of each 4ul of solution according to the thin layer chromatography test, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with phenol-water 7:2 is developing solvent, launches, and takes out, 105 ℃ were heated 5-10 minute, spray immediately with 0.2% ethanol solution of ninhydrin, it is clear to developing the color to be heated to speckle at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as show the speckle of same color, then composition exists;
The discrimination method of described Calculus Bovis composition is: get capsule 's content 8g, add methanol 30ml, supersound process 30 minutes filters, and filtrate is waved to 5ml, as need testing solution.Other gets cholic acid, the Hyodeoxycholic Acid reference substance is an amount of, makes the mixed solution that every 1ml contains 1mg with methanol, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of each 10ul of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with normal hexane-ethyl acetate-acetic acid-methanol 20:25:2:3 upper solution, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, it is clear to be heated to speckle colour developing at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists;
The discrimination method of described Radix Aucklandiae composition is: get capsule 's content 8g, add chloroform 30ml, supersound process 30 minutes filters, and filtrate is waved to 1ml, as need testing solution; Other removes hydrogen constuslactone reference substance, costunolide reference substance, adds chloroform and makes the mixed solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with chloroform-cyclohexane extraction 5:1, launch, take out, dry, the vanillin sulfuric acid solution of spray 1%, it is clear to be heated to the speckle colour developing, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists;
The discrimination method of described Lignum Dalbergiae Odoriferae composition is: get capsule 's content 6g, and the 30ml that adds diethyl ether, supersound process 30 minutes filters, and filtrate volatilizes, and residue adds ethanol 1ml dissolving, as need testing solution; Other gets Lignum Dalbergiae Odoriferae control medicinal material 0.5g, shine medical material solution in pairs with legal system, draw need testing solution 10 μ l according to thin layer chromatography, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-ether-chloroform 7:2:1 is developing solvent, launch, take out, dry, spray is with 1% vanillin sulfuric acid solution and dehydrated alcohol (1:9) mixed liquor, it is clear to be heated to speckle colour developing at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists;
The discrimination method of described Fructus Piperis Longi composition is: get capsule 's content 5.0g, add dehydrated alcohol 30ml, supersound process 30 minutes, filter, filtrate is concentrated into 2ml, and as need testing solution, it is an amount of that other gets the piperine reference substance, add dehydrated alcohol and make the solution that every 1ml contains piperine 2mg, product solution according to the thin layer chromatography test, is drawn above-mentioned two kinds of solution, 10 μ l in contrast, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-ethyl acetate-acetone 7:2:1 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as show the speckle of same color, then composition exists;
The discrimination method of described Cortex cinnamomi japonici (Ramulus Cinnamomi) composition is: get this product content 6g, 20ml adds diethyl ether, supersound process 30 minutes, filter, filtrate is waved to 2ml, as need testing solution, it is an amount of that other gets the cinnamic aldehyde reference substance, adds diethyl ether to make the reference substance solution that every 1ml contains cinnamic aldehyde 1 μ l, tests according to thin layer chromatography, draw need testing solution 5 μ l, reference substance solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with petroleum ether (60-90 ℃)-ethyl acetate (9:1), launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, on test agent and the corresponding position of reference substance chromatograph, as show the speckle of same color, then composition exists;
The discrimination method of described Stigma Croci composition is: differentiate: get this product content 3g, add methanol 20ml, supersound process 10 minutes, leave standstill and make clarification, get supernatant as need testing solution, other gets Stigma Croci control medicinal material 20mg, shine medical material solution in pairs with legal system, according to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ethyl acetate-methanol-water 100:16.5:13.5 is developing solvent, launch, take out, dry, inspect under the daylight, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists.
One of characteristics of the present invention are: the inclusion technique that adopts beta-cyclodextrin inclusion compound volatile oil, overcome in the conventional formulation and volatile oil directly to be sprayed on drug powder or particulate way, avoid the ease of volatile oil to lose, increased stability of drug, improved bioavailability of medicament.
Two of characteristics of the present invention are: the medical material supersound extraction, concentrating under reduced pressure, the drying that will contain water soluble ingredient in will writing out a prescription; Be characterized in proposing to contain in the medical material effective ingredient of physiologically active, thereby patient's dose is greatly reduced, have only half of former dosage form 25-component pearl ball, increased the compliance that the patient takes medicine greatly, help improving the curative effect of medicine.
Description of drawings:
Fig. 1 is technological process of production figure of the present invention.
The specific embodiment:
Describe the present invention with example below in conjunction with accompanying drawing,
To produce 1000 preparation units is example:
Prescription: Margarita 8.44g Semen Myristicae 16.89g Tufa 42.23g
Fructus Tsaoko 12.67g Flos Caryophylli 21.11g Lignum Dalbergiae Odoriferae 42.23g
Fructus Amomi Rotundus 16.89g Fructus Chebulae 54.89g Lignum Santali Albi 33.78g
Fructus Phyllanthi 42.23g Lignum Aquilariae Resinatum 33.78g Cortex cinnamomi japonici (Ramulus Cinnamomi) 16.89g
Fructus Terminaliae Billericae 42.23g Eriocheir sinensis 21.11g Radix Aucklandiae 33.78g
Fructus Malvae 33.78g Fructus Piperis Longi 16.89g seedling of Fructus Fragariae Ananssae 42.23g
Lapis Micae Aureus 16.89g Pulvis Cornus Bubali Concentratus 25.34g seed of Ajowan 16.89g.
Stigma Croci 8.44g Semen Nigellae 12.67g Calculus Bovis 0.42g
Moschus 0.42g
With classification and the chemical property of the 25-component medical material in the prescription, be divided into the valuable medicine of mineral substance, expensive thin medicine, contain the volatile oil medical material, contain water soluble ingredient medical material four parts according to each flavour of a drug.
A group: Eriocheir sinensis, Tufa, Stigma Croci, Lapis Micae Aureus, Fructus Piperis Longi, Margarita powder are broken into fine powder, cross 80 mesh sieves, mix homogeneously;
B group: Semen Myristicae, Fructus Tsaoko, Lignum Santali Albi, Cortex cinnamomi japonici (Ramulus Cinnamomi), Lignum Aquilariae Resinatum, Flos Caryophylli, Fructus Amomi Rotundus, the Radix Aucklandiae, Lignum Dalbergiae Odoriferae, Semen Nigellae, seed of Ajowan are mixed, are ground into coarse powder, add 8 times of water gagings, ultrasonic distillation 6 hours, collect volatile oil, with 40 ℃ of dry 4h of beta-cyclodextrin inclusion compound volatile oil (beta-schardinger dextrin-and volatile oil ratio are 6-8:1), get clathrate.Carry the medical material filtering liquid medicine behind the volatile oil, add 6 times of water gaging supersound extraction 1 hour again, 2 times extracting solution merges;
The C group: Fructus Chebulae, Fructus Phyllanthi, Fructus Terminaliae Billericae, Fructus Malvae, seedling of Fructus Fragariae Ananssae mix, are ground into coarse powder, add 8 times of water gagings, supersound extraction 3 times, and each one hour, 3 times extracting solution merged.
Above extracting solution filters respectively, merges concentrating under reduced pressure (60 ℃ of mensuration; relative density 1.25～1.35); mix with A group medicated powder,, pulverized 80 mesh sieves 80 ℃ of dryings; with expensive thin medicine: Pulvis Cornus Bubali Concentratus, Calculus Bovis, Moschus grind to form fine powder respectively; with the medicated powder facing-up, add Benexate Hydrochloride, add an amount of dextrin mix homogeneously; with No. 1 capsule dress capsule, 0.25 gram/grain.
Assay: adopting high performance liquid chromatography, is filler with octadecyl silane, and methanol-water (77:33) is a mobile phase; Detect wavelength 343nm.Number of theoretical plate calculates by the piperine peak should be not less than 1500.The preparation of reference substance solution: it is an amount of that precision takes by weighing the piperine reference substance, puts in the brown measuring bottle, adds dehydrated alcohol and make the solution that every 1ml contains 15 μ g, standby.Precision is measured above-mentioned solution 2ml and is put in the brown measuring bottle of 25ml during mensuration, adds dehydrated alcohol to scale, shakes up, in contrast product solution.The preparation of need testing solution: get the content under this product content uniformity inspection item, porphyrize, precision take by weighing about 0.4g, put in the brown measuring bottle of 25ml, add the about 20ml of dehydrated alcohol, supersound process 20 minutes is put coldly, is diluted to scale with dehydrated alcohol, shake up, filter with dry filter, discard filtrate just, get subsequent filtrate as need testing solution.Algoscopy: accurate respectively reference substance solution and each 4 μ l of need testing solution of drawing, inject high performance liquid chromatograph, measure, promptly.Every of the present invention contains Fructus Piperis Longi with piperine (C
17H
19NO
3) meter, must not be less than 0.18mg.
Composition is differentiated:
1, Lignum Aquilariae Resinatum is differentiated: get capsule 's content 6g, and the 40ml that adds diethyl ether, supersound process 30 minutes filters, and filtrate volatilizes, and residue adds methanol 1ml as need testing solution.Other gets Lignum Aquilariae Resinatum control medicinal material 0.8g, shines medical material solution in pairs with legal system.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with normal hexane-ethyl acetate-formic acid (9:1:0.2) is developing solvent, launch, take out, dry, spray is heated to clear spot with 5% vanillin sulfuric acid solution at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of identical color, then composition exists.
2, Flos Caryophylli is differentiated: get capsule 's content 4g, and the 20ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and residue adds dehydrated alcohol 1ml dissolving, as need testing solution.It is an amount of that other gets the eugenol reference substance, adds dehydrated alcohol and make the solution that every 1ml contains 1 μ l, in contrast product solution.According to thin layer chromatography (" appendix VIB of Chinese pharmacopoeia version in 2005) test, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with petroleum ether (60-90 ℃)-ethyl acetate (9:1) is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, as showing the speckle of same color, then composition exists.
3, Margarita is differentiated: get capsule 's content 3g, add acetone 20ml, supersound process 20 minutes, filter, 0.2g is got in the medicinal residues oven dry, put in the peace bottle, add dilute hydrochloric acid test solution 5ml, seal, put in the baking oven, 105 ℃ were heated 20 hours, take out, supernatant is as need testing solution. and other gets Margarita control medicinal material 0.02g, shines medical material solution in pairs with legal system.According to thin layer chromatography (" appendix VIB of Chinese pharmacopoeia version in 2005) test, draw above-mentioned two kinds of each 4ul of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with phenol-water (7:2) is developing solvent, launch, take out, 105 ℃ were heated 5-10 minute, spray immediately with 0.2% ethanol solution of ninhydrin, it is clear to be heated to speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of identical color, then composition exists.
4, Calculus Bovis is differentiated: get capsule 's content 8g, add methanol 30ml, supersound process 30 minutes filters, and filtrate is waved to 5ml, as need testing solution.Other gets cholic acid, the Hyodeoxycholic Acid reference substance is an amount of, makes the mixed solution that every 1ml contains 1mg with methanol, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw above-mentioned two kinds of each 10ul of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with normal hexane-ethyl acetate-acetic acid-methanol (20:25:2:3) upper solution is developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, as showing the speckle of same color, then composition exists.
5, the Radix Aucklandiae is differentiated: get capsule 's content 8g, add chloroform 30ml, supersound process 30 minutes filters, and filtrate is waved to 1ml, as need testing solution.Other removes hydrogen constuslactone reference substance, costunolide reference substance, adds chloroform and makes the mixed solution that every 1ml contains 0.5mg, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with chloroform-cyclohexane extraction (5:1) is developing solvent, launch, take out, dry, spray 1% vanillin sulfuric acid solution, it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of identical color, then composition exists.
6, Lignum Dalbergiae Odoriferae is differentiated: get capsule 's content 6g, and the 30ml that adds diethyl ether, supersound process 30 minutes filters, and filtrate volatilizes, and residue adds ethanol 1ml dissolving, as need testing solution.Other gets Lignum Dalbergiae Odoriferae control medicinal material 0.5g, shines medical material solution in pairs with legal system.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution 10 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with toluene-ether-chloroform (7:2:1), launch, take out, dry, spray is with 1% vanillin sulfuric acid solution and dehydrated alcohol (1:9) mixed liquor, 105 ℃ be heated to speckle develop the color clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
7, Fructus Piperis Longi is differentiated: get capsule 's content 5.0g, add dehydrated alcohol 30ml, supersound process 30 minutes filters, and filtrate is concentrated into 2ml, as need testing solution.It is an amount of that other gets the piperine reference substance, adds dehydrated alcohol and make the solution that every 1ml contains piperine 2mg, in contrast product solution.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw above-mentioned two kinds of solution, 10 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with benzene-ethyl acetate-acetone (7:2:1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, as showing the speckle of same color, then composition exists.
8, Cortex cinnamomi japonici (Ramulus Cinnamomi) is differentiated: get capsule 's content 6g, and the 20ml that adds diethyl ether, supersound process 30 minutes filters, and filtrate is waved to 2ml, as need testing solution.It is an amount of that other gets the cinnamic aldehyde reference substance, adds diethyl ether to make the reference substance solution that every 1ml contains cinnamic aldehyde 1 μ l.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw need testing solution 5 μ l, reference substance solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with petroleum ether (60-90 ℃)-ethyl acetate (9:1), launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of identical color, then composition exists.
9, Stigma Croci is differentiated: get capsule 's content 3g, add methanol 20ml, supersound process 10 minutes leaves standstill and makes clarification, gets supernatant as need testing solution.Other gets Stigma Croci control medicinal material 20mg, shines medical material solution in pairs with legal system.According to thin layer chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with ethyl acetate-methanol-water (100:16.5:13.5), launch, take out, dry, inspect under the daylight, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of identical color, then composition exists.
Claims (21)
1, pearl capsule with twenty-five components, its prescription is:
Margarita 8.44g Semen Myristicae 16.89g Tufa 42.23g
Fructus Tsaoko 12.67g Flos Caryophylli 21.11g Lignum Dalbergiae Odoriferae 42.23g
Fructus Amomi Rotundus 16.89g Fructus Chebulae 54.89g Lignum Santali Albi 33.78g
Fructus Phyllanthi 42.23g Lignum Aquilariae Resinatum 33.78g Cortex cinnamomi japonici (Ramulus Cinnamomi) 16.89g
Fructus Terminaliae Billericae 42.23g Eriocheir sinensis 21.11g Radix Aucklandiae 33.78g
Fructus Malvae 33.78g Fructus Piperis Longi 16.89g seedling of Fructus Fragariae Ananssae 42.23g
Lapis Micae Aureus 16.89g Pulvis Cornus Bubali Concentratus 25.34g seed of Ajowan 16.89g.
Stigma Croci 8.44g Semen Nigellae 12.67g Calculus Bovis 0.42g
Moschus 0.42g;
It is characterized in that the 25-component medical material in the prescription is divided into mineral substance and valuable medicine, expensive thin medicine, contains the volatile oil medical material, contains water soluble ingredient medical material four parts, mineral medicine and valuable medicinal were crushed to 80 mesh sieves, mix homogeneously; The pulverizing medicinal materials that will contain the innage that volatilizees becomes coarse powder, extracts volatile oil, uses beta-cyclodextrin inclusion compound; After will containing water soluble ingredient medical material water and carrying, be evaporated to relative density 1.25～1.35, with above three partially mixed, 60 ℃～80 ℃ dryings, pulverized 80 mesh sieves; With expensive thin medicine: Pulvis Cornus Bubali Concentratus, Calculus Bovis, Moschus grind to form fine powder respectively, behind the facing-up, add beta-schardinger dextrin-and dextrin and mix, and be encapsulated.
2, pearl capsule with twenty-five components as claimed in claim 1 is characterized in that described mineral substance and valuable medicine are meant Eriocheir sinensis, Lapis Micae Aureus, Tufa, Stigma Croci, Fructus Piperis Longi, Margarita.
3, pearl capsule with twenty-five components as claimed in claim 1 is characterized in that the described medical material that contains the innage that volatilizees is meant Semen Myristicae, Fructus Tsaoko, Lignum Santali Albi, Cortex cinnamomi japonici (Ramulus Cinnamomi), Lignum Aquilariae Resinatum, Flos Caryophylli, Fructus Amomi Rotundus, the Radix Aucklandiae, Lignum Dalbergiae Odoriferae, Semen Nigellae, seed of Ajowan.
4, pearl capsule with twenty-five components as claimed in claim 1 is characterized in that the described water soluble ingredient medical material that contains is meant Fructus Chebulae, Fructus Phyllanthi, Fructus Terminaliae Billericae, Fructus Malvae, seedling of Fructus Fragariae Ananssae.
5, the preparation method of pearl capsule with twenty-five components, its raw material is: Margarita, Semen Myristicae, Tufa, Fructus Tsaoko, Flos Caryophylli, Lignum Dalbergiae Odoriferae, Fructus Amomi Rotundus, the Fructus Chebulae, Lignum Santali Albi, Fructus Phyllanthi, Lignum Aquilariae Resinatum, Cortex cinnamomi japonici (Ramulus Cinnamomi), Fructus Terminaliae Billericae, Eriocheir sinensis, the Radix Aucklandiae, Fructus Malvae, Fructus Piperis Longi, seedling of Fructus Fragariae Ananssae, Lapis Micae Aureus, Pulvis Cornus Bubali Concentratus, seed of Ajowan, Stigma Croci, Semen Nigellae, Calculus Bovis, Moschus, it is characterized in that the 25-component medical material in the prescription is divided into mineral substance and valuable medicine, expensive thin medicine, contain the volatile oil medical material, contain water soluble ingredient medical material four parts, mineral medicine and valuable medicinal were crushed to 80 mesh sieves, mix homogeneously; The pulverizing medicinal materials that will contain the innage that volatilizees becomes coarse powder, extracts volatile oil, uses beta-cyclodextrin inclusion compound; After will containing water soluble ingredient medical material water and carrying, be evaporated to relative density 1.25～1.35, with above three partially mixed, 60 ℃～80 ℃ dryings, pulverized 80 mesh sieves; With expensive thin medicine: Pulvis Cornus Bubali Concentratus, Calculus Bovis, Moschus grind to form fine powder respectively, behind the facing-up, add beta-schardinger dextrin-and dextrin and mix, and be encapsulated.
6, the preparation method of pearl capsule with twenty-five components as claimed in claim 5 is characterized in that described mineral substance and valuable medicine are meant Eriocheir sinensis, Tufa, Stigma Croci, Fructus Piperis Longi, Margarita.
7, the preparation method of pearl capsule with twenty-five components as claimed in claim 5 is characterized in that the described medical material that contains the innage that volatilizees is meant Semen Myristicae, Fructus Tsaoko, Lignum Santali Albi, Cortex cinnamomi japonici (Ramulus Cinnamomi), Lignum Aquilariae Resinatum, Flos Caryophylli, Fructus Amomi Rotundus, the Radix Aucklandiae, Lignum Dalbergiae Odoriferae, Semen Nigellae, seed of Ajowan.
8, the preparation method of pearl capsule with twenty-five components as claimed in claim 5 is characterized in that the described water soluble ingredient medical material that contains is meant Fructus Chebulae, Fructus Phyllanthi, Fructus Terminaliae Billericae, Fructus Malvae, seedling of Fructus Fragariae Ananssae.
9, the preparation method of pearl capsule with twenty-five components as claimed in claim 5, it is characterized in that describedly extracting to such an extent that the technology of volatile oil is that raw material adds 8 times of water gagings, ultrasonic distillation 6 hours, collect volatile oil, use beta-cyclodextrin inclusion compound volatile oil, beta-schardinger dextrin-and volatile oil ratio are 6-8:1,40 ℃ of dry 4h, get clathrate, carry the medical material filtering liquid medicine behind the volatile oil, add 6 times of water gaging supersound extraction 1 hour again, 2 times extracting solution merges.
10, the preparation method of pearl capsule with twenty-five components as claimed in claim 5 is characterized in that the described water soluble ingredient medical material extraction process by water that contains is, raw material adds 8 times of water gagings, supersound extraction 3 times, and each one hour, 3 times extracting solution merged.
11, pearl capsule with twenty-five components quality determining method as claimed in claim 1, it is characterized in that adopting the content of piperine in the high effective liquid chromatography for measuring preparation, its chromatographic condition is: with octadecyl silane is filler, and methanol-water: 77:33 is a mobile phase; Detect wavelength 343nm, number of theoretical plate calculates by the piperine peak and is not less than 1500.
12, pearl capsule with twenty-five components quality determining method as claimed in claim 1; it is characterized in that it is detected object that Lignum Aquilariae Resinatum, Flos Caryophylli, Margarita, Calculus Bovis, the Radix Aucklandiae, Lignum Dalbergiae Odoriferae, Fructus Piperis Longi, Cortex cinnamomi japonici (Ramulus Cinnamomi), Stigma Croci are selected in the composition discriminating; adopt thin layer chromatography; prepare sample solution and reference substance solution earlier; two kinds of solution put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, comparison colour developing situation.
13, pearl capsule with twenty-five components quality determining method as claimed in claim 12, it is characterized in that the discrimination method of Lignum Aquilariae Resinatum composition is: get capsule 's content 6g, 40ml adds diethyl ether, supersound process 30 minutes, filter, filtrate volatilizes, and residue adds methanol 1ml as need testing solution; Other gets Lignum Aquilariae Resinatum control medicinal material 0.8g, shine medical material solution in pairs with legal system, draw each 10 μ l of above-mentioned two kinds of solution according to thin layer chromatography, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with normal hexane-ethyl acetate-formic acid 9:1:0.2, be developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, be heated to clear spot at 105 ℃, on test agent and the corresponding position of control medicinal material chromatograph, as showing the speckle of same color, then composition exists.
14, pearl capsule with twenty-five components quality determining method as claimed in claim 12, it is characterized in that the discrimination method of Flos Caryophylli composition is: get capsule 's content 4g, 20ml adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, residue adds dehydrated alcohol 1ml dissolving, as need testing solution; It is an amount of that other gets the eugenol reference substance, adds dehydrated alcohol and make the solution that every 1ml contains 1 μ l, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with petroleum ether (60-90 ℃)-ethyl acetate 9:1, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, it is clear to developing the color to be heated to speckle at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists.
15, pearl capsule with twenty-five components quality determining method as claimed in claim 12, the discrimination method that it is characterized in that pearl composition is: get capsule 's content 3g, add acetone 20ml, supersound process 20 minutes, filter, 0.2g is got in the medicinal residues oven dry, puts in the peace bottle, add dilute hydrochloric acid test solution 5ml, seal, put in the baking oven, 105 ℃ were heated 20 hours, take out, supernatant is as need testing solution, and other gets Margarita control medicinal material 0.02g, shines medical material solution in pairs with legal system, test according to thin layer chromatography, draw above-mentioned two kinds of each 4ul of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with phenol-water 7:2, launch, take out, 105 ℃ were heated 5-10 minute, and sprayed immediately with 0.2% ethanol solution of ninhydrin, it is clear to developing the color to be heated to speckle at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists.
16, pearl capsule with twenty-five components quality determining method as claimed in claim 12 is characterized in that the discrimination method of Calculus Bovis composition is: get capsule 's content 8g, add methanol 30ml, supersound process 30 minutes filters, and filtrate is waved to 5ml, as need testing solution.Other gets cholic acid, the Hyodeoxycholic Acid reference substance is an amount of, makes the mixed solution that every 1ml contains 1mg with methanol, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds of each 10ul of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with normal hexane-ethyl acetate-acetic acid-methanol 20:25:2:3 upper solution, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, it is clear to be heated to speckle colour developing at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists.
17, pearl capsule with twenty-five components quality determining method as claimed in claim 12 is characterized in that the discrimination method of Radix Aucklandiae composition is: get capsule 's content 8g, add chloroform 30ml, supersound process 30 minutes, filter, filtrate is waved to 1ml, as need testing solution; Other removes hydrogen constuslactone reference substance, costunolide reference substance, adds chloroform and makes the mixed solution that every 1ml contains 0.5mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, be developing solvent with chloroform-cyclohexane extraction 5:1, launch, take out, dry, the vanillin sulfuric acid solution of spray 1%, it is clear to be heated to the speckle colour developing, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists.
18, pearl capsule with twenty-five components quality determining method as claimed in claim 12, it is characterized in that the discrimination method of Lignum Dalbergiae Odoriferae composition is: get capsule 's content 6g, 30ml adds diethyl ether, supersound process 30 minutes filters, and filtrate volatilizes, residue adds ethanol 1ml dissolving, as need testing solution; Other gets Lignum Dalbergiae Odoriferae control medicinal material 0.5g, shine medical material solution in pairs with legal system, draw need testing solution 10 μ l according to thin layer chromatography, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene-ether-chloroform 7:2:1 is developing solvent, launch, take out, dry, spray is with 1% vanillin sulfuric acid solution and dehydrated alcohol (1:9) mixed liquor, it is clear to be heated to speckle colour developing at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists.
19, pearl capsule with twenty-five components quality determining method as claimed in claim 12, the discrimination method that it is characterized in that the Fructus Piperis Longi composition is: get capsule 's content 5.0g, add dehydrated alcohol 30ml, supersound process 30 minutes filters, and filtrate is concentrated into 2ml, as need testing solution, it is an amount of that other gets the piperine reference substance, adds dehydrated alcohol and make the solution that every 1ml contains piperine 2mg, in contrast product solution, test according to thin layer chromatography, draw above-mentioned two kinds of solution, 10 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with benzene-ethyl acetate-acetone 7:2:1, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 105 ℃, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists.
20, pearl capsule with twenty-five components quality determining method as claimed in claim 12, the discrimination method that it is characterized in that the Cortex cinnamomi japonici (Ramulus Cinnamomi) composition is: get this product content 6g, 20ml adds diethyl ether, supersound process 30 minutes, filter, filtrate is waved to 2ml, and as need testing solution, it is an amount of that other gets the cinnamic aldehyde reference substance, add diethyl ether and make the reference substance solution that every 1ml contains cinnamic aldehyde 1 μ l, according to the thin layer chromatography test, draw need testing solution 5 μ l, reference substance solution 3 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (60-90 ℃)-ethyl acetate (9:1) is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, on test agent and the corresponding position of reference substance chromatograph, as showing the speckle of same color, then composition exists.
21, pearl capsule with twenty-five components quality determining method as claimed in claim 12, the discrimination method that it is characterized in that the Stigma Croci composition is: get this product content 3g, add methanol 20ml, supersound process 10 minutes, leave standstill and make clarification, get supernatant as need testing solution, other gets Stigma Croci control medicinal material 20mg, shines medical material solution in pairs with legal system, tests according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with ethyl acetate-methanol-water 100:16.5:13.5, launch, take out, dry, inspect under the daylight, on test agent and the corresponding position of reference substance chromatograph, as show the speckle of same color, then composition exists.
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| CN104360033B (en) * | 2014-11-12 | 2016-06-22 | 内蒙古天奇中蒙制药股份有限公司 | The method of inspection of NARU SANWEI WAN |
| CN104360033A (en) * | 2014-11-12 | 2015-02-18 | 内蒙古天奇中蒙制药股份有限公司 | Quality standard of Naru three-ingredient pills and detection method of quality standard |
| CN106841176A (en) * | 2017-02-13 | 2017-06-13 | 青海出入境检验检疫局检验检疫综合技术中心 | A kind of global quality control method of Ershiwuwei zhenzhu wan |
| CN107349295A (en) * | 2017-07-25 | 2017-11-17 | 江西中医药大学 | Tibetan medicine ten sweet dew pellet preparations and its preparation technology simply |
| CN107519148A (en) * | 2017-07-25 | 2017-12-29 | 江西中医药大学 | A kind of taste pearl micropill of Tibetan medicine 70 and its preparation technology |
| CN109085284A (en) * | 2018-08-28 | 2018-12-25 | 王智森 | A kind of quick thin-layer identification method of multiple medicine taste of Ershiwuwei zhenzhu wan |
| CN110441440A (en) * | 2019-09-20 | 2019-11-12 | 广东一方制药有限公司 | A kind of construction method and its discrimination method of Fructus Malvae Vertillatae medicinal material UPLC characteristic spectrum |
| CN110441440B (en) * | 2019-09-20 | 2022-03-29 | 广东一方制药有限公司 | Construction method and identification method of UPLC (unified Power level liquid chromatography) characteristic spectrum of cluster mallow fruit medicinal material |
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| CN101530590B (en) | 2011-09-07 |
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Address after: 750101 Telescope Development Zone, Yongning County, Yinchuan City, Ningxia Hui Autonomous Region Patentee after: Ningxia Zhouyang Pharmaceutical Co.,Ltd. Address before: 750101 Yongning Economic Development Zone, Yongning County, the Ningxia Hui Autonomous Region, Yinchuan Patentee before: NINGXIA DUOWEI PHARMACEUTICAL Co.,Ltd. |