CN101229248A - Quality standard and test method of hoove pill and preparation threrewith - Google Patents

Quality standard and test method of hoove pill and preparation threrewith Download PDF

Info

Publication number
CN101229248A
CN101229248A CNA2008100565035A CN200810056503A CN101229248A CN 101229248 A CN101229248 A CN 101229248A CN A2008100565035 A CNA2008100565035 A CN A2008100565035A CN 200810056503 A CN200810056503 A CN 200810056503A CN 101229248 A CN101229248 A CN 101229248A
Authority
CN
China
Prior art keywords
volume
parts
solution
ethyl acetate
ethanol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CNA2008100565035A
Other languages
Chinese (zh)
Other versions
CN101229248B (en
Inventor
陈致慜
李春雷
霍志金
李红梅
刘宇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HANDAN PHARMACEUTICAL CO., LTD.
Original Assignee
HANDAN PHARMACEUTICAL CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HANDAN PHARMACEUTICAL CO Ltd filed Critical HANDAN PHARMACEUTICAL CO Ltd
Priority to CN 200810056503 priority Critical patent/CN101229248B/en
Publication of CN101229248A publication Critical patent/CN101229248A/en
Application granted granted Critical
Publication of CN101229248B publication Critical patent/CN101229248B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Medicinal Preparation (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses an ascites pill and a quality control method for the preparation of the ascites pill, wherein the preparation is provided with a plurality of formulations by adding conventional accessories according to the ascites pill preparation formula in the second volume of traditional Chinese medicine set prescriptions preparations of Drug Standards of Ministry of Health of the People's Republic of China. The quality control method which comprises a content determination or content identification or one of the content determination and the content identification increases the thin layer identification of euphorbia Gansui Root, jujube oleanolic acid and elecampane based on the original quality standards, revises the thin layer identification of melanterite and builds the content determination for the green copperas (FeSO4 7H2O) and improves the controllability of the product quality.

Description

The quality standard of ascites pill and preparation thereof and detection method
Technical field
The present invention relates to a kind of method of quality control and detection method of drug combination preparation, the method for quality control and the detection method thereof of particularly swollen disease ball and preparation thereof.
Background technology
Ascites pill is second medicine that records of " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, is clinical Chinese patent medicine commonly used, is made up of five kinds of Chinese medicine such as Melanteritum (vinegar system), Radix Kansui, Fructus Jujubaes.Have the effect of inducing diuresis to remove edema, dehumidifying spleen invigorating, be mainly used in symptoms such as distension disease, distension and fullness of the chest and abdomen, extremity edema, constipation, oliguria with reddish urine.The ascites pill quality standard records in second in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, primary standard has only been recorded a chromogenic reaction and has been differentiated, and specificity is poor, and the detection index is few and do not have the assay index, can not effectively control product quality.
Summary of the invention
One object of the present invention is to disclose the method for quality control and the detection method thereof of swollen disease ball and preparation thereof.
The present invention seeks to be achieved through the following technical solutions:
The method of quality control of drug combination preparation of the present invention comprises one or more in following discriminating and/or the assay:
Differentiate: A. gets drug combination preparation 5～40 weight portions of the present invention, porphyrize, add methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 40～80 parts by volume, supersound process or hot reflux or merceration extracted 10～60 minutes, filter, the filtrate evaporate to dryness, residue adds water 20～40 parts by volume makes dissolving, with n-butyl alcohol, chloroform or ethyl acetate extraction three times, each solvent is 10～20 parts by volume, merge extractive liquid,, evaporate to dryness, residue adds methanol or ethanol 1 parts by volume makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 1～8 weight portion, add methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 30～50 parts by volume, supersound process or hot reflux or merceration extracted 10～60 minutes, filter, the filtrate evaporate to dryness, residue adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 1 parts by volume makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 0.005～0.02 parts by volume, control medicinal material solution 0.002～0.008 parts by volume, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: formic acid=5～40: 1～8: 0.1～8 solution is developing solvent, launch, take out, dry, put ultra-violet lamp and under 365nm, inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. get drug combination preparation 5～40 weight portions of the present invention, porphyrize adds petroleum ether, chloroform or ethyl acetate 40～80 parts by volume of methanol, ethanol, n-butyl alcohol, 60～90 ℃ of boiling ranges, flooded 20～80 minutes, hot reflux or supersound process 10～60 minutes discard solvent, and medicinal residues are flung to solvent, 40～60 parts by volume add diethyl ether, flooded 1～2 hour, hot reflux or supersound process 10～60 minutes filter, filtrate is concentrated into 1 parts by volume, as need testing solution; Other evens up pier fruit acid reference substance, adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate and makes the solution that per 1 parts by volume contains 0.001～0.003 weight portion, product solution in contrast; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 0.005～0.02 parts by volume, reference substance solution 0.002～0.008 parts by volume, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone: ethyl acetate=1～15: 1～8: 1～8 solution is developing solvent, launch, take out, dry, spray is with 5～15% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C. get drug combination preparation 5～40 weight portions of the present invention, porphyrize, the petroleum ether or chloroform 40～80 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration extracted 10～60 minutes, filter, petroleum ether or chloroform 1 parts by volume that filtrate evaporate to dryness, residue add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.2～5 weight portion, the petroleum ether or chloroform 5～15 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration 10～60 minutes, filter, the filtrate evaporate to dryness, petroleum ether or chloroform 1 parts by volume that medicinal residues add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 0.005～0.015 parts by volume of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone=5～12: 1～8 solution is developing solvent, launch, take out, dry, spray is with 5～15% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Assay:
The preparation of reference substance solution: ferrous sulfate reference substance 0.2～0.6 weight portion decided in accurate title, put in the 100ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 0.5-1.5 parts by volume and water 60-100 parts by volume makes dissolving to the 100ml measuring bottle, add water to scale, shake up, precision is measured 1～3 parts by volume, puts in the 100ml measuring bottle, adds water to scale, shake up, promptly getting concentration is the reference substance solution of ferrous 0.06～0.1 weight portion of sulfur acid in per 1 parts by volume;
The preparation of standard curve: precision is measured reference substance solution 1 parts by volume, 2 parts by volume, 4 parts by volume, 6 parts by volume, 8 parts by volume, put respectively in the 25ml measuring bottle, add water to 5～20 parts by volume, add 2 of 1～3% oxammonium hydrochloride. solution, 1 parts by volume and 0.1～0.3% again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 1～3% oxammonium hydrochloride. solution, 1 parts by volume and 0.1%～0.3%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance;
Algoscopy: get drug combination preparation of the present invention, porphyrize, accurate claim fixed 0.1～10 weight portion, put in the 250ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 2-3 parts by volume and water 80-120 parts by volume to the 250ml measuring bottle, supersound process adds water to scale to all molten diffusing, shakes up, filter, discard filtrate 15～30 parts by volume just, precision is measured subsequent filtrate 10～20 parts by volume, puts in the 100ml measuring bottle, add water to scale, shake up, precision is measured 3～8 parts by volume, puts in the 25ml measuring bottle, add water to 5～20 parts by volume, add 2 of 1～3% oxammonium hydrochloride. solution, 1 parts by volume and 0.1～0.3% again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing, add water to scale, shake up; Get 2 of 1～3% oxammonium hydrochloride. solution, 1 parts by volume and 0.1%～0.3%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; From the weight that standard curve is read ferrous sulfate the need testing solution, calculate, that is, drug combination preparation of the present invention per diem taking dose meter contains Melanteritum with ferrous sulfate FeSO47H 2The O meter must not be lower than 0.624 weight portion.
The method of quality control of drug combination preparation of the present invention is preferably as follows one or more in discriminating and/or the assay:
Differentiate: A. gets drug combination preparation 10～30 weight portions of the present invention, and porphyrize adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 60 parts by volume, supersound process or hot reflux or merceration extracted 20～60 minutes, filter, filtrate evaporate to dryness, residue add water 30 parts by volume makes dissolving, with n-butyl alcohol, chloroform or ethyl acetate extraction three times, each solvent is 20 parts by volume, merge extractive liquid,, evaporate to dryness, residue adds methanol or ethanol 1 parts by volume makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 1～5 weight portion, add methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 40 parts by volume, supersound process or hot reflux or merceration extracted 20～60 minutes, filter, the filtrate evaporate to dryness, residue adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 1 parts by volume makes dissolving, in contrast medical material solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 0.01 parts by volume, control medicinal material solution 0.005 parts by volume, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: formic acid=10～30: 1～5: 0.1～5 solution is developing solvent, launch, take out, dry, put ultra-violet lamp and under 365nm, inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. get drug combination preparation 10～30 weight portions of the present invention, porphyrize, the petroleum ether, chloroform or ethyl acetate 50 parts by volume that add methanol, ethanol, n-butyl alcohol, 60～90 ℃ of boiling ranges, flooded 30～60 minutes, hot reflux or frequency are 250W 40KHz supersound process 20～60 minutes, discard solvent, medicinal residues are flung to solvent, 50 parts by volume add diethyl ether, flooded 1 hour, hot reflux or frequency are 250W 40KHz supersound process 20～60 minutes, filter, filtrate is concentrated into 1 parts by volume, as need testing solution; Other evens up pier fruit acid reference substance, adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate and makes the solution that per 1 parts by volume contains 0.001 weight portion, product solution in contrast; Test according to an appendix VI of Chinese Pharmacopoeia 2B005 version B thin layer chromatography, draw need testing solution 0.010 parts by volume, reference substance solution 0.005 parts by volume, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone: ethyl acetate=1～10: 1～5: 1～5 solution 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; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C. get drug combination preparation 10～30 weight portions of the present invention, porphyrize, the petroleum ether or chloroform 50 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration extracted 20～60 minutes, filter, petroleum ether or chloroform 1 parts by volume that filtrate evaporate to dryness, residue add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.5～3 weight portion, the petroleum ether or chloroform 10 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration 30～90 minutes, filter, the filtrate evaporate to dryness, petroleum ether or chloroform 1 parts by volume that medicinal residues add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 0.01 parts by volume of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone=6～10: 1～5 solution is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Assay:
The preparation of reference substance solution: get ferrous sulfate reference substance 0.4 weight portion, accurate claim surely, put in the 100ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 1 parts by volume and water 80 parts by volume and to the 100ml measuring bottle, make dissolving, add water to scale, shake up, precision is measured 2 parts by volume, put in the 100ml measuring bottle, add water to scale, shake up, promptly getting concentration is the reference substance solution of ferrous 0.08 weight portion of sulfur acid in per 1 parts by volume;
The preparation of standard curve: precision is measured reference substance solution 1 parts by volume, 2 parts by volume, 4 parts by volume, 6 parts by volume, 8 parts by volume, put respectively in the 25ml measuring bottle, add water to 10 parts by volume, add 1% oxammonium hydrochloride. solution, 1 parts by volume and 0.2%2 again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 1% oxammonium hydrochloride. solution, 1 parts by volume and 0.2%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance;
Algoscopy: get drug combination preparation of the present invention, porphyrize is got 0.1～10 weight portion, and accurate the title decides, put in the 250ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 2.5 parts by volume and water 100 parts by volume to the 250ml measuring bottle, frequency is a 250W 40KHz supersound process to whole molten loosing, add water to scale, shake up, filter, discard subsequent filtrate 20 parts by volume, precision is measured subsequent filtrate 10 parts by volume, put in the 100ml measuring bottle, add water to scale, shake up, precision is measured 5 parts by volume, put in the 25ml measuring bottle, add water to 10 parts by volume, add 1% oxammonium hydrochloride. solution, 1 parts by volume and 0.2%2 again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 1% oxammonium hydrochloride. solution, 1 parts by volume and 0.2%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; From the weight that standard curve is read ferrous sulfate the need testing solution, calculate, that is, drug combination preparation of the present invention per diem taking dose meter contains Melanteritum in ferrous sulfate FeSO47H2O, must not be lower than 0.624 weight portion.
The method of quality control of drug combination preparation of the present invention is preferably as follows one or more in discriminating and/or the assay:
Differentiate: A. gets drug combination preparation 20 weight portions of the present invention, and porphyrize adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 60 parts by volume, supersound process or hot reflux or merceration extracted 40 minutes, filter, filtrate evaporate to dryness, residue add water 30 parts by volume makes dissolving, with n-butyl alcohol, chloroform or ethyl acetate extraction three times, each solvent is 15 parts by volume, merge extractive liquid,, evaporate to dryness, residue adds methanol or ethanol 1 parts by volume makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 3 weight portions, add methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 40 parts by volume, supersound process or hot reflux or merceration extracted 40 minutes, filter, the filtrate evaporate to dryness, residue adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 1 parts by volume makes dissolving, in contrast medical material solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 0.01 parts by volume, control medicinal material solution 0.005 parts by volume, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: the solution of formic acid=15: 3: 3 is developing solvent, launch, take out, dry, put ultra-violet lamp and under 365nm, inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. get drug combination preparation 20 weight portions of the present invention, porphyrize adds petroleum ether, chloroform or ethyl acetate 50 parts by volume of methanol, ethanol, n-butyl alcohol, 60～90 ℃ of boiling ranges, flooded 45 minutes, hot reflux or frequency are 250W 40KHz supersound process 40 minutes, discard solvent, and medicinal residues are flung to solvent, 50 parts by volume add diethyl ether, flooded 1 hour, hot reflux or frequency are 250W 40KHz supersound process 40 minutes, filter, filtrate is concentrated into 1 parts by volume, as need testing solution; Other evens up pier fruit acid reference substance, adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate and makes the solution that per 1 parts by volume contains 0.001 weight portion, product solution in contrast; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 0.010 parts by volume, reference substance solution 0.005 parts by volume, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone: the solution of ethyl acetate=5: 3: 3 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; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C. get drug combination preparation 20 weight portions of the present invention, porphyrize, the petroleum ether or chloroform 50 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration extracted 40 minutes, filter, petroleum ether or chloroform 1 parts by volume that filtrate evaporate to dryness, residue add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 2 weight portions, the petroleum ether or chloroform 10 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration 40 minutes, filter, the filtrate evaporate to dryness, petroleum ether or chloroform 1 parts by volume that medicinal residues add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, in contrast medical material solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw each 0.01 parts by volume of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: the solution of acetone=8: 3 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Assay:
The preparation of reference substance solution: get ferrous sulfate reference substance 0.5 weight portion, accurate claim surely, put in the 100ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 1 parts by volume and water 80 parts by volume and to the 100ml measuring bottle, make dissolving, add water to scale, shake up, precision is measured 2 parts by volume, put in the 100ml measuring bottle, add water to scale, shake up, promptly getting concentration is the reference substance solution of ferrous 0.08 weight portion of sulfur acid in per 1 parts by volume;
The preparation of standard curve: precision is measured reference substance solution 1 parts by volume, 2 parts by volume, 4 parts by volume, 6 parts by volume, 8 parts by volume, put respectively in the 25ml measuring bottle, add water to 18 parts by volume, add 2% oxammonium hydrochloride. solution, 1 parts by volume and 0.25%2 again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 2% oxammonium hydrochloride. solution, 1 parts by volume and 0.25%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance;
Algoscopy: get drug combination preparation of the present invention, porphyrize is got 4 weight portions, and accurate the title decides, put in the 250ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 2.5 parts by volume and water 100 parts by volume to the 100ml measuring bottle, frequency is a 250W 40KHz supersound process to whole molten loosing, add water to scale, shake up, filter, discard subsequent filtrate 25 parts by volume, precision is measured subsequent filtrate 6 parts by volume, put in the 100ml measuring bottle, add water to scale, shake up, precision is measured 7 parts by volume, put in the 25ml measuring bottle, add water to 15 parts by volume, add 2% oxammonium hydrochloride. solution, 1 parts by volume and 0.25%2 again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 2% oxammonium hydrochloride. solution, 1 parts by volume and 0.25%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; From the weight that standard curve is read ferrous sulfate the need testing solution, calculate, that is, drug combination preparation of the present invention per diem taking dose meter contains Melanteritum with ferrous sulfate FeSO47H 2The O meter must not be lower than 0.624 weight portion.
Wherein, drug combination preparation of the present invention is by the prescription of the ascites pill preparation described in second in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, adds tablet, capsule, powder, soft capsule, drop pill, honeyed pill, pill, granule, soft extract with bee honey agent, slow releasing preparation, quick releasing formulation, controlled release preparation, oral liquid or the ejection preparation that conventional adjuvant is made according to conventional method.
The ratio of weight portion of the present invention and parts by volume is a grams per milliliter.Pharmaceutical composition method of quality control of the present invention can be applied to the various dosage forms of compositions, as clinical acceptable forms such as tablet, capsule, oral liquid, drop pill, spray, granules, because the wherein contained suitable crude drug amount of preparation of different dosage form is identical, therefore each dosage form is when carrying out quality control, selected sample size can be unified conversion and be suitable crude drug amount, this method of quality control is the per unit preparation with suitable crude drug amount 3.9g, and the per unit preparation can be every, every, every or every ball etc.
Description of drawings:
Fig. 1: reference substance scintigram
Fig. 2: sample scintigram
Fig. 3: negative scintigram
Technical problem to be solved by this invention is to improve the initial quality standard, the controllability of improving the quality of products. The thin layer that has increased oleanolic acid, the banksia rose in the root of gansui, the date on the basis of initial quality standard is differentiated, the thin layer of melanterite is differentiated revised, and set up ferrous sulfate (FeSO in the melanterite4·7H 2O) assay. By quality control of the present invention, improved product stability, be conducive to the quality control of suitability for industrialized production.
Following experimental example and embodiment are used for further specifying but are not limited to the present invention.
Experimental example 1 ultraviolet chromatographic condition
The selection ferrous sulfate of A, absorbing wavelength has the absorption maximum degree at the 522nm place, and the negative control product are noiseless at the 522nm place, see Fig. 1,2,3.
The selection of B, Pretreatment drug combination preparation pre-treating method of the present invention contains quantifier with reference to the FUFANG ZAOFAN WAN in Chinese Pharmacopoeia 2005 version (an one). Also tested the content determination of the Chinese Pharmacopoeia middle ferrous sulfate of version (two ones) in 2005, because the filtrate after the drug combination preparation dissolving of the present invention takes on a red color, with can't distinguish with the fixed terminal colour pink of permanganate titration drop, color becomes blackish green after namely using active carbon filtration, also can't accurately distinguish, so the method can not be used.
Should note when this method operates: the ferrous sulfate reference substance solution must be prepared before use, even and this solution can not preserve refrigeration condition under.
Experimental example 2 veracity and precisions are measured
A, the degree of accuracy: precision takes by weighing 9 parts in the sample of 0.375g, and the ferrous sulfate reference substance that adds respectively (3 dosage add with the solution form, and addition sees Table 1) is measured by content assaying method of the present invention. The results are shown in Table 1.
Table 1 average recovery result of the test
Test sample sampling amount (g) Ferrous sulfate content (mg) in the test sample Reference substance addition (mg) The amount of recording (mg) The rate of recovery (%) Average recovery rate (%)   RSD(％)
  0.2598   0.2531   0.2522   0.2566   0.2583   0.2541   0.2533   0.2567   0.2519   97.4   94.9   94.6   96.2   96.9   95.3   95.0   96.3   94.5   40.5   40.5   40.5   81   81   81   121.5   121.5   121.5   138.0   136.2   135.6   177.0   176.5   177.5   219.5   217.5   217.5   100.2   102.0   101.2   99.8   98.3   101.5   102.5   99.8   101.2           100.7           1.31
The result shows: recording its average recovery rate is 100.7%, RSD=1.31% (n=9).
B, precision:
Replica test: the sample content assaying method in accordance with regulations to same lot number carries out 9 (3 dosage) parallel determinations, calculates content, the results are shown in Table 2.
Table 2 replica test result
Test sample sampling amount (g) Measurement result (g/g) Mean value (g/g)   RSD(％)
    0.5319       0.5024       0.5166   0.363   0.367   0.365   0.362   0.364   0.363   0.366   0.363   0.364           0.364           0.44
Mean value is 0.364g/g, and RSD=0.44% (n=9) shows the method repeatability better.
C, instrument precision
Get reference substance solution 4ml, after the colour developing, 5 traps of METHOD FOR CONTINUOUS DETERMINATION the results are shown in Table 3.
Table 3 instrument precision result of the test
Trap     0.5048   0.5047   0.5047     0.5048     0.5049
Mean value RSD (%)   0.5048   0.017
Mean value is 0.5048, RSD=0.017% (n=5), shows that instrument precision is good.
Experimental example 3 linear relationships
Get reference substance solution (81.4 μ g/ml) 1ml, 2ml, 4ml, 6ml, 8ml, after the colour developing, the 522nm place measures absorbance, take reference substance concentration (x) as abscissa, trap (y) is ordinate, the drawing standard curve, and calculate regression equation: y=0.03836x+0.00376, r=0.99996. The results are shown in Table 4.
The linear result that investigates of table 4
Sampling amount (ml)     1     2     4     6     8
Concentration (μ g/ml)    3.256   6.512   13.024   19.536   26.048
Trap    0.1274   0.2527   0.5048   0.7575   0.9995
Regression equation     y＝0.03836x+0.00376
r     0.99996
Show that ferrous sulfate has good linear relationship with trap in 3～26 μ g/ml scopes.
Experimental example 4 specificities
Lack the analog sample of melanterite according to the prescription of drug combination preparation of the present invention, method for making preparation, make the melanterite negative control solution by the preparation method of need testing solution. With ferrous sulfate reference substance solution, need testing solution and melanterite negative control solution, between 400～650nm, scan result such as accompanying drawing 1,2,3. Scintigram shows that ferrous sulfate reference substance solution and need testing solution have absorption maximum at the 522nm place, and the figure spectral shape is basically identical, shows that it is rational measuring absorbance with the wavelength of 522nm; Without absorption maximum, and the figure spectral shape substantially linearly, illustrates that other flavour of a drug do not disturb the check of melanterite in the relevant position for the melanterite negative control solution.
Experimental example 5 scopes are measured
The trap of sample is investigated it ± 50% scope, i.e. precision, accuracy and the linearity of trap between 0.3～0.9 greatly about about 0.6 in the test again.Again because when the drawing standard curve, the trap scope of variable concentrations reference substance is between 0.1～1.0, and precision, accuracy and linearity in this is interval all meet the requirements, so precision, accuracy and linearity also meet the requirements in 0.3～0.9 interval.Therefore the scope of this method of testing requirement meets the requirements.
Experimental example 6 ruggedness
Get reference substance solution 6ml, after the colour developing, with 0,1,2,3,4,6,8,12, the time interval determination trap of 24h, the results are shown in Table 5.
Table 5 solution stability testing result
At interval/h 0 1 2 3 4 6 8 12 24
Trap meansigma methods RSD 0.761 0.763 0.762 0.762 0.760 0.760 0.28％ 0.761 0.760 0.757 0.757
RSD=0.28% (n=9) shows that ferrous sulfate is stable in the 24h after colour developing at least.
Experimental example 7 content limits are formulated
Measure the sample of different lot numbers, totally 12 batches, 22 groups of data (seeing Table 6), and the randomization content detection of raw material Melanteritum (seeing Table 7).Following data are used for the foundation that content limit is formulated.
Ferrous sulfate content (g/g) in table 6 sample
Lot number 040301 040302 040303 050901
Content 0.207 0.208 0.216 0.215 0.220 0.220 0.256 0.255
Lot number 050902 050903 051101 051102
Content 0.262 0.262 0.255 0.256 0.228 0.230 0.234 0.234
Lot number 051103 051104 060501 060502
Content 0.237 0.239 0.251 0.248 0.252 0.251 0.257 0.257
Ferrous sulfate content (%) in the table 7 raw material Melanteritum
Numbering 1 2 3 45
Content 94.7 90.1 93.9 92.492.7
The sample limiting figure is 0.207～0.262g/g, and the Melanteritum limiting figure is 90.1～94.7%.According to above-mentioned data actual transfer rate scope is 62.0～74.7%.Raw material Melanteritum master contains water containing ferrous sulfate (FeSO 47H 2O), very easily rotten, exposing in the air is air slaking, becomes anhydrous slufuric acid ferrum; Oxidation generates ferric subsulfate rapidly in humid air.So Melanteritum is perishable in the process of storage, vinegar system.Because the unstability of raw material, so the fluctuation of the content of finished product is bigger.According to the minimum value downward modulation 20% of being surveyed, the gained data are made as content lower limit, i.e. 0.160g/g.
Following embodiment all can realize the effect of above-mentioned experimental example.
The specific embodiment
Embodiment 1: the discrimination method of pharmaceutical composition pill of the present invention and content assaying method
Differentiate: A. gets pharmaceutical composition pill 8g of the present invention, and porphyrize adds methanol 70ml, supersound process 20 minutes, filter, filtrate evaporate to dryness, residue add water 35ml makes dissolving, with n-butanol extraction three times, each solvent is 15ml, merge extractive liquid,, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 7g, adds methanol 35ml, and supersound process 50 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 0.006ml, control medicinal material solution 0.005ml, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: the solution of formic acid=6: 2: 0.2 is developing solvent, launch, take out, dry, put ultra-violet lamp and under 365nm, inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. get pharmaceutical composition pill 35g of the present invention, porphyrize adds ethanol 45ml, floods 50 minutes, and hot reflux 40 minutes discards solvent, and medicinal residues are flung to solvent, and the 55ml that adds diethyl ether flooded 1 hour, and hot reflux 30 minutes filters, and filtrate is concentrated into 1ml, as need testing solution; Other evens up pier fruit acid reference substance, adds chloroform and makes the solution that every 1ml contains 0.0015g, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 0.02ml, reference substance solution 0.003ml, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone: the solution of ethyl acetate=14: 6: 6 is developing solvent, launch, take out, dry, spray is with 6% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C. get pharmaceutical composition pill 8g of the present invention, porphyrize, the 70ml that adds diethyl ether, supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 4g, adds ethyl acetate 8ml, and supersound process 40 minutes filters, and filtrate evaporate to dryness, medicinal residues add n-butyl alcohol makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned two kinds of each 8ml of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: the solution of acetone=6: 2 is developing solvent, launch, take out, dry, spray is with 12% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Assay:
The preparation of reference substance solution: get ferrous sulfate reference substance 0.3g, accurate claim surely, put in the 100ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 1 parts by volume and water 80 parts by volume and to the 100ml measuring bottle, make dissolving, add water to scale, shake up, precision is measured 1～3ml, put in the 100ml measuring bottle, add water to scale, shake up, promptly get the reference substance solution that concentration is the ferrous 0.09g of sulfur acid among every 1ml;
The preparation of standard curve: precision is measured 5 parts of reference substance solution, and liquor capacity is 5ml, puts respectively in the 25ml measuring bottle, adds water to 6ml, adds 2% oxammonium hydrochloride. solution 1ml and 0.1%2 again, 2-bipyridyl alcoholic solution 1ml, and mixing adds water to scale, shakes up; Get 2% oxammonium hydrochloride. solution 1ml and 0.1%2,2-bipyridyl alcoholic solution 1ml, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance;
Algoscopy: get pharmaceutical composition pill of the present invention, porphyrize, 7g decided in accurate title, put in the 250ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 2.5 parts by volume and water 100 parts by volume to the 250ml measuring bottle, frequency is that 250W 40KHz supersound process is extremely all molten diffusing, adds water to scale, shakes up, filter, discard filtrate 16ml just, precision is measured subsequent filtrate 19ml, puts in the 100ml measuring bottle, add water to scale, shake up, precision is measured 4ml, puts in the 25ml measuring bottle, add water to 6ml, add 2% oxammonium hydrochloride. solution 1ml and 0.1%2 again, 2-bipyridyl alcoholic solution 1ml, mixing, add water to scale, shake up; Get 2% oxammonium hydrochloride. solution 1ml and 0.1%2,2-bipyridyl alcoholic solution 1ml, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; From the weight that standard curve is read ferrous sulfate the need testing solution, calculate, that is, pharmaceutical composition pill of the present invention per diem taking dose meter contains Melanteritum in ferrous sulfate FeSO47H2O, must not be lower than 0.624 weight portion.
Embodiment 2: the discrimination method of pharmaceutical composition tablet of the present invention and content assaying method
A. get pharmaceutical composition tablet 20g of the present invention, porphyrize adds ethyl acetate 60ml, hot reflux was extracted 40 minutes, filter, filtrate evaporate to dryness, residue add water 30ml makes dissolving, with ethyl acetate extraction three times, each solvent is 20ml, merge extractive liquid,, evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 3g, adds ethyl acetate 40ml, and hot reflux was extracted 40 minutes, filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 0.01ml, control medicinal material solution 0.005ml, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: the solution of formic acid=15: 3: 3 is developing solvent, launch, take out, dry, put ultra-violet lamp and under 365nm, inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. get pharmaceutical composition tablet 20g of the present invention, porphyrize adds ethyl acetate 50ml, flooded 45 minutes, frequency is 250W 40KHz supersound process 40 minutes, discards solvent, and medicinal residues are flung to solvent, 50ml adds diethyl ether, flooded 1 hour, frequency is 250W 40KHz supersound process 40 minutes, filters, filtrate is concentrated into 1ml, as need testing solution; Other evens up pier fruit acid reference substance, adds ethyl acetate and makes the solution that every 1ml contains 0.001g, in contrast product solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 0.01ml, reference substance solution 0.005ml, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone: the solution of ethyl acetate=5: 3: 3 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; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
Assay:
The preparation of reference substance solution: get ferrous sulfate reference substance 0.4g, accurate claim surely, put in the 100ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 1 parts by volume and water 80 parts by volume and to the 100ml measuring bottle, make dissolving, add water to scale, shake up, precision is measured 2ml, put in the 100ml measuring bottle, add water to scale, shake up, promptly get the reference substance solution that concentration is the ferrous 0.08g of sulfur acid among every 1ml;
The preparation of standard curve: precision is measured reference substance solution 1ml, 2ml, 4ml, 6ml, 8ml, puts respectively in the 25ml measuring bottle, adds water to 10ml, adds 1% oxammonium hydrochloride. solution 1ml and 0.2%2 again, 2-bipyridyl alcoholic solution 1ml, and mixing adds water to scale, shakes up; Get 2% oxammonium hydrochloride. solution 1ml and 0.1%2,2-bipyridyl alcoholic solution 1ml, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance;
Algoscopy: get pharmaceutical composition tablet of the present invention, porphyrize is got 0.5g, accurate claim surely, put in the 250ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 2.5 parts by volume and water 100 parts by volume to the 250ml measuring bottle, frequency is that 250W 40KHz supersound process is extremely all molten diffusing, adds water to scale, shake up, filter, discard the about 20ml of filtrate just, precision is measured subsequent filtrate 12ml, put in the 100ml measuring bottle, add water to scale, shake up, precision is measured 5ml, put in the 25ml measuring bottle, add water to 10ml, add 1% oxammonium hydrochloride. solution 1ml and 0.2%2 again, 2-bipyridyl alcoholic solution 1ml, mixing adds water to scale, shakes up; Get 1% oxammonium hydrochloride. solution 1ml and 0.2%2,2-bipyridyl alcoholic solution 1ml, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, wavelength place at 522nm measures absorbance, with the absorbance is that vertical coordinate, concentration are abscissa drawing standard curve, the weight of reading ferrous sulfate the need testing solution from standard curve, calculate, that is, pharmaceutical composition tablet of the present invention per diem taking dose meter contains Melanteritum in ferrous sulfate FeSO47H2O, must not be lower than 0.624 weight portion.
Embodiment 3: the discrimination method of drug composition oral liquid formulation of the present invention:
Get drug composition oral liquid formulation 25ml of the present invention, add the petroleum ether 50ml of 60～90 ℃ of boiling ranges, merceration extracted 40 minutes, filtered, and filtrate evaporate to dryness, residue add n-butyl alcohol 1ml makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 3g, adds methanol 10ml, and merceration 40 minutes filters, and filtrate evaporate to dryness, medicinal residues add ethanol 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw above-mentioned two kinds of each 0.01ml of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: the solution of acetone=9: 2 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiment 4: the content assaying method of medicament composition granule agent of the present invention
The preparation of reference substance solution: ferrous sulfate reference substance 0.3g decided in accurate title, put in the 100ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 1 parts by volume and water 80 parts by volume and to the 100ml measuring bottle, make dissolving, add water to scale, shake up, precision is measured 2ml, puts in the 100ml measuring bottle, adds water to scale, shake up, promptly get the reference substance solution that concentration is the ferrous 0.08g of sulfur acid among every 1ml;
The preparation of standard curve: precision is measured reference substance solution 1ml, 2ml, 4ml, 6ml, 8ml, puts respectively in the 25ml measuring bottle, adds water to 12ml, add 2 of 2% oxammonium hydrochloride. solution 1ml and 0.2% again, 2-bipyridyl alcoholic solution 1ml, mixing, add water to scale, shake up; Get 2% oxammonium hydrochloride. solution 1ml and 0.2%2,2-bipyridyl alcoholic solution 1ml, mixing adds water to 25 ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance;
Algoscopy: get medicament composition granule agent of the present invention, porphyrize, 5g decided in accurate title, put in the 250ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 2.5 parts by volume and water 100 parts by volume to the 250ml measuring bottle, supersound process adds water to scale to all molten diffusing, shakes up, filter, discard filtrate 25ml just, precision is measured subsequent filtrate 10ml, puts in the 100ml measuring bottle, add water to scale, shake up, precision is measured 6ml, puts in the 25ml measuring bottle, add water to 12ml, add 2 of 2% oxammonium hydrochloride. solution 1ml and 0.2% again, 2-bipyridyl alcoholic solution 1ml, mixing, add water to scale, shake up; Get 2% oxammonium hydrochloride. solution 1ml and 0.2%2,2-bipyridyl alcoholic solution 1ml, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; From the weight that standard curve is read ferrous sulfate the need testing solution, calculate, that is, medicament composition granule agent of the present invention per diem taking dose meter contains Melanteritum in ferrous sulfate FeSO47H2O, must not be lower than 0.624 weight portion.
Embodiment 5: the discrimination method of medicament composition capsule preparation of the present invention:
A. get medicament composition capsule preparation content 25g of the present invention, porphyrize adds ethyl acetate 70ml, merceration extracted 50 minutes, filter, filtrate evaporate to dryness, residue add water 30ml makes dissolving, with chloroform extraction three times, each solvent is 15ml, merge extractive liquid,, evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 6g, adds n-butyl alcohol 40ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 0.01ml, control medicinal material solution 0.005ml, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: the solution of formic acid=35: 6: 4 is developing solvent, launch, take out, dry, put ultra-violet lamp and under 365nm, inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. get medicament composition capsule preparation content 10g of the present invention, porphyrize adds the petroleum ether 50ml of 60～90 ℃ of boiling ranges, flooded 70 minutes, hot reflux 20 minutes discards solvent, and medicinal residues are flung to solvent, 60ml adds diethyl ether, flooded 1 hour, hot reflux or frequency are 250W 40KHz supersound process 40 minutes, filter, filtrate is concentrated into 1ml, as need testing solution; Other evens up pier fruit acid reference substance, adds methanol and makes the solution that every 1ml contains 0.001g, in contrast product solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 0.010ml, reference substance solution 0.005ml, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone: the solution of ethyl acetate=12: 2: 7 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; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C. get medicament composition capsule preparation content 30g of the present invention, porphyrize adds chloroform 50ml, and hot reflux 40 minutes filters, and filtrate evaporate to dryness, the residue 1ml that adds diethyl ether makes dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 4g, adds ethyl acetate 12ml, and supersound process 30 minutes filters, and filtrate evaporate to dryness, medicinal residues add ethanol 1ml makes dissolving, in contrast medical material solution; According to the test of an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw above-mentioned two kinds of each 8ml of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: the solution of acetone=6: 7 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

Claims (3)

1. the method for quality control of a drug combination preparation is characterized in that this method comprises one or more in following discriminating and/or the content:
Differentiate: A. compositions preparation 5～40 weight portions of getting it filled, porphyrize adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 40～80 parts by volume, supersound process or hot reflux or merceration extracted 10～60 minutes, filter, filtrate evaporate to dryness, residue add water 20～40 parts by volume makes dissolving, with n-butyl alcohol, chloroform or ethyl acetate extraction three times, each solvent is 10～20 parts by volume, merge extractive liquid,, evaporate to dryness, residue adds methanol or ethanol 1 parts by volume makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 1～8 weight portion, add methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 30～50 parts by volume, supersound process or hot reflux or merceration extracted 10～60 minutes, filter, the filtrate evaporate to dryness, residue adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 1 parts by volume makes dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 0.005～0.02 parts by volume, control medicinal material solution 0.002～0.008 parts by volume, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: formic acid=5～40: 1～8: 0.1～8 solution is developing solvent, launch, take out, dry, put ultra-violet lamp and under 365nm, inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. compositions preparation 5～40 weight portions of getting it filled, porphyrize adds petroleum ether, chloroform or ethyl acetate 40～80 parts by volume of methanol, ethanol, n-butyl alcohol, 60～90 ℃ of boiling ranges, flooded 20～80 minutes, hot reflux or supersound process 10～60 minutes discard solvent, and medicinal residues are flung to solvent, 40～60 parts by volume add diethyl ether, flooded 1～2 hour, hot reflux or supersound process 10～60 minutes filter, filtrate is concentrated into 1 parts by volume, as need testing solution; Other evens up pier fruit acid reference substance, adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate and makes the solution that per 1 parts by volume contains 0.001～0.003 weight portion, product solution in contrast; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw need testing solution 0.005～0.02 parts by volume, reference substance solution 0.002～0.008 parts by volume, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone: ethyl acetate=1～15: 1～8: 1～8 solution is developing solvent, launch, take out, dry, spray is with 5～15% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C. compositions preparation 5～40 weight portions of getting it filled, porphyrize, the petroleum ether or chloroform 40～80 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration extracted 10～60 minutes, filter, petroleum ether or chloroform 1 parts by volume that filtrate evaporate to dryness, residue add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.2～5 weight portion, the petroleum ether or chloroform 5～15 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration 10～60 minutes, filter, the filtrate evaporate to dryness, petroleum ether or chloroform 1 parts by volume that medicinal residues add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, in contrast medical material solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw each 0.005～0.015 parts by volume of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone=5～12: 1～8 solution is developing solvent, launch, take out, dry, spray is with 5～15% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Assay:
The preparation of reference substance solution: ferrous sulfate reference substance 0.2～0.6 weight portion decided in accurate title, put in the 100ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 0.5-1.5 parts by volume and water 60-100 parts by volume makes dissolving to the 100ml measuring bottle, add water to scale, shake up, precision is measured 1～3 parts by volume, puts in the 100ml measuring bottle, adds water to scale, shake up, promptly getting concentration is the reference substance solution of ferrous 0.06～0.1 weight portion of sulfur acid in per 1 parts by volume; The preparation of standard curve: precision is measured reference substance solution 1 parts by volume, 2 parts by volume, 4 parts by volume, 6 parts by volume, 8 parts by volume, put respectively in the 25ml measuring bottle, add water to 5～20 parts by volume, add 2 of 1～3% oxammonium hydrochloride. solution, 1 parts by volume and 0.1～0.3% again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 1～3% oxammonium hydrochloride. solution, 1 parts by volume and 0.1%～0.3%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; Algoscopy: the compositions preparation of getting it filled, porphyrize, accurate claim fixed 0.1～10 weight portion, put in the 250ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 2-3 parts by volume and water 80-120 parts by volume to the 250ml measuring bottle, supersound process adds water to scale to all molten diffusing, shakes up, filter, discard filtrate 15～30 parts by volume just, precision is measured subsequent filtrate 10～20 parts by volume, puts in the 100ml measuring bottle, add water to scale, shake up, precision is measured 3～8 parts by volume, puts in the 25ml measuring bottle, add water to 5～20 parts by volume, add 2 of 1～3% oxammonium hydrochloride. solution, 1 parts by volume and 0.1～0.3% again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing, add water to scale, shake up; Get 2 of 1～3% oxammonium hydrochloride. solution, 1 parts by volume and 0.1%～0.3%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; From the weight that standard curve is read ferrous sulfate the need testing solution, calculate, that is, drug combination preparation per diem taking dose meter contains Melanteritum with ferrous sulfate FeSO 47H 2The O meter must not be lower than 0.624 weight portion;
Wherein said drug combination preparation is by the prescription of the ascites pill preparation described in second in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, adds tablet, capsule, powder, soft capsule, drop pill, honeyed pill, pill, granule, soft extract with bee honey agent, slow releasing preparation, quick releasing formulation, controlled release preparation, oral liquid or the ejection preparation that conventional adjuvant is made according to conventional method.
2. method of quality control as claimed in claim 1 is characterized in that this method comprises one or more in following discriminating and/or the content:
Differentiate: A. compositions preparation 10～30 weight portions of getting it filled, porphyrize adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 60 parts by volume, supersound process or hot reflux or merceration extracted 20～60 minutes, filter, filtrate evaporate to dryness, residue add water 30 parts by volume makes dissolving, with n-butyl alcohol, chloroform or ethyl acetate extraction three times, each solvent is 20 parts by volume, merge extractive liquid,, evaporate to dryness, residue adds methanol or ethanol 1 parts by volume makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 1～5 weight portion, add methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 40 parts by volume, supersound process or hot reflux or merceration extracted 20～60 minutes, filter, the filtrate evaporate to dryness, residue adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 1 parts by volume makes dissolving, in contrast medical material solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 0.01 parts by volume, control medicinal material solution 0.005 parts by volume, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: formic acid=10～30: 1～5: 0.1～5 solution is developing solvent, launch, take out, dry, put ultra-violet lamp and under 365nm, inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. compositions preparation 10～30 weight portions of getting it filled, porphyrize adds petroleum ether, chloroform or ethyl acetate 50 parts by volume of methanol, ethanol, n-butyl alcohol, 60～90 ℃ of boiling ranges, flooded 30～60 minutes, hot reflux or frequency are 250W40KHz supersound process 20～60 minutes, discard solvent, and medicinal residues are flung to solvent, 50 parts by volume add diethyl ether, flooded 1 hour, hot reflux or frequency are 250W 40KHz supersound process 20～60 minutes, filter, filtrate is concentrated into 1 parts by volume, as need testing solution; Other evens up pier fruit acid reference substance, adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate and makes the solution that per 1 parts by volume contains 0.001 weight portion, product solution in contrast; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 0.010 parts by volume, reference substance solution 0.005 parts by volume, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone: ethyl acetate=1～10: 1～5: 1～5 solution 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; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C. compositions preparation 10～30 weight portions of getting it filled, porphyrize, the petroleum ether or chloroform 50 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration extracted 20～60 minutes, filter, petroleum ether or chloroform 1 parts by volume that filtrate evaporate to dryness, residue add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 0.5～3 weight portion, the petroleum ether or chloroform 10 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration 30～90 minutes, filter, the filtrate evaporate to dryness, petroleum ether or chloroform 1 parts by volume that medicinal residues add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 0.01 parts by volume of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone=6～10: 1～5 solution is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Assay:
The preparation of reference substance solution: get ferrous sulfate reference substance 0.4 weight portion, accurate claim surely, put in the 100ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 1 parts by volume and water 80 parts by volume and to the 100ml measuring bottle, make dissolving, add water to scale, shake up, precision is measured 2 parts by volume, put in the 100ml measuring bottle, add water to scale, shake up, promptly getting concentration is the reference substance solution of ferrous 0.08 weight portion of sulfur acid in per 1 parts by volume; The preparation of standard curve: precision is measured reference substance solution 1 parts by volume, 2 parts by volume, 4 parts by volume, 6 parts by volume, 8 parts by volume, put respectively in the 25ml measuring bottle, add water to 10 parts by volume, add 1% oxammonium hydrochloride. solution, 1 parts by volume and 0.2%2 again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 1% oxammonium hydrochloride. solution, 1 parts by volume and 0.2%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix VA of Chinese Pharmacopoeia version in 2005 ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; Algoscopy: the compositions preparation of getting it filled, porphyrize is got 0.1～10 weight portion, and accurate the title decides, put in the 250ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 2.5 parts by volume and water 100 parts by volume to the 250ml measuring bottle, frequency is a 250W 40KHz supersound process to whole molten loosing, add water to scale, shake up, filter, discard filtrate 20 parts by volume just, precision is measured subsequent filtrate 10 parts by volume, put in the 100ml measuring bottle, add water to scale, shake up, precision is measured 5 parts by volume, put in the 25ml measuring bottle, add water to 10 parts by volume, add 1% oxammonium hydrochloride. solution, 1 parts by volume and 0.2%2 again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 1% oxammonium hydrochloride. solution, 1 parts by volume and 0.2%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix VA of Chinese Pharmacopoeia version in 2005 ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; From the weight that standard curve is read ferrous sulfate the need testing solution, calculate, that is, drug combination preparation per diem taking dose meter contains Melanteritum with ferrous sulfate FeSO 4The 7H2O meter must not be lower than 0.624 weight portion.
3. method of quality control as claimed in claim 1 is characterized in that this method comprises one or more in following discriminating and/or the content:
Differentiate: A. compositions preparation 20 weight portions of getting it filled, porphyrize adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 60 parts by volume, supersound process or hot reflux or merceration extracted 40 minutes, filter, filtrate evaporate to dryness, residue add water 30 parts by volume makes dissolving, with n-butyl alcohol, chloroform or ethyl acetate extraction three times, each solvent is 15 parts by volume, merge extractive liquid,, evaporate to dryness, residue adds methanol or ethanol 1 parts by volume makes dissolving, as need testing solution; Other gets Radix Kansui control medicinal material 3 weight portions, add methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 40 parts by volume, supersound process or hot reflux or merceration extracted 40 minutes, filter, the filtrate evaporate to dryness, residue adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate 1 parts by volume makes dissolving, in contrast medical material solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 0.01 parts by volume, control medicinal material solution 0.005 parts by volume, put respectively on same silica gel g thin-layer plate, with chloroform: ethyl acetate: the solution of formic acid=15: 3: 3 is developing solvent, launch, take out, dry, put ultra-violet lamp and under 365nm, inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
B. compositions preparation 20 weight portions of getting it filled, porphyrize adds petroleum ether, chloroform or ethyl acetate 50 parts by volume of methanol, ethanol, n-butyl alcohol, 60～90 ℃ of boiling ranges, flooded 45 minutes, hot reflux or frequency are 250W 40KHz supersound process 40 minutes, discard solvent, and medicinal residues are flung to solvent, 50 parts by volume add diethyl ether, flooded 1 hour, hot reflux or frequency are 250W 40KHz supersound process 40 minutes, filter, filtrate is concentrated into 1 parts by volume, as need testing solution; Other evens up pier fruit acid reference substance, adds methanol, ethanol, n-butyl alcohol, chloroform or ethyl acetate and makes the solution that per 1 parts by volume contains 0.001 weight portion, product solution in contrast; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 0.010 parts by volume, reference substance solution 0.005 parts by volume, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: acetone: the solution of ethyl acetate=5: 3: 3 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; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C. compositions preparation 20 weight portions of getting it filled, porphyrize, the petroleum ether or chloroform 50 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration extracted 40 minutes, filter, petroleum ether or chloroform 1 parts by volume that filtrate evaporate to dryness, residue add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, as need testing solution; Other gets Radix Aucklandiae control medicinal material 2 weight portions, the petroleum ether or chloroform 10 parts by volume that add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges, supersound process or hot reflux or merceration 40 minutes, filter, the filtrate evaporate to dryness, petroleum ether or chloroform 1 parts by volume that medicinal residues add methanol, ethanol, ether, ethyl acetate, n-butyl alcohol, 60～90 ℃ of boiling ranges make dissolving, in contrast medical material solution; Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 0.01 parts by volume of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction: the solution of acetone=8: 3 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and is moistening fully to the plate face; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
Assay:
The preparation of reference substance solution: get ferrous sulfate reference substance 0.5 weight portion, accurate claim surely, put in the 100ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 1 parts by volume and water 80 parts by volume and to the 100ml measuring bottle, make dissolving, add water to scale, shake up, precision is measured 2 parts by volume, put in the 100ml measuring bottle, add water to scale, shake up, promptly getting concentration is the reference substance solution of ferrous 0.08 weight portion of sulfur acid in per 1 parts by volume;
The preparation of standard curve: precision is measured reference substance solution 1 parts by volume, 2 parts by volume, 4 parts by volume, 6 parts by volume, 8 parts by volume, put respectively in the 25ml measuring bottle, add water to 18 parts by volume, add 2% oxammonium hydrochloride. solution, 1 parts by volume and 0.25%2 again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 2% oxammonium hydrochloride. solution, 1 parts by volume and 0.25%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix V of Chinese Pharmacopoeia version in 2005 A ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; Algoscopy: the compositions preparation of getting it filled, porphyrize is got 4 weight portions, and accurate the title decides, put in the 250ml measuring bottle, get sulphuric acid 1ml and be dissolved in the 20ml water and make sulfuric acid solution, add above-mentioned sulfuric acid solution 2.5 parts by volume and water 100 parts by volume to the 100ml measuring bottle, frequency is a 250W 40KHz supersound process to whole molten loosing, add water to scale, shake up, filter, discard filtrate 25 parts by volume just, precision is measured subsequent filtrate 6 parts by volume, put in the 100ml measuring bottle, add water to scale, shake up, precision is measured 7 parts by volume, put in the 25ml measuring bottle, add water to 15 parts by volume, add 2% oxammonium hydrochloride. solution, 1 parts by volume and 0.25%2 again, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to scale, shakes up; Get 2 of 2% oxammonium hydrochloride. solution, 1 parts by volume and 0.25%, 2-bipyridyl alcoholic solution 1 parts by volume, mixing adds water to 25ml, is blank solution; According to an appendix VA of Chinese Pharmacopoeia version in 2005 ultraviolet visible spectrophotometry, measure absorbance at the wavelength place of 522nm, be that vertical coordinate, concentration are abscissa drawing standard curve with the absorbance; From the weight that standard curve is read ferrous sulfate the need testing solution, calculate, that is, drug combination preparation per diem taking dose meter contains Melanteritum with ferrous sulfate FeSO 47H 2The O meter must not be lower than 0.624 weight portion.
CN 200810056503 2008-01-21 2008-01-21 Quality standard and test method of hoove pill and detection method Active CN101229248B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200810056503 CN101229248B (en) 2008-01-21 2008-01-21 Quality standard and test method of hoove pill and detection method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200810056503 CN101229248B (en) 2008-01-21 2008-01-21 Quality standard and test method of hoove pill and detection method

Related Child Applications (1)

Application Number Title Priority Date Filing Date
CN201110222362.1A Division CN102305840B (en) 2008-01-21 2008-01-21 Hoove pill and quality standard and test method for preparation of hoove pill

Publications (2)

Publication Number Publication Date
CN101229248A true CN101229248A (en) 2008-07-30
CN101229248B CN101229248B (en) 2013-10-30

Family

ID=39896262

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 200810056503 Active CN101229248B (en) 2008-01-21 2008-01-21 Quality standard and test method of hoove pill and detection method

Country Status (1)

Country Link
CN (1) CN101229248B (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105749017A (en) * 2016-04-28 2016-07-13 邯郸制药股份有限公司 Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition
CN105749018A (en) * 2016-04-28 2016-07-13 邯郸制药股份有限公司 Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition
CN105749019A (en) * 2016-04-28 2016-07-13 邯郸制药股份有限公司 Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition
CN105796975A (en) * 2016-04-28 2016-07-27 邯郸制药股份有限公司 Traditional Chinese medicine composition capable of treating hoove
CN105796976A (en) * 2016-04-28 2016-07-27 邯郸制药股份有限公司 Traditional Chinese medicine composition and preparation capable of treating hoove
CN105920390A (en) * 2016-04-28 2016-09-07 邯郸制药股份有限公司 Traditional Chinese medicinal composition for treating hoove and preparation of traditional Chinese medicinal composition
CN105920389A (en) * 2016-04-28 2016-09-07 邯郸制药股份有限公司 Traditional Chinese medicinal composition for treating hoove and preparation of traditional Chinese medicinal composition

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1440772A (en) * 2003-04-08 2003-09-10 邯郸制药有限公司 Composite Chinese medicine for treating bloat and its prepn process and quality control method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1440772A (en) * 2003-04-08 2003-09-10 邯郸制药有限公司 Composite Chinese medicine for treating bloat and its prepn process and quality control method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
中华人民共和国卫生部药典委员会: "《卫生部颁药品标准中药成方制剂第二册》", 31 December 1990 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105749017A (en) * 2016-04-28 2016-07-13 邯郸制药股份有限公司 Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition
CN105749018A (en) * 2016-04-28 2016-07-13 邯郸制药股份有限公司 Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition
CN105749019A (en) * 2016-04-28 2016-07-13 邯郸制药股份有限公司 Traditional Chinese medicine composition for treating hoove and preparation of traditional Chinese medicine composition
CN105796975A (en) * 2016-04-28 2016-07-27 邯郸制药股份有限公司 Traditional Chinese medicine composition capable of treating hoove
CN105796976A (en) * 2016-04-28 2016-07-27 邯郸制药股份有限公司 Traditional Chinese medicine composition and preparation capable of treating hoove
CN105920390A (en) * 2016-04-28 2016-09-07 邯郸制药股份有限公司 Traditional Chinese medicinal composition for treating hoove and preparation of traditional Chinese medicinal composition
CN105920389A (en) * 2016-04-28 2016-09-07 邯郸制药股份有限公司 Traditional Chinese medicinal composition for treating hoove and preparation of traditional Chinese medicinal composition

Also Published As

Publication number Publication date
CN101229248B (en) 2013-10-30

Similar Documents

Publication Publication Date Title
CN101229248B (en) Quality standard and test method of hoove pill and detection method
CN102854281B (en) Detection method of sugar-free strong loquat syrup
CN102590433B (en) A kind of quality determining method of the smooth preparation of liver
CN102323371B (en) Detection method of haemostasis medicine
CN106370749A (en) Quality detection method of ginseng basis-consolidating oral solution
CN102579861B (en) Method for detecting quality of An'erning granules
CN104758515A (en) Traditional Chinese medicinal composition for treating nephropathy as well as preparation method and detection method thereof
CN105301136B (en) Nine-element wind-extinguishing particle component quantitative detection method and fingerprint construction method
CN102269752B (en) Detection method for pharmaceutical composition preparation
CN101982189A (en) Method for detecting salvia heart-soothing capsules
CN101181589A (en) Method for detecting the mass of tsunematsu 8-flavour agilawood tambac tablet
CN104069200B (en) A kind of SANHUANG XIEXIN TANG granule and preparation method thereof and detection method
CN102305840B (en) Hoove pill and quality standard and test method for preparation of hoove pill
CN104614475A (en) Thirst quenching clearing particle content detection method
CN104345108B (en) Qualitative quantitative determination method for liver-heat-clearing tablet
CN103823016B (en) Detecting method of DanTianJingShu oral preparation
CN102078503A (en) Detection method for pulse-activating decoction traditional Chinese medicine preparation
CN101912522A (en) Detection method of Liuweisheng tablets
CN100998617A (en) Quality control method for Xindakang preparation
CN103405664B (en) Daochi powder formula granule as well as preparation method, use and detection method thereof
CN102353731A (en) Method for detecting astragalus-chickpea particles
CN102068599B (en) Detection method for phlegm eliminating and asthma relieving cough syrup
CN101011450A (en) Quality control method for lucid ganoderma gynostemma pentaphylla oral liquid
CN109917041A (en) The measuring method of a variety of active ingredients content in xiaoshuan tongluo tablet
CN104345115B (en) A kind of method for qualitative and quantitative detection of Kanggu-Zengsheng tablet

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C56 Change in the name or address of the patentee

Owner name: HANDAN PHARMACY CO., LTD.

Free format text: FORMER NAME: HANDAN MOLUODAN PHARMACEUTICAL CO., LTD.

CP01 Change in the name or title of a patent holder

Address after: 056005 No. 309 National Road, Handan Industrial Park, Hebei, 18

Patentee after: HANDAN PHARMACEUTICAL CO., LTD.

Address before: 056005 No. 309 National Road, Handan Industrial Park, Hebei, 18

Patentee before: Handan Moluodan Pharmaceutical Co., Ltd.