CN102866213A - Quality control method of intestine astringe antidiarrheic preparation - Google Patents
Quality control method of intestine astringe antidiarrheic preparation Download PDFInfo
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- CN102866213A CN102866213A CN201210340301XA CN201210340301A CN102866213A CN 102866213 A CN102866213 A CN 102866213A CN 201210340301X A CN201210340301X A CN 201210340301XA CN 201210340301 A CN201210340301 A CN 201210340301A CN 102866213 A CN102866213 A CN 102866213A
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Abstract
The invention discloses a quality control method of intestine astringe antidiarrheic preparation. The intestine astringe antidiarrheic preparation consists of 7 to 18 parts by weight of featherleaf rodgersflower extract, 700 to 800 parts by weight of bentonite and auxiliary materials with appropriate quantity. The quality control method of the intestine astringe antidiarrheic preparation comprises the following steps of utilizing high-efficient liquid-phase chromatography to determine content of bergenin in the preparation; determining content of aluminum oxide in the intestine astringe antidiarrheic preparation; and determining content of silicon dioxide in the intestine astringe antidiarrheic preparation. The quality control method is characterized in that on the basis of the traditional standard, the main active component bergenin is quantitatively detected, and main active components such as aluminum oxide and silicon dioxide in the preparation are quantitatively detected. The method is operable, simple, feasible and capable of effectively controlling the quality of the intestine astringe antidiarrheic preparation.
Description
Technical field
The invention belongs to the traditional Chinese medicine quality technical field, be specifically related to a kind of method of quality control of relieving diarrhea with astringents pharmaceutical preparation.
Background technology
The relieving diarrhea with astringents that uses in the market circulation at present is loose, be used for the treatment of and have loose bowels due to the deficiency of spleen-QI and stomach-QI, acute chronic enteritis, enteritis anaphylactica, indigestion, bowel dysfunction etc. are seen above-mentioned disease person's Chinese patent drug, this product records in the 643rd page in " national standard for traditional Chinese medicines compilation " internal medicine taste fascicle, method of quality control in its quality standard is too simple, specificity is not strong, is difficult to the preparation active component is carried out effectively quantitatively control.Be the ultraviolet spectrophotometry of " Bergenin " under its quality standard assay item, sensitivity and accuracy slightly a little less than, and main active alundum (Al2O3), silicon dioxide in the prescription are not quantitatively controlled, can't be embodied the controllable principle of drug quality.Therefore, research set up a kind of relieving diarrhea with astringents pharmaceutical preparation accurately controlled active component quantitative control methodin be very important.
Summary of the invention
The object of the present invention is to provide a kind of have operability, simple, the accurate method of quality control of controlled relieving diarrhea with astringents pharmaceutical preparation.
The object of the present invention is achieved like this, and described relieving diarrhea with astringents pharmaceutical preparation is comprised of Rhizoma Rodgersiae extract 7 ~ 18 weight portions, bentonitic clay 700 ~ 800 weight portions and proper auxiliary materials, and described relieving diarrhea with astringents pharmaceutical preparation active component method of quality control comprises:
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Take methanol-water solution as mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: accurately weighed Bergenin reference substance adds methyl alcohol and makes the solution that every 1ml contains 0.05 ~ 0.15mg; The preparation of need testing solution: get the content 0. 5 ~ 1.5g in the preparation, accurately weighed, to the 50ml measuring bottle, add the ultrasonic processing 7 ~ 13min of methyl alcohol, let cool, add methyl alcohol to scale, shake up, filter, get subsequent filtrate as need testing solution; Determination method: precision is drawn reference substance solution and each 5 ~ 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculates Determination of Bergenin in the described relieving diarrhea with astringents pharmaceutical preparation;
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get the content 1 ~ 3g in the preparation, accurately weighed, put in the porcelain dish, add respectively sulfuric acid 4 ~ 8ml and nitric acid 8 ~ 12ml, treat effect fully, evaporate to dryness, let cool, add dilute sulfuric acid 20 ~ 40ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 2 ~ 5 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper with decantation, use hot wash, residue is for subsequent use; Filtrate merges, put in the 100ml measuring bottle, let cool, add water to scale, shake up, precision is measured 20ml, adds the alkalescent test solution to just separating out precipitation, drips the low concentration mineral acid again and extremely precipitates till the just dissolving, damping fluid 5 ~ the 15ml that adds pH6.0, the accurate Calcium Disodium Versenate vs 20 ~ 30ml that adds 0.05mol/L boils 3 ~ 5min again, lets cool, add xylenol orange indicator solution 0.5 ~ 2.5ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3, calculate the Al in the described relieving diarrhea with astringents pharmaceutical preparation
2O
3Content;
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 750 ~ 850 ℃ of lower blazing 1.5 ~ 2.5h, lets cool, and is accurately weighed; With the residue water-wet, add 5 ~ 9 in hydrofluorite 5 ~ 9ml and sulfuric acid again, evaporate to dryness at 750 ~ 850 ℃ of lower blazing 4 ~ 6min, lets cool, and is accurately weighed, subtracts the weight of mistake, is SiO in the described relieving diarrhea with astringents pharmaceutical preparation
2Content.
The present invention quantitatively detects the Bergenin prior art with HPLC and is applied to the relieving diarrhea with astringents oral solid formulation.By sample pre-treatments, chromatographic condition and system suitability Depth Study, the interference of other active components and interpolation auxiliary material in effectively avoiding writing out a prescription.Set up accurate, stable, the reliable Bergenin assay method of relieving diarrhea with astringents oral formulations.In addition, increased the composition alundum (Al2O3) of main active substances smectite, the content assaying method of silicon dioxide in the bentonitic clay, thereby can control bentonitic quality.
Description of drawings
Fig. 1 is the linear graph of linear test of the present invention.
Embodiment
The present invention is further illustrated below in conjunction with embodiment, but never in any form the present invention is limited, and any conversion or replacement based on training centre of the present invention is done all belong to protection scope of the present invention.
Relieving diarrhea with astringents pharmaceutical preparation of the present invention is comprised of Rhizoma Rodgersiae extract 7 ~ 18 weight portions, bentonitic clay 700 ~ 800 weight portions and proper auxiliary materials, and described relieving diarrhea with astringents pharmaceutical preparation method of quality control comprises:
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Take methanol-water solution as mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: accurately weighed Bergenin reference substance adds methyl alcohol and makes the solution that every 1ml contains 0.05 ~ 0.15mg; The preparation of need testing solution: get the content 0. 5 ~ 1.5g in the preparation, accurately weighed, to the 50ml measuring bottle, add the ultrasonic processing 7 ~ 13min of methyl alcohol, let cool, add methyl alcohol to scale, shake up, filter, get subsequent filtrate as need testing solution; Determination method: precision is drawn reference substance solution and each 5 ~ 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculates Determination of Bergenin in the described relieving diarrhea with astringents pharmaceutical preparation;
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get the content 1 ~ 3g in the preparation, accurately weighed, put in the porcelain dish, add respectively sulfuric acid 4 ~ 8ml and nitric acid 8 ~ 12ml, treat effect fully, evaporate to dryness, let cool, add dilute sulfuric acid 20 ~ 40ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 2 ~ 5 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper with decantation, use hot wash, residue is for subsequent use; Filtrate merges, put in the 100ml measuring bottle, let cool, add water to scale, shake up, precision is measured 20ml, adds the alkalescent test solution to just separating out precipitation, drips the low concentration mineral acid again and extremely precipitates till the just dissolving, damping fluid 5 ~ the 15ml that adds pH6.0, the accurate Calcium Disodium Versenate vs 20 ~ 30ml that adds 0.05mol/L boils 3 ~ 5min again, lets cool, add xylenol orange indicator solution 0.5 ~ 2.5ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3, the Al in the described relieving diarrhea with astringents pharmaceutical preparation of calculating
2O
3Content;
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 750 ~ 850 ℃ of lower blazing 1.5 ~ 2.5h, lets cool, and is accurately weighed; With the residue water-wet, add 5 ~ 9 in hydrofluorite 5 ~ 9ml and sulfuric acid again, evaporate to dryness at 750 ~ 850 ℃ of lower blazing 4 ~ 6min, lets cool, and is accurately weighed, subtracts the weight of mistake, is SiO in the described relieving diarrhea with astringents pharmaceutical preparation
2Content.
The method of quality control of described relieving diarrhea with astringents pharmaceutical preparation comprises:
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Take methanol-water solution as mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: accurately weighed Bergenin reference substance adds methyl alcohol and makes the solution that every 1ml contains 0.1mg; The preparation of need testing solution: get the content 0. 5 ~ 1.5g in the preparation, accurately weighed, to the 50ml measuring bottle, it is an amount of to add methyl alcohol, and ultrasonic processing 9 ~ 11min lets cool, and adds methyl alcohol to scale, shakes up, and filters, and gets subsequent filtrate as need testing solution; Determination method: precision is drawn reference substance solution and each 5 ~ 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculates Determination of Bergenin in the described relieving diarrhea with astringents pharmaceutical preparation;
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get the content 1 ~ 3g in the preparation, accurately weighed, put in the porcelain dish, add respectively sulfuric acid 5 ~ 7ml and nitric acid 9 ~ 11ml, treat effect fully, evaporate to dryness, let cool, add dilute sulfuric acid 30ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 3 ~ 4 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper with decantation, use hot wash, residue is for subsequent use; Filtrate merges, put in the 100ml measuring bottle, let cool, add water to scale, shake up, precision is measured 20ml, adds the alkalescent test solution to just separating out precipitation, drips the low concentration mineral acid again and extremely precipitates till the just dissolving, damping fluid 8 ~ the 12ml that adds pH6.0, the accurate Calcium Disodium Versenate vs 25ml that adds 0.05mol/L boils 3 ~ 5min again, lets cool, add xylenol orange indicator solution 0.5 ~ 1.5ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3, the Al in the described relieving diarrhea with astringents pharmaceutical preparation of calculating
2O
3Content;
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 750 ~ 850 ℃ of lower blazing 1.5 ~ 2.5h, lets cool, and is accurately weighed; With the residue water-wet, add 5 ~ 9 in hydrofluorite 5 ~ 9ml and sulfuric acid again, evaporate to dryness at 750 ~ 850 ℃ of lower blazing 4 ~ 6min, lets cool, and is accurately weighed, subtracts the weight of mistake, is SiO in the described relieving diarrhea with astringents pharmaceutical preparation
2Content.
The long-pending ratio of mobile phase methanol in the described A step-aqueous solution liquid is 0.2 ~ 0.3:0.7 ~ 0.8.
The long-pending ratio of described mobile phase methanol-aqueous solution liquid is 0.25:0.75.
What filter to use in the described A step is miillpore filter, and described miillpore filter is a kind of in teflon membrane filter, nylon leaching film, the regenerated cellulose filter membrane, and described filter membrane aperture is 0.4 ~ 0.50 μ m.
Described methanol concentration is 99.0 ~ 99.9%.
Described
BWhat the evaporate to dryness mode can be in sand bath evaporate to dryness, the water bath method in the step is a kind of.
What buffer solution can be in acetic acid-ammonium acetate buffer or the phosphate buffer in the described B step is a kind of.
What the alkalescent test solution can be in ammonia solution, sodium citrate, malate, the sodium phenate solution in the described B step is a kind of, and what described low concentration mineral acid can be in dilute sulfuric acid, watery hydrochloric acid or the rare nitric acid is a kind of.
Described preparation formulation is tablet, powder, granule, capsule or pill.
Content obtains through following method in the preparation: the content of tablet, pill is to obtain after grinding, and powder, granule directly use, and capsule obtains through removing capsule shells.
Characteristics of the present invention:
1, be the ultraviolet spectrophotometry of " Bergenin " under loose its quality standard assay item of relieving diarrhea with astringents that " national standard for traditional Chinese medicines compilation " records, the more efficient liquid phase chromatography, sensitivity and accuracy slightly a little less than, and main active alundum (Al2O3), silicon dioxide in the prescription are not quantitatively controlled, can't be embodied the controllable principle of drug quality.
2, the present invention is based on approval listing relieving diarrhea with astringents oral formulations active component and quantitatively controls defective, has set up the chemistry in detecting of HPLC assay method accurate, stable, reliably Determination of Bergenin and alundum (Al2O3), dioxide-containing silica.
1. measure reason: main active is quantitatively controlled
Main effective constituent in the rodgersflower rhizome is Bergenin.Utilize ultraviolet spectrophotometry that Determination of Bergenin is measured, more efficient liquid phase chromatography, sensitivity and accuracy slightly a little less than.Therefore, need to set up the content of Bergenin in the corresponding high effective liquid chromatography for measuring rodgersflower rhizome and accumulate the assay data, formulate rational content limit.
In addition, bentonitic clay is principal ingredient in the prescription, and its main active substances is smectite.The smectite principal ingredient is dioctahedral smectite, the lamellar structure that this material is comprised of the octahedra aluminium oxide of ditetrahedron monox list, have lamellar structure and heterogeneity CHARGE DISTRIBUTION, the toxin of the virus in the alimentary canal, germ and generation thereof is had fixing, suction-operated; Gastrointestinal mucosal there is covering power, and by mutually combining with MGP, from quality and quantity two aspect reparations, improve mucosal barrier to the defense function of attack factor, has balance normal flora and local analgesic effect.Smectite is as antidiarrheal agent, is widely used in clinically, and potential of hydrogen, granularity, loss on drying, absorption affinity etc. are arranged in the inspection item of its quality standard; The content of major control silicon dioxide, alundum (Al2O3) in the assay project.And prior art is not quantitatively controlled main active alundum (Al2O3), silicon dioxide in the prescription, therefore comprehensively, effectively control aspect its inherent quality to be improved.
2. advantage of the present invention:
HPLC is quantitatively detected the Bergenin prior art be applied to the relieving diarrhea with astringents oral solid formulation.By sample pre-treatments, chromatographic condition and system suitability Depth Study, the interference of other active components and interpolation auxiliary material in effectively avoiding writing out a prescription.Set up accurate, stable, the reliable Bergenin assay method of relieving diarrhea with astringents oral formulations.In addition, increased the composition alundum (Al2O3) of main active substances smectite, the content assaying method of silicon dioxide in the bentonitic clay, thereby can control bentonitic quality.
3. beneficial effect:
For detection sensitivity and result's accuracy, high-efficient liquid phase technique has clear superiority than ultraviolet spectrophotometry.Especially for the detection of complex sample, high-efficient liquid phase technique can will disturb the impurity effective separation, obtains accurately and effectively the testing result of sample.The present invention is on the ultraviolet spectrophotometry basis of existing Bergenin, by sample pre-treatments, chromatographic condition and system suitability Depth Study, set up the high-performance liquid chromatogram determination method of Determination of Bergenin in accurate, stable, the reliable relieving diarrhea with astringents pharmaceutical preparation, the interference of other active components and interpolation auxiliary material in effectively avoiding writing out a prescription, thereby the inherent quality of prevailing active component in the Quality control more fully and effectively is for such Chinese medicine preparation total quality control provides good basis.
Alundum (Al2O3), silicon dioxide content test method in " relieving diarrhea with astringents is loose " of the present invention, simple and easy to do, remedied the deficiency that prior art is not quantitatively controlled main active alundum (Al2O3), silicon dioxide in the prescription, thus bentonitic inherent quality in can Quality control.
Embodiment 1
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Methanol-water solution take volume ratio as 0.2:0.8 is mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: get the Bergenin reference substance, accurately weighed, add 99.5% methyl alcohol and make the solution that every 1ml contains 0.05mg; The preparation of need testing solution: get powder content 0.5g, accurately weighed is 0.5010
g, to the 50ml measuring bottle, add the ultrasonic processing of 99.5% methyl alcohol 9min, let cool, add 99.5% methyl alcohol to scale, shake up, filter by 0.40 μ m nylon leaching film, getting subsequent filtrate is need testing solution; Determination method: precision is drawn reference substance solution and each 5 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculating the Determination of Bergenin result is 11.35 mg/g.
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get powder content 3g, accurately weighed is 2.9989g, puts in the porcelain dish, adds respectively sulfuric acid 8ml and nitric acid 12ml, treats effect fully, extremely
Sand bathUpper evaporate to dryness lets cool, and adds dilute sulfuric acid 30ml, boils, and upper strata liquid filters through ashless filter paper with decantation, and with hot wash 3 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper, uses hot wash with decantation, and residue is for subsequent use; Filtrate merges, and puts in the 100ml measuring bottle, lets cool, and adds water to scale, shakes up, and precision is measured 20ml, adds ammonia solution to just separating out precipitation, drips again
Dilute sulfuric acidTill the proper dissolving of precipitation, add the acetic acid of PH6.0-ammonium acetate buffer 10ml, precision adds the Calcium Disodium Versenate vs 25ml of 0.05mol/L again, boil 3min, let cool, add xylenol orange indicator solution 1ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3Calculate Al in the test sample
2O
3Content is 76.0mg
/ g
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 750 ℃ of lower blazing 2.5h, lets cool, and is accurately weighed; With the residue water-wet, add 6 in hydrofluorite 6ml and sulfuric acid again, evaporate to dryness at 750 ℃ of lower blazing 6min, lets cool, and is accurately weighed, calculates SiO in the test sample
2Content is 302.5mg/g.
Embodiment 2
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Methanol-water solution take volume ratio as 0.3:0.7 is mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: get the Bergenin reference substance, accurately weighed, add 99.0% methyl alcohol and make the solution that every 1ml contains 0.15mg; The preparation of need testing solution: get tablet porphyrize content 1.0g, accurately weighed is 1.0002g, to the 50ml measuring bottle, add the ultrasonic processing of 99.0% methyl alcohol 11min, let cool, add 99.0% methyl alcohol to scale, shake up, filter by 0.45 μ m teflon membrane filter, getting subsequent filtrate is need testing solution; Determination method: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculating the Determination of Bergenin result is 9.12mg/g.
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get the content 2g of tablet porphyrize, accurately weighed is 1.9997g, puts in the porcelain dish, adds respectively sulfuric acid 4ml and nitric acid 8ml, treats effect fully, extremely
Water-bathUpper evaporate to dryness lets cool, and adds dilute sulfuric acid 30ml, boils, and upper strata liquid filters through ashless filter paper with decantation, and with hot wash 3 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper, uses hot wash with decantation, and residue is for subsequent use; Filtrate merges, and puts in the 100ml measuring bottle, lets cool, add water to scale, shake up, precision is measured 20ml, the adding citric acid sodium solution drips watery hydrochloric acid again and extremely precipitates till the just dissolving to just separating out precipitation, adds the phosphate buffer 10ml of PH6.0, the accurate Calcium Disodium Versenate vs 25ml that adds 0.05mol/L boils 5min again, lets cool, add xylenol orange indicator solution 1ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3Calculate Al in the test sample
2O
3Content is 68.8mg/g.
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 850 ℃ of lower blazing 1.5h, lets cool, and is accurately weighed; With the residue water-wet, add 8 in hydrofluorite 8ml and sulfuric acid again, evaporate to dryness at 850 ℃ of lower blazing 4min, lets cool, and is accurately weighed, calculates SiO in the test sample
2Content is 269.4mg/g.
Embodiment 3
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Methanol-water solution take volume ratio as 0.25.:075 is mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: it is an amount of to get the Bergenin reference substance, accurately weighed, adds 99.9% methyl alcohol and makes the solution that every 1ml contains 0.1mg; The preparation of need testing solution: get the content 1.5g in the capsule, accurately weighed 1.4999g is to the 50ml measuring bottle, add the ultrasonic processing of 99.9% methyl alcohol 10min, let cool, add 99.9% methyl alcohol to scale, shake up, filter by 0.50 μ m nylon leaching film, getting subsequent filtrate is need testing solution; Determination method: precision is drawn reference substance solution and each 8 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculating the Determination of Bergenin result is 11.56mg/g.
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get the content 2.5g in the capsule, accurately weighed is 2.5002g, puts in the porcelain dish, add respectively sulfuric acid 6ml and nitric acid 10ml, treat effect fully, evaporate to dryness to the sand bath, let cool, add dilute sulfuric acid 30ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 3 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper with decantation, use hot wash, residue is for subsequent use; Filtrate merges, and puts in the 100ml measuring bottle, lets cool, add water to scale, shake up, precision is measured 20ml, add malate solution to just separating out precipitation, drip again rare nitric acid to precipitation just till the dissolving, add the acetic acid of PH6.0-ammonium acetate buffer 10ml, the accurate Calcium Disodium Versenate vs 25ml that adds 0.05mol/L boils 4min again, lets cool, add xylenol orange indicator solution 1ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3Calculate Al in the test sample
2O
3Content is 82.4mg/g.
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 800 ℃ of lower blazing 2h, lets cool, and is accurately weighed; With the residue water-wet, add 7 in hydrofluorite 7ml and sulfuric acid again, evaporate to dryness at 800 ℃ of lower blazing 5min, lets cool, and is accurately weighed, calculates SiO in the test sample
2Content is 328.7mg/g.
Embodiment 4
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Methanol-water solution take volume ratio as 0.23:.0.77 is mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: get the Bergenin reference substance, accurately weighed, add 99.6% methyl alcohol and make the solution that every 1ml contains 0.1mg; The preparation of need testing solution: get granule content 0.8g, accurately weighed is 0.7989g, to the 50ml measuring bottle, add the ultrasonic processing of 99.6% methyl alcohol 10min, let cool, add 99.6% methyl alcohol to scale, shake up, filter by 0.45 μ m regenerated cellulose filter membrane, getting subsequent filtrate is need testing solution; Determination method: precision is drawn reference substance solution and each 6 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculating the Determination of Bergenin result is 11.18mg/g.
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get granule content 2g, accurately weighed is 2.0011g, puts in the porcelain dish, add respectively sulfuric acid 5ml and nitric acid 9ml, treat effect fully, evaporate to dryness to the water-bath, let cool, add dilute sulfuric acid 30ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 3 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper with decantation, use hot wash, residue is for subsequent use; Filtrate merges, and puts in the 100ml measuring bottle, lets cool, add water to scale, shake up, precision is measured 20ml, add sodium phenate solution to just separating out precipitation, drip again dilute sulfuric acid and extremely precipitate till the just dissolving, add the phosphate buffer 10ml of PH6.0, the accurate Calcium Disodium Versenate vs 25ml that adds 0.05mol/L boils 5min again, lets cool, add xylenol orange indicator solution 1ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3Calculate Al in the test sample
2O
3Content is 80.3 mg/g.
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 820 ℃ of lower blazing 1.9h, lets cool, and is accurately weighed; With the residue water-wet, add 6 in hydrofluorite 8ml and sulfuric acid again, evaporate to dryness at 820 ℃ of lower blazing 5min, lets cool, and is accurately weighed, calculates SiO in the test sample
2Content is 339.7mg/g.
Embodiment 5
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Methanol-water solution take volume ratio as 0.25:.075 is mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: get the Bergenin reference substance, accurately weighed, add 99.9% methyl alcohol and make the solution that every 1ml contains 0.1mg; The preparation of need testing solution: get the content 1.1g of pill porphyrize, accurately weighed is 1.1003g, to the 50ml measuring bottle, add the ultrasonic processing of 99.9% methyl alcohol 10min, let cool, add 99.9% methyl alcohol to scale, shake up, filter by 0.50 μ m teflon membrane filter, getting subsequent filtrate is need testing solution; Determination method: precision is drawn reference substance solution and each 7 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculating the Determination of Bergenin result is 9.36mg/g.
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get the content 2.3g of pill porphyrize, accurately weighed is 2.2997g, puts in the porcelain dish, add respectively sulfuric acid 7ml and nitric acid 11ml, treat effect fully, evaporate to dryness to the water-bath, let cool, add dilute sulfuric acid 30ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 3 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper with decantation, use hot wash, residue is for subsequent use; Filtrate merges, and puts in the 100ml measuring bottle, lets cool, add water to scale, shake up, precision is measured 20ml, add ammonia solution to just separating out precipitation, drip again dilute sulfuric acid to precipitation just till the dissolving, add the acetic acid of PH6.0-ammonium acetate buffer 10ml, the accurate Calcium Disodium Versenate vs 25ml that adds 0.05mol/L boils 3min again, lets cool, add xylenol orange indicator solution 1ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3Calculate Al in the test sample
2O
3Content is 68.6mg/g.
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 790 ℃ of lower blazing 2h, lets cool, and is accurately weighed; With the residue water-wet, add 8 in hydrofluorite 8ml and sulfuric acid again, evaporate to dryness at 790 ℃ of lower blazing 6min, lets cool, and is accurately weighed, calculates SiO in the test sample
2Content is 279.5mg/g.
Experimental example 1: utilize HPLC to Determination of Bergenin method for measuring research in the relieving diarrhea with astringents pharmaceutical preparation
(1) main material and instrument
1, the loose sample of relieving diarrhea with astringents: Yunnan Shi Purui bioengineering company limited, lot number: C0711001, C0711002, C0711007, C0711010, C0711012, C0711016, C0711024, C0711027, C0711030, C0711046
2, Bergenin standard items: Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides, lot number: 111532-200202.
3, methyl alcohol: Tianjin chemical reagent three factories, analyze pure.
4, methyl alcohol: U.S. J.T.Baker, chromatographically pure.
5, ultraviolet-visible pectrophotometer: Australian GBC company, UV/VIS 916 types.
6, high performance liquid chromatograph: U.S. Agilent company, Agilent 1100 types.
7, electronic balance: U.S. METTLER company, AES260 type (100,000/).
(2) method and result
1, the HPLC method is measured the assay method of Determination of Bergenin in the preparation
Chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Take water-methanol (75:25) as mobile phase; Detect wavelength 275nm.Theoretical pedal number calculates by the Bergenin peak and is not less than 2000.
The preparation of reference substance solution: get the about 50mg of Bergenin standard items, accurately weighed, place the 50ml volumetric flask, add the methyl alcohol dissolving and be diluted to scale, shake up, precision is measured 5ml, places the 50ml volumetric flask, adds methyl alcohol to scale, shakes up, and get final product.
The preparation of test sample: precision takes by weighing the about 0.5g of sample, places the 50ml volumetric flask, and it is an amount of to add methyl alcohol, ultrasonic processing (power 250W, frequency 40kHz) 10 minutes, and the cooling constant volume shakes up, and 0.45 μ m aperture miillpore filter filters, and get final product.
Determination method: precision is drawn reference substance solution and need testing solution 5～10 μ l injection liquid chromatographies respectively, measures, and get final product.
2, linearity
Chromatographic condition and system suitability test: be filling agent with octadecylsilane chemically bonded silica; Take water-methanol (75:25) as mobile phase; Detect wavelength 275nm.Theoretical pedal number calculates by the Bergenin peak and is not less than 2000.
Precision takes by weighing Bergenin standard items 50mg, makes with methyl alcohol to be dissolved in the 50ml volumetric flask as storing solution.Precision is measured 2.5ml, 4ml, 5ml, 6ml, 7.5ml, 10ml in the 50ml volumetric flask, is diluted to scale with methyl alcohol respectively, shakes up, and tests by an appendix VI of 2005 editions pharmacopeia D high performance liquid chromatography.The results are shown in Table 1.
Table 1 linear test result
Related coefficient is: 0.99996; Regression equation and linear graph be as shown in Figure 1:
Conclusion: Linear Experiment related coefficient 0.99996, linear dependence is good, satisfies standard-required.
3, accuracy
Get this product of known content, precision takes by weighing in right amount (being equivalent to approximately contain Bergenin 5mg) 9 parts respectively, presses the standard of average recovery determination method, adds an amount of Bergenin standard items, presses method mensuration under the assay item, calculates.The results are shown in Table 2.
Table 2 accuracy test result
Conclusion: the accuracy test of this product, average recovery rate are 99.06%, RSD=2.35% (n=9), and accuracy meets the requirements.
4, precision
4.1 repeatability
Get same duplicate samples, press under the assay item method replication 6 times, calculate.The results are shown in Table 3.
Table 3 replica test result
Conclusion: the repeated RSD=0.78%(n=6 of this product), replica test meets the requirements.
4.2 middle precision
Get same duplicate samples, press method under the assay item, at different time, by different analyst's replications 6 times, calculate.The results are shown in Table 4.
Precision test result in the middle of the table 4
Conclusion: the middle precision RSD of this product=1.04%(n=12), middle precision test meets the requirements.
5, negative control
The negative control that does not contain Bergenin by the preparation prescription preparation is a, measures according to method under the assay item, and negative control is noiseless.
6, peak purity experiment
By adjusting the mobile phase ratio, reduce the ratio of methyl alcohol in the mobile phase so that appearance time is passed backward, whether examination exists assorted peak, and whether main peak purity reaches purity requirement.
Conclusion: the peak purity experiment exam meets the requirements, and the sample peak purity reaches requirement.
7, ten batch samples are measured
Get that 10 batches of relieving diarrhea with astringents are loose to keep sample, press the HPLC method and measure, the every batch of mensuration 2 times.The results are shown in Table 5.
Table 50 batch sample assay results
Conclusion: the assay result of 10 batch samples is all up to specification: greater than the 40mg/ bag.
7, conclusion
In sum, the Determination of Bergenin assay method empirical tests result of revision is:
7.1 linear test: linearly dependent coefficient is 0.99996, meets the requirements.
7.2 accuracy test: average recovery rate is 99.06%, RSD=2.35%(n=9), meets the requirements.
7.3 precision test: repeated RSD=0.78%(n=6), middle precision RSD=1.04%(n=12), meet the requirements.
7.4 negative control is noiseless.
7.5 10 batch sample assay results are all greater than the 40mg/ bag.
Therefore, the Determination of Bergenin assay method empirical tests of revision is feasible.
8, high-efficient liquid phase technique, ultraviolet spectrophotometry detect result's contrast of Determination of Bergenin in the preparation
8.1 ultraviolet spectrophotometry:
Get this product 0.5g under the content uniformity item, accurately weighed, add methyl alcohol and stir extraction 2 times, each 10ml stirred 30 minutes, filter, merging filtrate in the dislocation 25ml measuring bottle, adds methyl alcohol and is diluted to scale, shakes up, precision is measured 2ml, puts in the 25ml measuring bottle, adds methyl alcohol to scale, shakes up.According to spectrophotometric method (an appendix V of Chinese Pharmacopoeia version in 2005 Α), measure absorbance log at 275nm wavelength place, press Bergenin (C
14H
16O
9) absorption coefficient (E
1cm 1%) be 248 calculating, and get final product.
8.2 high-efficient liquid phase technique:
Measure according to high performance liquid chromatography (an appendix IV of Chinese Pharmacopoeia version in 2005 D).
The preparation of chromatographic condition and system suitability, reference substance solution, the preparation that supplies test, determination method are by the 1st execution in " method and result ".
8.3 the recovery contrast situation of two kinds of method testing results sees table 6 for details.
Get this product of known content, precision takes by weighing in right amount (being equivalent to approximately contain Bergenin 5mg) 6 parts respectively, presses the standard of average recovery determination method, adds an amount of Bergenin standard items, presses method mensuration under the assay item, calculates.The results are shown in Table 6.
Table 6 high-efficient liquid phase technique, ultraviolet spectrophotometry testing result and recovery contrast
The result shows: the average recovery rate of ultraviolet spectrophotometry testing result is that 85.58%, RSD is 3.21%, and the average recovery rate of high-efficient liquid phase technique testing result is that 98.43%, RSD is 1.54%, illustrates that the high-efficient liquid phase technique accuracy is high than ultraviolet spectrophotometry.
Experimental example 2: the methodological study of the assay of alundum (Al2O3), silicon dioxide in the relieving diarrhea with astringents pharmaceutical preparation
(1) main material and instrument
1, the loose sample of relieving diarrhea with astringents: Yunnan Shi Purui bioengineering company limited, lot number: C0711001, C0711002, C0711007, C0711010, C0711012, C0711016, C0711024, C0711027, C0711030, C0711046
2, silicon dioxide (high purity reagent 〉=99.99%): Chemical Reagent Co., Ltd., Sinopharm Group
3, alundum (Al2O3) (high purity reagent 〉=99.99%): Chemical Reagent Co., Ltd., Sinopharm Group
4, electronic balance: U.S. METTLER company, AES260 type (100,000/).
(2) silicon dioxide content test method and result
1, silicon dioxide content test method
Get this product 1.0g under the content uniformity item, accurately weighed, put in the porcelain dish, add respectively sulfuric acid 6 ml and nitric acid 10 ml, the effect for the treatment of fully, is put evaporate to dryness in the sand bath, let cool, add dilute sulfuric acid 30 ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 3 times, washing lotion filters residue in the lump, at last with on the residue dislocation filter paper with decantation, use hot wash, residue silicon dioxide to be done is used; Filtrate merges, and places 100 ml measuring bottles, lets cool to room temperature, and thin up shakes up to scale; Precision is measured 20 ml, adding ammonia solution is neutralized to and just separates out precipitation, drip dilute sulfuric acid to precipitation just till the dissolving again, add acetic acid-ammonium acetate buffer (PH6.0) 10 ml, precision adds Calcium Disodium Versenate vs (25 ml of 0.05mol/L) again, boiled 3 ~ 5 minutes, let cool to room temperature, add xylenol orange indicator solution 1 ml, with zinc vs (0.05mol/L) titration, change redness into from yellow to solution, and titration results is proofreaied and correct with blank test.(0.05mol/L) is the Al of 2.546mg quite for the Calcium Disodium Versenate vs of every 1ml
2O
3
2, accuracy
Get this product of known content, precision takes by weighing in right amount (being equivalent to approximately contain silicon dioxide 0.3g) 9 parts respectively, presses the average recovery determination method, adds an amount of silicon dioxide standard items, presses method mensuration under the assay item, calculates.The results are shown in Table 1.
Table 1 accuracy test result (silicon dioxide)
Conclusion: the accuracy test of this product, average recovery rate are 99.94%, RSD=1.62% (n=9), and accuracy meets the requirements.
3, precision
3.1 repeatability
Get same duplicate samples, press under the assay item method replication 6 times, calculate.The results are shown in Table 2.
Table
2Replica test result (silicon dioxide)
Conclusion: the standard deviation 0.0208 of this product replica test, relative standard deviation RSD=1.38%(n=6), replica test meets the requirements.
3.2 middle precision
Get same duplicate samples, press method under the assay item, at different time, by different analyst's replications 6 times, calculate.The results are shown in Table 3.
Table
3Middle Precision test result (silicon dioxide)
Conclusion: the standard deviation 0.0171 of precision test in the middle of this product, relative standard deviation RSD=1.12%(n=12), middle precision test meets the requirements.
4, negative control
Get 6 parts in not silica containing negative control sample, test by content assaying method.The results are shown in Table 4.
Table
4Negative control test findings (silicon dioxide)
| Sample number | Sample size (g) | Mensuration contains silica volume (g/ bag) |
| 1 | 1.1521 | 0 |
| 2 | 1.1215 | 0 |
| 3 | 0.9793 | 0 |
| 4 | 0.9641 | 0 |
| 5 | 1.1095 | 0 |
| 6 | 0.9758 | 0 |
5, ten batch samples are measured
Get that 10 batches of relieving diarrhea with astringents are loose to keep sample, press method under the assay item, the every batch of mensuration 2 times.The results are shown in Table 5.
Table
5Ten batch sample assay results (silicon dioxide)
Conclusion: the assay result of 10 batch samples is all up to specification: greater than the 1.5g/ bag.
6, conclusion
In sum, newly-increased silicon dioxide content test method, empirical tests result is:
6.1 accuracy test: average recovery rate is 99.48%, RSD=1.95%(n=9), meets the requirements.
6.2 precision test: repeatability standard deviation 0.0208, relative standard deviation RSD=1.38%; Middle precision standard deviation 0.0171, relative standard deviation RSD=1.12%(n=12), meet the requirements.
6.3 negative control is noiseless.
6.4 10 batch sample assay results are all greater than the 1.5g/ bag.
Conclusion, newly-increased silicon dioxide content test method empirical tests is feasible.
(3) alundum (Al2O3) content assaying method and result
1, alundum (Al2O3) content assaying method
Get silicon dioxide and measure residual residue and place platinum alloy crucible together with filter paper, drying was descended blazing 2 hours at 800 ℃, let cool, and is accurately weighed.With the residue water-wet, add 7 in hydrofluorite 7ml and sulfuric acid again, evaporate to dryness, blazing 5 minutes, let cool, accurately weighed, subtract the weight of mistake, be and contain SiO in the test sample
2Weight.
2, accuracy
Get this product of known content, precision takes by weighing in right amount (being equivalent to approximately contain alundum (Al2O3) 60mg) 9 parts respectively, presses the standard of average recovery determination method, adds an amount of alundum (Al2O3) standard items, presses method mensuration under the assay item, calculates.The results are shown in Table 6.
Table
6Accuracy test result (alundum (Al2O3))
Conclusion: the accuracy test of this product, average recovery rate are 99.93%, RSD=1.39% (n=9), and accuracy meets the requirements.
3, precision
3.1 repeatability
Get same duplicate samples, press under the assay item method replication 6 times, calculate.The results are shown in Table 7.
Table
7Replica test result (alundum (Al2O3))
Conclusion: the standard deviation 0.0061 of this product replica test, relative standard deviation RSD=1.70%(n=6), replica test meets the requirements.
3.2 middle precision
Get same duplicate samples, press method under the assay item, at different time, by different analyst's replications 6 times, calculate.The results are shown in Table 8.
Table
8Middle Precision test result (alundum (Al2O3))
Conclusion: the standard deviation of precision is 0.053 in the middle of this product, relative standard deviation RSD=1.46%(n=12), middle precision test meets the requirements.
4, negative control
Get 6 parts in the negative control sample that does not contain alundum (Al2O3), test by content assaying method.The results are shown in Table 9.
Table
9Negative control test findings (alundum (Al2O3))
| Sample number | Sample size (g) | Mensuration contains alundum (Al2O3) amount (g/g) |
| 1 | 1.0582 | 0 |
| 2 | 0.9715 | 0 |
| 3 | 1.0754 | 0 |
| 4 | 0.9628 | 0 |
| 5 | 1.0194 | 0 |
| 6 | 1.0762 | 0 |
5, ten batch samples are measured
Get that 10 batches of relieving diarrhea with astringents are loose to keep sample, press method under the assay item, the every batch of mensuration 2 times.The results are shown in Table 10.
Table
10Ten batch sample assay results (alundum (Al2O3))
Conclusion: the assay result of 10 batch samples is all up to specification: greater than the 0.3g/ bag.
6, conclusion
Through test, newly-increased alundum (Al2O3) content assaying method, empirical tests result is:
6.1 accuracy test: average recovery rate is 99.63%, RSD=2.04% (n=9), and accuracy meets the requirements.
6.2 precision test: the replica test standard deviation is 0.0061, relative standard deviation RSD=1.70%(n=6); Middle precision standard deviation is 0.0053, relative standard deviation RSD=1.46%(n=12), meet the requirements.
6.3 negative control is noiseless.
6.4 10 batch sample assay results are all greater than the 0.3g/ bag.
Conclusion, newly-increased alundum (Al2O3) content assaying method satisfies testing requirement through the methodology checking.
Through experimental study, this assay method accuracy test, precision test, specificity test, linear test all meet the requirement of state-promulgated pharmacopoeia relevant regulations, and this method of inspection can satisfy the corresponding requirements of assay.Can be applicable to the oral solid formulation that the relieving diarrhea with astringents prescription+the adaptation auxiliary material is made, comprise the quality control of the formulations such as powder, particle, capsule, tablet, pill.
Claims (10)
1. the method for quality control of a relieving diarrhea with astringents pharmaceutical preparation, described relieving diarrhea with astringents pharmaceutical preparation is comprised of Rhizoma Rodgersiae extract 7 ~ 18 weight portions, bentonitic clay 700 ~ 800 weight portions and proper auxiliary materials, it is characterized in that described relieving diarrhea with astringents pharmaceutical preparation method of quality control comprises:
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Take methanol-water solution as mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: accurately weighed Bergenin reference substance adds methyl alcohol and makes the solution that every 1ml contains 0.05 ~ 0.15mg; The preparation of need testing solution: get the content 0. 5 ~ 1.5g in the preparation, accurately weighed, to the 50ml measuring bottle, add the ultrasonic processing 7 ~ 13min of methyl alcohol, let cool, add methyl alcohol to scale, shake up, filter, get subsequent filtrate as need testing solution; Determination method: precision is drawn reference substance solution and each 5 ~ 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculates Determination of Bergenin in the described relieving diarrhea with astringents pharmaceutical preparation;
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get the content 1 ~ 3g in the preparation, accurately weighed, put in the porcelain dish, add respectively sulfuric acid 4 ~ 8ml and nitric acid 8 ~ 12ml, treat effect fully, evaporate to dryness, let cool, add dilute sulfuric acid 20 ~ 40ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 2 ~ 5 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper with decantation, use hot wash, residue is for subsequent use; Filtrate merges, put in the 100ml measuring bottle, let cool, add water to scale, shake up, precision is measured 20ml, adds the alkalescent test solution to just separating out precipitation, drips the low concentration mineral acid again and extremely precipitates till the just dissolving, damping fluid 5 ~ the 15ml that adds pH6.0, the accurate Calcium Disodium Versenate vs 20 ~ 30ml that adds 0.05mol/L boils 3 ~ 5min again, lets cool, add xylenol orange indicator solution 0.5 ~ 2.5ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3, calculate the Al in the described relieving diarrhea with astringents pharmaceutical preparation
2O
3Content;
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 750 ~ 850 ℃ of lower blazing 1.5 ~ 2.5h, lets cool, and is accurately weighed; With the residue water-wet, add 5 ~ 9 in hydrofluorite 5 ~ 9ml and sulfuric acid again, evaporate to dryness at 750 ~ 850 ℃ of lower blazing 4 ~ 6min, lets cool, and is accurately weighed, subtracts the weight of mistake, is SiO in the described relieving diarrhea with astringents pharmaceutical preparation
2Content.
2. the method for quality control of relieving diarrhea with astringents pharmaceutical preparation according to claim 1 is characterized in that the method comprises:
The content of Bergenin in A, the high effective liquid chromatography for measuring said preparation: take octadecyl silane as filling agent; Take methanol-water solution as mobile phase; The detection wavelength is 275nm; Number of theoretical plate calculates by the Bergenin peak should be not less than 2000; The preparation of reference substance solution: accurately weighed Bergenin reference substance adds methyl alcohol and makes the solution that every 1ml contains 0.1mg; The preparation of need testing solution: get the content 0. 5 ~ 1.5g in the preparation, accurately weighed, to the 50ml measuring bottle, it is an amount of to add methyl alcohol, and ultrasonic processing 9 ~ 11min lets cool, and adds methyl alcohol to scale, shakes up, and filters, and gets subsequent filtrate as need testing solution; Determination method: precision is drawn reference substance solution and each 5 ~ 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and calculates Determination of Bergenin in the described relieving diarrhea with astringents pharmaceutical preparation;
Alundum (Al2O3) assay in B, the relieving diarrhea with astringents pharmaceutical preparation: get the content 1 ~ 3g in the preparation, accurately weighed, put in the porcelain dish, add respectively sulfuric acid 5 ~ 7ml and nitric acid 9 ~ 11ml, treat effect fully, evaporate to dryness, let cool, add dilute sulfuric acid 30ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 3 ~ 4 times, washing lotion filters residue in the lump, at last residue is moved on the filter paper with decantation, use hot wash, residue is for subsequent use; Filtrate merges, put in the 100ml measuring bottle, let cool, add water to scale, shake up, precision is measured 20ml, adds the alkalescent test solution to just separating out precipitation, drips the low concentration mineral acid again and extremely precipitates till the just dissolving, damping fluid 8 ~ the 12ml that adds pH6.0, the accurate Calcium Disodium Versenate vs 25ml that adds 0.05mol/L boils 3 ~ 5min again, lets cool, add xylenol orange indicator solution 0.5 ~ 1.5ml, with the zinc vs titration of 0.05mol/L, transfer redness to from yellow to solution, and titration results is proofreaied and correct with blank test; The Al of the suitable 2.546mg of Calcium Disodium Versenate vs of the 0.05mol/L of every 1ml
2O
3, calculate the Al in the described relieving diarrhea with astringents pharmaceutical preparation
2O
3Content;
Silicon dioxide content test in C, the relieving diarrhea with astringents pharmaceutical preparation: get residue for subsequent use in the B step, together with filter paper as in the platinum alloy crucible, drying, straight fiery carbonization at 750 ~ 850 ℃ of lower blazing 1.5 ~ 2.5h, lets cool, and is accurately weighed; With the residue water-wet, add 5 ~ 9 in hydrofluorite 5 ~ 9ml and sulfuric acid again, evaporate to dryness at 750 ~ 850 ℃ of lower blazing 4 ~ 6min, lets cool, and is accurately weighed, subtracts the weight of mistake, is SiO in the described relieving diarrhea with astringents pharmaceutical preparation
2Content.
3. the method for quality control of relieving diarrhea with astringents pharmaceutical preparation according to claim 1 and 2 is characterized in that the long-pending ratio of mobile phase methanol in the described A step-aqueous solution liquid is 0.2 ~ 0.3:0.7 ~ 0.8.
4. the method for quality control of relieving diarrhea with astringents pharmaceutical preparation according to claim 3 is characterized in that the long-pending ratio of described mobile phase methanol-aqueous solution liquid is 0.25:0.75.
5. the method for quality control of relieving diarrhea with astringents pharmaceutical preparation according to claim 1 and 2, it is characterized in that in the described A step filtering what use is miillpore filter, described miillpore filter is a kind of in teflon membrane filter, nylon leaching film, the regenerated cellulose filter membrane, and described filter membrane aperture is 0.4 ~ 0.50 μ m.
6. the method for quality control of relieving diarrhea with astringents pharmaceutical preparation according to claim 1 and 2 is characterized in that described methanol concentration is 99.0 ~ 99.9%.
7. the method for quality control of relieving diarrhea with astringents pharmaceutical preparation according to claim 1 and 2 is characterized in that described
BWhat the evaporate to dryness mode can be in sand bath evaporate to dryness, the water bath method in the step is a kind of.
8. the method for quality control of relieving diarrhea with astringents pharmaceutical preparation according to claim 1 and 2, what it is characterized in that buffer solution in the described B step can be in acetic acid-ammonium acetate buffer or the phosphate buffer is a kind of.
9. the method for quality control of relieving diarrhea with astringents pharmaceutical preparation according to claim 1 and 2, what it is characterized in that alkalescent test solution in the described B step can be in ammonia solution, sodium citrate, malate, the sodium phenate solution is a kind of, and what described low concentration mineral acid can be in dilute sulfuric acid, watery hydrochloric acid or the rare nitric acid is a kind of.
10. the method for quality control of relieving diarrhea with astringents pharmaceutical preparation according to claim 1 and 2 is characterized in that described preparation formulation is tablet, powder, granule, capsule or pill.
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| CN105454288A (en) * | 2016-01-11 | 2016-04-06 | 济南康众医药科技开发有限公司 | Pesticide prepared from montmorillonite and used for preventing and controlling crop diseases |
| CN105454287A (en) * | 2016-01-11 | 2016-04-06 | 济南康众医药科技开发有限公司 | Pesticide prepared from montmorillonite and using method thereof |
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