CN101987146A - Preparation method of capsule for treating pharyngitis and infection of upper respiratory tract and detection method of capsule - Google Patents
Preparation method of capsule for treating pharyngitis and infection of upper respiratory tract and detection method of capsule Download PDFInfo
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Abstract
The invention provides a preparation method of a capsule preparation (Antaituo capsule) for treating pharyngitis and infection of the upper respiratory tract and a quality detection method of the capsule. The preparation method comprises the steps of: taking 350 g of iris tectorum maxim total flavonoids, drying to make the moisture content lower than 5%, smashing into fine powder which can pass through a 60-mesh screen, adding talcum powder accounting for1-3% by weight of the fine power,mixing evenly, and loading into a number one hard capsule. Besides a check on general projects according to the pharmacopoeia general rule, in the detection method, methods for identifying the main active ingredient tectoridin are formulated, comprising spectrophotometry and thin layer chromatography; the content of the iris tectorum maxim total flavonoids is determined through the spectrophotometry to ensure that the quantity of the active ingredient is more steady, and the quality of the preparation is effectively controlled to ensure the clinical effects, thereby the safe and effective medication for people is ensured.
Description
Technical field
The present invention relates to a kind of pure Chinese medicinal preparation, relate in particular to safe and sound appropriate capsular preparation method of a kind of medicine for the treatment of pharyngolaryngitis and upper respiratory tract infection----and quality determining method thereof.
Background technology
Existing a kind of medicine for the treatment of pharyngolaryngitis and upper respiratory tract infection is a kind of Chinese medicine decoction that is formed through decoction by the Chinese crude drug Rhizoma Belamcandae, and it has heat-clearing and toxic substances removing, the effect of detumescence sore-throat relieving; The laryngopharynx swelling and pain, hoarseness, the cough expectorant Huang that are used for the treatment of due to acute pharyngitis, laryngitis and the acute upper respiratory tract infection have better curative effect.But it has the trouble of decocting, and is difficult for storing, and carries and takes inconvenience, is not easy to accurate divided dose, and patient is to amount of water, and decocting time etc. are had little understanding or disliked trouble, and do not decoct on request, and shortcoming such as affect the treatment.Someone is directly taken by the active ingredient Rhizoma Belamcandae total flavones that the Chinese crude drug Rhizoma Belamcandae has extracted Rhizoma Belamcandae, and same existence is carried and taken inconvenience, is not easy to shortcomings such as accurate divided dose affects the treatment.
The existing medicine of being made by the Chinese crude drug Rhizoma Belamcandae does not have to set up relevant quality control standard yet, therefore need provide the detection method of this medicine being carried out quality control, makes it can control the quality of this pharmaceutical preparation effectively, guarantees clinical efficacy.
Summary of the invention
Primary and foremost purpose of the present invention, it is the shortcoming of directly taking at above Rhizoma Belamcandae Chinese medicine decoction and Rhizoma Belamcandae extract Rhizoma Belamcandae active ingredient Rhizoma Belamcandae total flavones, and provide a kind of preparation method for the treatment of the capsule preparations (safe and sound appropriate capsule) of pharyngolaryngitis and upper respiratory tract infection, the safe and sound appropriate capsule of this method preparation is easy to store, and is easy to carry, is convenient to divided dose exactly when taking, can directly take, dose is little, and effect is rapid, safety and sanitation.
Another object of the present invention is intended to provide a kind of quality determining method for the treatment of pharyngolaryngitis and upper respiratory tract infection capsule preparations.It is not set up any relevant quality control standard at said preparation, content, characteristic and preparation technology according to our medical material, having studied and defined relevant composition differentiates and content assaying method, except carrying out according to the pharmacopeia general rule the inspection of general data, also formulated the discrimination method that mainly contains the effective constituent belamcandin wherein, comprise the discriminating of spectrophotography and thin layer chromatography, also use spectrophotometry Rhizoma Belamcandae content of total flavone, make the amount of its active ingredient more stable, control the quality of said preparation effectively, guarantee its clinical efficacy.
Technical scheme of the present invention is as follows:
This treatment pharyngolaryngitis and upper respiratory tract infection capsule are to add appropriate amount of auxiliary materials by Rhizoma Belamcandae total flavones 350g to be prepared from.
The capsular preparation method of this treatment pharyngolaryngitis and upper respiratory tract infection: get Rhizoma Belamcandae total flavones 350g, dry, make its moisture be lower than 5%, pulverize with pulverizer, cross 60 eye mesh screens, add the Pulvis Talci of fine powder gross weight 1%～3%, mix homogeneously, be filled in No. 1 hard capsule with capsule filler, promptly get 1000 in this medicament capsule preparation.
Preparation method is more specifically:
Get Rhizoma Belamcandae total flavones 350g, put it in the exsiccator and under 75 ℃～95 ℃ temperature, carry out drying, make its moisture be lower than 5%, prepared Rhizoma Belamcandae total flavones is pulverized with pulverizer, cross 60 eye mesh screens, the Pulvis Talci that adds Rhizoma Belamcandae total flavones fine powder gross weight 2%, in blender, mixed 20～40 minutes, make its mix homogeneously, homogeneous mixture is filled in No. 1 hard capsule with capsule filler, making the Rhizoma Belamcandae total flavones fine powder of filling in every capsules is 0.35g, makes 1000 of capsules altogether.
Described pulverizer is a Universalpulverizer.
Described blender is multidirectional motion blender.
Described exsiccator is the heat-wind circulate drying device.
The capsular detection method of this treatment pharyngolaryngitis and upper respiratory tract infection, comprise in character, inspection, discriminating and the assay project partly or entirely; Wherein: character should meet the pertinent regulations under the capsule item, inspection should meet relevant every regulation under an appendix IL of Chinese Pharmacopoeia version in 2005 the capsule item, discriminating is the discriminating to belamcandin in the preparation, and assay is that Rhizoma Belamcandae content of total flavone in the preparation is measured.
The discriminating of belamcandin is to be contrast with the belamcandin reference substance, adopts spectrophotography and thin layer chromatography to differentiate respectively.
Concrete composition discrimination method is:
Get this product content 25mg, place the 50ml volumetric flask, the dissolve with ethanol with 65%～75% also is diluted to scale, shake up, the accurate 1ml that draws is in the 50ml volumetric flask, and the ethanol dilution with 65%～75% shakes up to scale, promptly get need testing solution, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, the ethanol with 65%～75% is blank solution, in the interscan of wavelength 200～400nm scope, the recording light spectrogram, there is absorption maximum at the place at 264～268nm wavelength; Or
Get belamcandin reference substance 5mg, place the 50ml volumetric flask, add 65%～75% dissolve with ethanol and be diluted to scale, in contrast product solution; Get this product content 25mg and place the 50ml volumetric flask, the dissolve with ethanol with 65%～75% also is diluted to scale, shakes up, as need testing solution; According to 2005 editions one appendix VIB thin layer chromatography test of Chinese Pharmacopoeia, drawing each 10 μ l of need testing solution and reference substance solution, put respectively on same silica GF254 lamellae, is developing solvent with chloroform, methanol, formic acid, chloroform wherein: methanol: formic acid=8～12: 0.5～1.5: 0.05～0.15, launch, take out, dry, put under the 254nm ultraviolet light and inspect, the test sample chromatograph should show three principal spots, with reference substance chromatograph relevant position on, show identical speckle;
The Rhizoma Belamcandae determination of total flavonoids is to be contrast with the belamcandin reference substance, adopts spectrophotography to measure.
Concrete content assaying method is:
The preparation of reference substance solution: precision takes by weighing the belamcandin reference substance 15mg that is dried to constant weight, puts in the 50ml volumetric flask, and the dissolve with ethanol with 65%～75% also is diluted to scale, shakes up, and promptly gets reference substance solution;
The preparation of need testing solution: get this product content 25mg, put in the 50ml volumetric flask, the accurate title, decide, and the dissolve with ethanol with 65%～75% also is diluted to scale, shakes up, and promptly gets need testing solution;
Precision is measured reference substance solution and each 1ml of need testing solution, put respectively in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, the ethanol with 65%～75% is blank solution, measure the trap of reference substance solution and need testing solution respectively at 266nm wavelength place, calculate, promptly
Every of this product contains the Rhizoma Belamcandae total flavones with belamcandin (C
11H
22O
11) calculate, must not be less than 180mg.
Detection method of the present invention comprises:
Character: this product is a hard capsule, and content is pale brown toner end, feeble QI suffering, bitter in the mouth;
Differentiate: get this product content 25mg and place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, the accurate 1ml that draws is in the 50ml volumetric flask, with 70% ethanol dilution to scale, shake up, promptly get need testing solution, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, with 70% ethanol is blank solution, in the interscan of wavelength 200～400nm scope, the recording light spectrogram, there is absorption maximum at the place at 264～268nm wavelength; Or
Get belamcandin reference substance 5mg, place the 50ml volumetric flask, add 70% dissolve with ethanol and be diluted to scale, in contrast product solution; Get this product content 25mg, place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, as need testing solution; According to 2005 editions one appendix VIB thin layer chromatography of Chinese Pharmacopoeia, draw each 10 μ l of need testing solution and reference substance solution, put respectively on same silica GF254 lamellae, with chloroform: methanol: formic acid=10: 1: 0.1 is developing solvent, launches, take out, dry, put under the ultraviolet light (254nm) and inspect, the test sample chromatograph should show three principal spots, with reference substance chromatograph relevant position on, show identical speckle;
Check: should meet relevant every regulation under an appendix IL of Chinese Pharmacopoeia version in 2005 the capsule item;
Assay: the preparation of reference substance solution: precision takes by weighing the belamcandin reference substance 15mg that is dried to constant weight at 105 ℃, puts in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shakes up, and promptly gets reference substance solution;
The preparation of need testing solution: get this product content 25mg, put in the 50ml volumetric flask, accurate claim surely, with 70% dissolve with ethanol and be diluted to scale, shake up, promptly get need testing solution;
Precision is measured reference substance solution and each 1ml of need testing solution, put respectively in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, be blank solution with 70% ethanol, measure the trap of reference substance solution and need testing solution respectively at 266nm wavelength place, calculate, promptly;
Every of this product contains the Rhizoma Belamcandae total flavones with belamcandin (C
11H
22O
11) calculate, must not be less than 180mg.
In order to ensure method for making of the present invention and quality determining method science, reasonable, feasible, the applicant studies methods such as composition discriminating, content detection in preparation method and the detection method, and concrete experimental data is as follows:
(1) preparation technology investigates:
For the preparation technology's that investigates this product optimum condition, the applicant has designed orthogonal test.By trial test, determined that tentatively the Rhizoma Belamcandae total flavones adds suitable adjuvant direct packaging capsule, does not need to carry out granulation process.By trial test, know that the fineness of Rhizoma Belamcandae total flavones is influential to packing control content uniformity, so the fineness of Rhizoma Belamcandae total flavones is investigated, respectively different degrees of grinding are tested.The main effect that adds adjuvant has two, and the one, increase flowability, be convenient to packing control content uniformity, make loading amount accurate; The 2nd, make capsular content be easy to dissolving, met the requirements the disintegration of this product.In addition, the very easy moisture absorption of Rhizoma Belamcandae total flavones is so the relative humidity of control production environment is necessary, so the relative humidity of production packing environment is also investigated.In order to make capsular content be easy to dissolving, met the requirements the disintegration of this product, also add a certain amount of cane sugar powder and investigate.
In order scientifically to investigate preparation technology, designed following orthogonal test:
The smashing fineness of Rhizoma Belamcandae total flavones is respectively and does not pulverize, pulverized 60 mesh sieves, pulverized 100 mesh sieves;
Adding talcous amount is respectively and does not add, adds 2%, adds 5%;
The relative humidity of capsule subpackage environment is respectively 35%, 45%, 55%.
The amount that adds cane sugar powder be respectively do not add, add 5%, adding 10%;
According to the method for orthogonal test, carried out 9 tests altogether, investigate the amount of the smashing fineness of Rhizoma Belamcandae total flavones, the relative humidity that adds talcous amount, capsule subpackage environment, adding cane sugar powder respectively.
The orthogonal test planning chart
From above computational analysis, A factor (smashing fineness of Rhizoma Belamcandae total flavones) having the greatest impact to content uniformity, next is that B factor (adding talcous amount) is bigger to the influence of content uniformity, and C factor (relative humidity of capsule subpackage environment) and D factor (amount that adds cane sugar powder) do not have influence to content uniformity basically.Generally speaking, difference is little, but from result of the test, can the factor level combination be: the amount that the Rhizoma Belamcandae total flavones pulverized 60 mesh sieves, add that talcous amount is 5%, the relative humidity of capsule subpackage environment is 55%, add cane sugar powder is 5%.
It more than is statistical analysis to result of the test.Test situation binding isotherm from reality comes above Several Factors is analyzed again, as can be seen, it is optimum that the Rhizoma Belamcandae total flavones was pulverized 60 mesh sieves, if because the Rhizoma Belamcandae total flavones is not pulverized, have the uneven situation of thickness, cause content uniformity big, if the smashing fineness of Rhizoma Belamcandae total flavones is too little, also can influence its flowability, make its mobile variation, cause content uniformity big; From above statistical computation, add talcous amount and be 5% best, still, statistical result T2 is 51, T3 is 49, is more or less the same, and from the angle of medicine, can then lack usefulness with adjuvant less as far as possible, is 2% so decision adds talcous amount; From above statistical computation, the relative humidity of capsule subpackage environment is 55% best, but, statistical result T1 is 56, T2 is 57, T3 is 55, substantially the same, so the relative humidity of capsule subpackage environment seems that content uniformity is not had influence, in theory, if air humidity is big, the Rhizoma Belamcandae total flavones is easily moisture absorption again, be to produce bigger influence to content uniformity, but because the packing process time is shorter, it is short that the Rhizoma Belamcandae total flavones is exposed to the airborne time, so show and do not have influence, in actual production process, as long as meet the requirement of " Good Manufacturing Practice and Quality Control of Drug ", promptly relative humidity in 45% to 65% scope just, humidity is low more good more in theory, but humidity is too low, and the easy dehydration of capsule shells becomes fragile, and also is unfavorable for capsule subpackage; From above statistical computation, the amount that adds cane sugar powder is 5% best, but, statistical result T1 is 57, T2 is 55, T3 is 56, substantially the same, so add cane sugar powder content uniformity there is not influence, in theory, adding cane sugar powder does not have shadow to content uniformity yet, and the purpose that adds cane sugar powder is in order to make capsular disintegration shorter.
As can be seen, adding the relative humidity of talcous amount, capsule subpackage environment and the amount of adding cane sugar powder does not all have influence to the disintegration of this product from above orthogonal test planning chart, and its numeral is respectively 18,18,18,17,16,16,16,16,16; From above orthogonal test planning chart as can be seen, add talcous amount, the amount of the relative humidity of capsule subpackage environment and adding cane sugar powder is not to all there being influence the disintegration of this product, just the smashing fineness of Rhizoma Belamcandae total flavones is slightly influential to it, do not pulverize, pulverized 60 mesh sieves, pulverized 100 mesh sieves, be respectively its disintegration 18 minutes, 16 minutes, 16 minutes, analyze theoretically, the Rhizoma Belamcandae total flavones is a Chinese medicine extract, it is a material that purity is higher, its dissolubility is also better, its smashing fineness is slightly influential to its dissolving, so it is slightly influential to disintegration, just reach the purpose that disintegrate is in the short period of time dissolved but can not add cane sugar powder fully, so decision does not add cane sugar powder.
From above test and statistical analysis, theory analysis as can be seen, this preparation method is rationally feasible.
(2) check
Raw material Rhizoma Belamcandae total flavones is extracted by the Chinese crude drug Rhizoma Belamcandae; be brown yellow granule or powder; once raw material Rhizoma Belamcandae total flavones is directly encapsulated; the result just causes capsular content uniformity very big; so raw material Rhizoma Belamcandae total flavones is pulverized; be ground into behind the fine powder encapsulatedly again, its content uniformity is just little as a result, but the bigger situation of content uniformity is arranged still the time.Think it is the flowability problem of Rhizoma Belamcandae total flavones powder, add an amount of Pulvis Talci or magnesium stearate, encapsulated again behind the mixing, its content uniformity is just very little, can meet the requirement that pharmacopeia capsule general rule content uniformity is checked fully.
(3) differentiate
Composition differentiates that spectrophotography is differentiated:
Belamcandin is the Main Ingredients and Appearance in the Rhizoma Belamcandae total flavones, by trial test, known its maximum absorption wavelength near 266nm, so with spectrophotometer to its solution in the interscan of wavelength 200～400nm scope, the recording light spectrogram is sought the accurate position of its maximum absorption wavelength.By test of many times, determined that it should have absorption maximum at 266+2nm wavelength place.In order to prepare the need testing solution of suitable concentration, done test of many times, determined following method at last:
Get this product content 25mg and place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, 0.5mg/ml solution, accurate this solution 1ml that draws, shakes up to scale with 70% ethanol dilution in the 50ml volumetric flask, promptly gets need testing solution liquid.Getting need testing solution, press 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, is blank with 70% ethanol, in the interscan of wavelength 200～400nm scope, recording light spectrogram.By test of many times, its repeatability is better, and should there be absorption maximum at the place at 266 ± 2nm wavelength.
Thin layer chromatography is differentiated:
Because this product Main Ingredients and Appearance is a belamcandin, so select the belamcandin reference substance to compare, because the preparation that this product is made for the single medicinal substances extract, its test sample directly just can dissolve fully with 70% ethanol, so, get this product content 25mg and place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, get 0.5mg/m1 solution, as need testing solution.Done a large amount of tests for the selection of developing solvent and lamellae.Use the silica GF254 lamellae, put under the ultraviolet light (254nm) and inspect, its several principal spots are obvious and clear.The applicant has investigated several development systems, from simple to complexity, chloroform is arranged: methanol, chloroform: formic acid, chloroform: ethanol etc., still find at last with chloroform: methanol: formic acid=10: 1: 0.1 is developing solvent, and separating degree is good, and clear spot launches effective.So following method is adopted in decision:
Get belamcandin reference substance 5mg, place the 50ml volumetric flask, add 70% dissolve with ethanol and be diluted to scale, in contrast product solution.According to 2005 editions appendix VIB tests of Chinese Pharmacopoeia, draw each 10 μ l of need testing solution and reference substance solution, put respectively on same silica GF254 lamellae, with chloroform: methanol: formic acid=10: 1: 0.1 is developing solvent, launches, and takes out, dry, put under the ultraviolet light (254nm) and inspect.By test of many times, the test sample chromatograph all shows three principal spots, with reference substance chromatograph relevant position on, show identical speckle.Its repeatability is better.
(4) assay
The Rhizoma Belamcandae content of total flavone is measured:
By prescription analysis, belamcandin as the index composition, is carried out the control of finished product content.Adopt spectrophotography to carry out assay.
1. instrument and reagent
TU-1901 dualbeam uv-spectrophotometric instrument, the AG285 electronic analytical balance.Water is double distilled water, and all the other reagent are analytical pure.
2. the preparation of sample solution
Get this product content 15mg, put in the 50ml volumetric flask, accurate claim surely, with 70% dissolve with ethanol and be diluted to scale, shake up, promptly get need testing solution; Precision is measured reference substance solution and each 1ml of need testing solution, puts respectively in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shakes up, promptly.
3. the preparation of reference substance solution
Precision takes by weighing the belamcandin reference substance 5mg that is dried to constant weight at 105 ℃, puts in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shakes up, promptly.
4. measure the selection of wavelength
Because belamcandin is the Main Ingredients and Appearance in the Rhizoma Belamcandae total flavones, by trial test, known its maximum absorption wavelength near 266nm, the applicant with spectrophotometer to its solution in the interscan of wavelength 200～400nm scope, the recording light spectrogram is sought the accurate position of its maximum absorption wavelength.
By test of many times, sample is consistent with the absorption curve of reference substance, and at 266+2nm wavelength place maximum absorption band is arranged, and therefore, the applicant determines with 266nm to be to measure wavelength.
5. the preparation of standard curve
Accurate reference substance solution 1ml, 2ml, 3ml, 4ml, 5ml, the 6ml of drawing puts respectively in the 50ml measuring bottle, with 70% ethanol, dissolve and be diluted to scale, shakes up.With 70% ethanol is blank liquid, measures the trap of reference substance and need testing solution respectively at 266nm wavelength place, is vertical coordinate with trap A, and concentration C is an abscissa, the drawing standard curve.Its trap A and concentration C are good linear relationship, regression equation and correlation coefficient: A=0.4548C-0.0174, γ=0.9999 (C is a belamcandin concentration, and A is a trap).
6. assay
The applicant has measured 4 batches safe and sound appropriate capsular Rhizoma Belamcandae total flavones rhythm content with said method, and all passes through methodological studies such as precision, repeatability, stability, average recovery test, proves that this method effect is better.
4 batches safe and sound appropriate capsular Rhizoma Belamcandae content of total flavone
| Lot number | 091001? | ?091002? | ?091003? | ?091004? |
| The mg/ grain | 221? | ?227? | ?216? | ?219? |
The beneficial effect fruit that produces effect of the present invention:
Preparation method of the present invention, its preparation method is simple, and the adjuvant of interpolation is few, is convenient to large-scale production, and price economy is reasonable, is suitable for broad masses and selects for use; Simultaneously, this method is processed into capsule with the medicine material preparation, can increase stability of drug effectively, is easy to store, and is easy to carry, is convenient to divided dose exactly when taking, and can directly take: dose is little, and effect is rapid, safety and sanitation.
Quality determining method of the present invention, except carrying out according to the pharmacopeia general rule the inspection of general data, also formulated the discrimination method that mainly contains the effective constituent belamcandin wherein, comprise the discriminating of spectrophotography and thin layer chromatography, also use spectrophotometry Rhizoma Belamcandae content of total flavone, make the amount of its active ingredient more stable.By these quality control methods, just can reflect the quality of this treatment pharyngolaryngitis and upper respiratory tract infection (safe and sound appropriate capsule) better and more comprehensively, guarantee that its quality and curative effect reach requirement, thereby guarantee that the masses are safe and effective for medication.
The specific embodiment
Embodiment 1: treatment pharyngolaryngitis and the capsular preparation method of upper respiratory tract infection
Get Rhizoma Belamcandae total flavones 350g, put it in the heat-wind circulate drying device and under 80 ℃～85 ℃ temperature, carrying out drying, make its moisture be lower than 5%, prepared Rhizoma Belamcandae total flavones is pulverized with Universalpulverizer, cross 60 eye mesh screens, the Pulvis Talci that adds Rhizoma Belamcandae total flavones fine powder gross weight 2%, in multidirectional motion blender, mixed 30 minutes, make its mix homogeneously, homogeneous mixture is filled in No. 1 hard capsule with capsule filler, making the Rhizoma Belamcandae total flavones fine powder of filling in every capsules is 0.35g, makes 1000 of capsules altogether.
Embodiment 2: treatment pharyngolaryngitis and the capsular quality determining method one of upper respiratory tract infection
Character: this product is a hard capsule, and content is pale brown toner end, feeble QI suffering, bitter in the mouth;
Differentiate: get this product content 25mg, place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, the accurate 1ml that draws, shakes up to scale with 70% ethanol dilution in the 50ml volumetric flask, promptly get need testing solution, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, be blank solution with 70% ethanol, in the interscan of wavelength 200～400nm scope, the recording light spectrogram, there is absorption maximum at the place at 266 ± 2nm wavelength.Or
Get belamcandin reference substance 5mg, place the 50ml volumetric flask, add 70% dissolve with ethanol and be diluted to scale, in contrast product solution; Get this product content 25mg and place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, as need testing solution; According to 2005 editions one appendix VIB thin layer chromatography of Chinese Pharmacopoeia, draw each 10 μ 1 of need testing solution and reference substance solution, put respectively on same silica GF254 lamellae, with chloroform: methanol: formic acid=10: 1: 0.1 is developing solvent, launches, take out, dry, put under the 254nm ultraviolet light and inspect, the test sample chromatograph should show three principal spots, with reference substance chromatograph relevant position on, show identical speckle.
Check: should meet relevant every regulation under an appendix IL of Chinese Pharmacopoeia version in 2005 the capsule item.
Assay: the preparation precision of reference substance solution takes by weighing the belamcandin reference substance 15mg that is dried to constant weight at 105 ℃, puts in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shakes up, and promptly gets reference substance solution;
This product content 25mg is got in the preparation of need testing solution, puts in the 50ml volumetric flask, accurate claims surely, with 70% dissolve with ethanol and be diluted to scale, shakes up, and promptly gets need testing solution;
Precision is measured reference substance solution and each 1ml of need testing solution, put respectively in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, be blank solution with 70% ethanol, measure the trap of reference substance solution and need testing solution respectively at 266nm wavelength place, calculate, promptly;
Every of this product contains the Rhizoma Belamcandae total flavones with belamcandin (C
11H
22O
11) calculate, must not be less than 180mg.
Embodiment 3: treatment pharyngolaryngitis and the capsular quality determining method two of upper respiratory tract infection
Character: this product is a hard capsule, and content is pale brown toner end, feeble QI suffering, bitter in the mouth.
Differentiate: get this product content 25mg, place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, the accurate 1ml that draws, shakes up to scale with 70% ethanol dilution in the 50ml volumetric flask, promptly get need testing solution, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, be blank solution with 70% ethanol, in the interscan of wavelength 200～400nm scope, the recording light spectrogram, there is absorption maximum at the place at the 266+2nm wavelength.Or
Get belamcandin reference substance 5mg, place the 50ml volumetric flask, add 70% dissolve with ethanol and be diluted to scale, in contrast product solution; Get this product content 25mg and place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, as need testing solution; According to 2005 editions one appendix VIB thin layer chromatography of Chinese Pharmacopoeia, draw each 10 μ l of need testing solution and reference substance solution, put respectively on same silica GF254 lamellae, with chloroform: methanol: formic acid=10: 1: 0.1 is developing solvent, launches, take out, dry, put under the 254nm ultraviolet light and inspect, the test sample chromatograph should show three principal spots, with reference substance chromatograph relevant position on, show identical speckle.
Check: should meet relevant every regulation under an appendix IL of Chinese Pharmacopoeia version in 2005 the capsule item.
Embodiment 4: treatment pharyngolaryngitis and the capsular quality determining method three of upper respiratory tract infection
Character: this product is a hard capsule, and content is pale brown toner end, feeble QI suffering, bitter in the mouth.
Check: should meet relevant every regulation under an appendix IL of Chinese Pharmacopoeia version in 2005 the capsule item.
Assay: the preparation precision of reference substance solution takes by weighing the belamcandin reference substance 15mg that is dried to constant weight at 105 ℃, puts in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shakes up, and promptly gets reference substance solution;
This product content 25mg is got in the preparation of need testing solution, puts in the 50ml volumetric flask, accurate claims surely, with 70% dissolve with ethanol and be diluted to scale, shakes up, and promptly gets need testing solution;
Precision is measured reference substance solution and each 1ml of need testing solution, put respectively in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, be blank solution with 70% ethanol, measure the trap of reference substance solution and need testing solution respectively at 266nm wavelength place, calculate, promptly;
Every of this product contains the Rhizoma Belamcandae total flavones with belamcandin (C
11H
22O
11) calculate, must not be less than 180mg.
Embodiment 5: treatment pharyngolaryngitis and the capsular quality determining method four of upper respiratory tract infection
Character: this product is a hard capsule, and content is pale brown toner end, feeble QI suffering, bitter in the mouth.
Differentiate: get this product content 25mg, place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, the accurate 1ml that draws, shakes up to scale with 70% ethanol dilution in the 50ml volumetric flask, promptly get need testing solution, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, be blank solution with 70% ethanol, in the interscan of wavelength 200～400nm scope, the recording light spectrogram, there is absorption maximum at the place at 266 ± 2nm wavelength.Or
Get belamcandin reference substance 5mg, place the 50ml volumetric flask, add 70% dissolve with ethanol and be diluted to scale, in contrast product solution; Get this product content 25mg and place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, as need testing solution; According to 2005 editions one appendix VIB thin layer chromatography of Chinese Pharmacopoeia, draw each 10 μ l of need testing solution and reference substance solution, put respectively on same silica GF254 lamellae, with chloroform: methanol: formic acid=10: 1: 0.1 is developing solvent, launches, take out, dry, put under the 254nm ultraviolet light and inspect, the test sample chromatograph should show three principal spots, with reference substance chromatograph relevant position on, show identical speckle.
Assay:
The preparation of reference substance solution: precision takes by weighing the belamcandin reference substance 15mg that is dried to constant weight at 105 ℃, puts in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shakes up, and promptly gets reference substance solution;
The preparation of need testing solution: get this product content 25mg, put in the 50ml volumetric flask, accurate claim surely, with 70% dissolve with ethanol and be diluted to scale, shake up, promptly get need testing solution;
Precision is measured reference substance solution and each 1ml of need testing solution, put respectively in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, be blank solution with 70% ethanol, measure the trap of reference substance solution and need testing solution respectively at 266nm wavelength place, calculate, promptly;
Every of this product contains the Rhizoma Belamcandae total flavones with belamcandin (C
11H
22O
11) calculate, must not be less than 180mg.
Claims (7)
1. treat pharyngolaryngitis and the capsular preparation method of upper respiratory tract infection for one kind, it is characterized in that: get Rhizoma Belamcandae total flavones 350g, dry, make its moisture be lower than 5%, pulverize, cross 60 eye mesh screens with pulverizer, the Pulvis Talci that adds fine powder gross weight 1%～3%, mix homogeneously is filled in No. 1 hard capsule with capsule filler, promptly gets 1000 in this medicament capsule preparation.
2. according to described treatment pharyngolaryngitis of claim 1 and the capsular preparation method of upper respiratory tract infection, it is characterized in that: described medicament capsule preparation is to be prepared from by following concrete grammar
Get Rhizoma Belamcandae total flavones 350g, put it in the exsiccator and under 75 ℃～95 ℃ temperature, carry out drying, make its moisture be lower than 5%, prepared Rhizoma Belamcandae total flavones is pulverized with pulverizer, crossed 60 eye mesh screens, add the Pulvis Talci of Rhizoma Belamcandae total flavones fine powder gross weight 2%, in blender, mixed 20～40 minutes, make its mix homogeneously, homogeneous mixture is filled in No. 1 hard capsule with capsule filler, making the Rhizoma Belamcandae total flavones fine powder of filling in every capsules is 0.35g.
3. according to described treatment pharyngolaryngitis of claim 2 and the capsular preparation method of upper respiratory tract infection, it is characterized in that: described pulverizer is a Universalpulverizer.
4. according to described treatment pharyngolaryngitis of claim 2 and the capsular preparation method of upper respiratory tract infection, it is characterized in that: described blender is multidirectional motion blender.
5. according to described treatment pharyngolaryngitis of claim 2 and the capsular preparation method of upper respiratory tract infection, it is characterized in that: described exsiccator is the heat-wind circulate drying device.
6. a claim 1 or 2 described treatment pharyngolaryngitis and the capsular detection method of upper respiratory tract infection is characterized in that: this detection method comprise in character, inspection, discriminating and the assay project partly or entirely; Described discriminating is that the composition of belamcandin is differentiated that described assay is that the Rhizoma Belamcandae content of total flavone is measured;
Described discrimination method is:
Get this product content 25mg, place the 50ml volumetric flask, the dissolve with ethanol with 65%～75% also is diluted to scale, shake up, the accurate 1ml that draws is in the 50ml volumetric flask, and the ethanol dilution with 65%～75% shakes up to scale, promptly get need testing solution, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, the ethanol with 65%～75% is blank solution, in the interscan of wavelength 200～400nm scope, the recording light spectrogram, there is absorption maximum at the place at 264～268nm wavelength; Or
Get belamcandin reference substance 5mg, place the 50ml volumetric flask, add 65%～75% dissolve with ethanol and be diluted to scale, in contrast product solution; Get this product content 25mg and place the 50ml volumetric flask, the dissolve with ethanol with 65%～75% also is diluted to scale, shakes up, as need testing solution; According to 2005 editions one appendix VIB thin layer chromatography test of Chinese Pharmacopoeia, drawing each 10 μ l of need testing solution and reference substance solution, put respectively on same silica GF254 lamellae, is developing solvent with chloroform, methanol, formic acid, chloroform wherein: methanol: formic acid=8～12: 0.5～1.5: 0.05～0.15, launch, take out, dry, put under the 254nm ultraviolet light and inspect, the test sample chromatograph should show three principal spots, with reference substance chromatograph relevant position on, show identical speckle;
Described content assaying method is:
The preparation of reference substance solution: precision takes by weighing the belamcandin reference substance 15mg that is dried to constant weight, puts in the 50ml volumetric flask, and the dissolve with ethanol with 65%～75% also is diluted to scale, shakes up, and promptly gets reference substance solution;
The preparation of need testing solution: get this product content 25mg, put in the 50ml volumetric flask, the accurate title, decide, and the dissolve with ethanol with 65%～75% also is diluted to scale, shakes up, and promptly gets need testing solution;
Precision is measured reference substance solution and each 1ml of need testing solution, put respectively in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, the ethanol with 65%～75% is blank solution, measure the trap of reference substance solution and need testing solution respectively at 266nm wavelength place, calculate, promptly
Every of this product contains the Rhizoma Belamcandae total flavones to be calculated with belamcandin, must not be less than 180mg.
7. according to described treatment pharyngolaryngitis of claim 6 and the capsular detection method of upper respiratory tract infection, it is characterized in that described detection method comprises:
Character: this product is a hard capsule, and content is pale brown toner end, feeble QI suffering, bitter in the mouth;
Differentiate, get this product content 25mg, place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, the accurate 1ml that draws is in the 50ml volumetric flask, with 70% ethanol dilution to scale, shake up, promptly get need testing solution, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, with 70% ethanol is blank solution, in the interscan of wavelength 200～400nm scope, the recording light spectrogram, there is absorption maximum at the place at 264～268nm wavelength; Or
Get belamcandin reference substance 5mg, place the 50ml volumetric flask, add 70% dissolve with ethanol and be diluted to scale, in contrast product solution; Get this product content 25mg and place the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, as need testing solution; According to 2005 editions one appendix VIB thin layer chromatography of Chinese Pharmacopoeia, draw each 10 μ l of need testing solution and reference substance solution, put respectively on same silica GF254 lamellae, with chloroform: methanol: formic acid=10: 1: 0.1 is developing solvent, launches, take out, dry, put under the 254nm ultraviolet light and inspect, the test sample chromatograph should show three principal spots, with reference substance chromatograph relevant position on, show identical speckle;
Check: should meet relevant every regulation under an appendix IL of Chinese Pharmacopoeia version in 2005 the capsule item;
Assay: the preparation precision of reference substance solution takes by weighing the belamcandin reference substance 15mg that is dried to constant weight at 105 ℃, puts in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shakes up, and promptly gets reference substance solution;
This product content 25mg is got in the preparation of need testing solution, puts in the 50ml volumetric flask, accurate claims surely, with 70% dissolve with ethanol and be diluted to scale, shakes up, and promptly gets need testing solution;
Precision is measured reference substance solution and each 1ml of need testing solution, put respectively in the 50ml volumetric flask, with 70% dissolve with ethanol and be diluted to scale, shake up, according to 2005 editions one appendix VA spectrophotography of Chinese Pharmacopoeia, be blank solution with 70% ethanol, measure the trap of reference substance solution and need testing solution respectively at 266nm wavelength place, calculate, promptly;
Every of this product contains the Rhizoma Belamcandae total flavones to be calculated with belamcandin, must not be less than 180mg.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010285742 CN101987146A (en) | 2010-09-17 | 2010-09-17 | Preparation method of capsule for treating pharyngitis and infection of upper respiratory tract and detection method of capsule |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010285742 CN101987146A (en) | 2010-09-17 | 2010-09-17 | Preparation method of capsule for treating pharyngitis and infection of upper respiratory tract and detection method of capsule |
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| CN101987146A true CN101987146A (en) | 2011-03-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103134897A (en) * | 2013-02-02 | 2013-06-05 | 四川逢春制药有限公司 | Rhiaoma iridis tectori capsule detecting method |
| CN104597197A (en) * | 2015-01-23 | 2015-05-06 | 贵州神奇药物研究院 | Method for detecting accumulation-dispersing and bowel-relaxing pharmaceutical preparation |
| CN109700899A (en) * | 2019-03-12 | 2019-05-03 | 四川省中医药科学院 | A kind of Rhizoma Belamcandae skullcapflavone extract and its preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1839862A (en) * | 2005-04-01 | 2006-10-04 | 四川省中药研究所 | Pharyngolaryngitis-treating pharmaceutical compositions and its preparing method |
-
2010
- 2010-09-17 CN CN 201010285742 patent/CN101987146A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1839862A (en) * | 2005-04-01 | 2006-10-04 | 四川省中药研究所 | Pharyngolaryngitis-treating pharmaceutical compositions and its preparing method |
Non-Patent Citations (3)
| Title |
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| 《华西药学杂志》 20061231 张春荣等 射干的提取纯化工艺研究 447-449 1-7 第21卷, 第5期 2 * |
| 《四川中医》 20091231 袁崇均等 川射干总黄酮含量测定方法的比较研究 58-59 1-7 第8卷, 第8期 2 * |
| 《齐鲁药事》 20071231 王姣等 射干的现代研究概况 168-171 1-7 第26卷, 第3期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103134897A (en) * | 2013-02-02 | 2013-06-05 | 四川逢春制药有限公司 | Rhiaoma iridis tectori capsule detecting method |
| CN103134897B (en) * | 2013-02-02 | 2014-12-24 | 四川逢春制药有限公司 | Rhiaoma iridis tectori capsule detecting method |
| CN104597197A (en) * | 2015-01-23 | 2015-05-06 | 贵州神奇药物研究院 | Method for detecting accumulation-dispersing and bowel-relaxing pharmaceutical preparation |
| CN104597197B (en) * | 2015-01-23 | 2016-04-13 | 贵州神奇药物研究院 | A kind of detection method of the long-pending defaecation pharmaceutical preparation that disappears |
| CN109700899A (en) * | 2019-03-12 | 2019-05-03 | 四川省中医药科学院 | A kind of Rhizoma Belamcandae skullcapflavone extract and its preparation method and application |
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Open date: 20110323 |