CN102735791A - Quality detection method for antifungal cream - Google Patents

Quality detection method for antifungal cream Download PDF

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CN102735791A
CN102735791A CN2012102494914A CN201210249491A CN102735791A CN 102735791 A CN102735791 A CN 102735791A CN 2012102494914 A CN2012102494914 A CN 2012102494914A CN 201210249491 A CN201210249491 A CN 201210249491A CN 102735791 A CN102735791 A CN 102735791A
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peaceful
skin
econazole nitrate
emulsifiable paste
solvent
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胡荣
张倩
冯华
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Third Military Medical University TMMU
First Affiliated Hospital of TMMU
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First Affiliated Hospital of TMMU
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Abstract

The invention relates to a quality detection method for Funing cream. The method comprises two steps: identification of antifungal active ingredient econazole nitrate and determination of econazole nitrate content, wherein the determination of antifungal active ingredient econazole nitrate by third derivative spectrometry comprises the steps of firstly separating and extracting econazole nitrate in the Funing cream: precisely weighing 1g of Funing cream to be determined, adding 15ml solvent, wherein the solvent is prepared by mixing 0.1mol/L HCL and methanol according to the volume ratio of 1:9, heating in water bath at 80 DEG C, stirring to be clear, cooling in a refrigerator to be lower than room temperature, filtering and washing for three times with 10ml solvent per time, combining filtrates, adding into a 50ml volumetric flask, adding the solvent for diluting to achieve the scale, shaking up, precisely weighing 2.5ml of diluent, adding into 25ml volumetric flask, adding the solvent to achieve the scale, and shaking up; secondly, determining the econazole nitrate content by adopting the third derivative method at 231nm through an ultraviolet and visible spectrophotometer. The detection method is accurate, good in specificity and repeatability, convenient to operate and low in cost.

Description

A kind of quality determining method of antimycotic emulsifiable paste
Technical field
The present invention relates to a kind of quality determining method of cream preparation, be specifically related to a kind of quality determining method of antimycotic emulsifiable paste.
Background technology
Because mostly skin infection is fungal infection, often merges bacterial infection [1], list is difficult to reach result of treatment with a kind of antifungal drug.Often select antifungal econazole nitrate and aminoglycosides microbiotic, gentamicin sulphate for use for the infection of skin at present according to these characteristics, and the peaceful emulsifiable paste of skin of hormone dexamethasone sodium phosphate compatibility, be used for diseases such as neurodermatitis, skin itching.Ning prescription skin cream: econazole 10g, gentamicin sulfate 10g, dexamethasone sodium phosphate 0.6g, A liquid (stearic acid 60g, Span 6016g, octadecanol 60g, liquid paraffin 90g, white Vaseline 60g), B solution (polysorbate resin 8044g, glycerin 100g, sorbic acid 2g, add distilled water to 1000g.), the A, B and two solutions were heated to about 80 ℃ water bath, the stirring solution was slowly added methyl acetate liquid, stirring plus side, Yun removed after mixing, stirring was continued cooled to about about 50 ℃ proportion to the econazole nitrate, sulfate, gentamicin, dexamethasone sodium phosphate was added thereto, and stirring was continued to the condensate, namely obtained.The peaceful emulsifiable paste of a plurality of manufacturer production skins is arranged, but the peaceful emulsifiable paste of skin applies to clinical antifungal drug as a kind of, need to formulate truly feasible method of quality control to guarantee product quality and clinical efficacy.
Utilize the principle and the experimental technique of spectroscopy to be called spectrographic method with structure and the chemical composition analysis method of confirming material.The material of various structures all has the characteristic spectrum of oneself, and spectrographic method is exactly the method for utilizing the characteristic spectrum research structure of matter or measuring chemical constitution.The ultraviolet-visible absorption spectroscopy method is the absorption spectrum in the research molecule absorption 190-750nm wavelength coverage.Ultraviolet-visible absorption spectroscopy mainly results from the transition of valence electron between electron level in the molecule; It is the analytical approach of research material electronic spectrum; Through measuring the absorption of molecule, can identify and measure a large amount of mineral compounds and organic compound to ultraviolet-visible.The molecular absorption spectrum that the material absorbing wavelength coverage produces at the interval electromagnetic radiation energy of 200~760nm is called ultraviolet---the visible absorption spectra of this material,---method qualitative, quantitative test that visible absorption spectra is carried out material is called ultraviolet---visible spectrophotometry of utilizing ultraviolet.Derivative spectrophotometry is common absorption spectrum to be carried out differential handle, and whenever (be generally the value that 1~2nm) pointwise calculates △ A/ △ λ, draw △ A/ △ λ~λ curve, the figure that obtains is exactly a first derivative spectrum at a distance from a closely-spaced △ λ of wavelength.Can obtain the derivative spectrum of higher order successively.Along with increasing of derivative exponent number, peak number increases, and peak width narrows down, and resolution characteristic improves, and helps the separation and the discriminating of overlapping bands of a spectrum and acromion.The interference that utilizes derivative spectrophotometry can eliminate the coexistence component absorbs the sensitivity that also can improve mensuration.At present, utilize the spectrophotometer that has microprocessor can calculate and directly depict derivative spectrums such as single order, second order, three rank, quadravalence automatically.
The multipurpose efficient of drug quality control at present liquid phase HPLC, but HPLC costs an arm and a leg, the maintenance difficulty, with respect to HPLC, the ultraviolet spectrometer (UVS) low price, simple to operate.At present, still there is not the non-HPLC method that in emulsifiable paste, detects complicated drug ingedients such as econazole nitrate.
Summary of the invention
The object of the invention is to provide the quality determining method of the peaceful emulsifiable paste of a kind of antifungal drug skin, and this method is easy and simple to handle, cost is low, can effectively guarantee quality and antimycotic clinical efficacy thereof of the peaceful emulsifiable paste of skin.
The present invention seeks to realize through following technical measures:
The quality determining method of the peaceful emulsifiable paste of a kind of skin comprises discriminating and Determination on content thereof to antimycotic effective constituent econazole nitrate, it is characterized in that: tlc identification method is adopted in the discriminating to said econazole nitrate, specifically is to get the peaceful emulsifiable paste 2g of skin to be measured; Methyl alcohol 20ml, 80 ℃ of heated and stirred of water-bath, ice bath cooling; Filter, the filtrating evaporate to dryness adds the 2ml dissolve with methanol as test liquid; Precision takes by weighing 20mg econazole nitrate sample, and the 2ml dissolve with methanol is obtained the 5ul point in silica gel plate as contrast liquid; Ether launches, and the iodine vapor colour developing compares;
Said is to adopt three rank spectroscopic methodologies reciprocal to the econazole nitrate Determination on content, the econazole nitrate in the peaceful emulsifiable paste of separation and Extraction skin at first, and precision takes by weighing the about 1g of the peaceful emulsifiable paste of skin to be measured; Add the 15ml solvent, said solvent is mixed with volume ratio 1:9 by HCL and the methyl alcohol of 0.1mol/L, and 80 ℃ of heated and stirred of water-bath are to clarification; Put refrigerator and cooled but to be lower than room temperature filtration, washing three times, use the said solvent of 10ml at every turn, merging filtrate adds said solvent dilution to scale to the 50ml volumetric flask; Shake up; Precision is measured said dilution 2.5ml in the 25ml volumetric flask, and solubilizer shakes up to scale; Next adopts ultraviolet-visible pectrophotometer, measures econazole nitrate content at the 231nm place with three order derivative methods.
The quality determining method of the peaceful emulsifiable paste of above-mentioned skin also comprises to be differentiated antibacterium effective constituent gentamicin sulphate; Specifically be to get the peaceful emulsifiable paste 0.5g of skin to be measured (sulfur acid gentamicin 5mg) to add water 10ml dissolving; The boiling water bath breakdown of emulsion; The water-saturated n-butanol solution 1ml and the pyridine 0.5ml that add 0.1wt% (mass percent concentration) triketohydrindene hydrate while hot, 100 ℃ of water-bath heating 5min develop the color.
The quality determining method of the peaceful emulsifiable paste of above-mentioned skin also comprises to be differentiated the dexamethasone sodium phosphate; Specifically be to get the peaceful emulsifiable paste 10g of skin to be measured (containing dexamethasone sodium phosphate 6mg); Add 10ml methyl alcohol, 80 ℃ of water-bath dissolvings, filtered while hot; The Rotary Evaporators evaporate to dryness is used in filtrating cooling back, develops the color in the residue adding 1ml sulfuric acid.
Specifically, the quality determining method of the peaceful emulsifiable paste of a kind of skin is discriminating and the Determination on content thereof to antimycotic effective constituent econazole nitrate, antibacterium effective constituent gentamicin sulphate is differentiated, and dexamethasone sodium phosphate composition is differentiated; It is characterized in that: tlc identification method is adopted in the discriminating to said econazole nitrate, specifically is to get the peaceful emulsifiable paste 2g of skin to be measured, methyl alcohol 20ml, 80 ℃ of heated and stirred of water-bath; The ice bath cooling is filtered, and the filtrating evaporate to dryness adds the 2ml dissolve with methanol as test liquid; Precision takes by weighing 20mg econazole nitrate sample, and the 2ml dissolve with methanol is obtained the 5ul point in silica gel plate as contrast liquid; Ether launches, and the iodine vapor colour developing compares; Said is to adopt three rank spectroscopic methodologies reciprocal to the econazole nitrate Determination on content, the econazole nitrate in the peaceful emulsifiable paste of separation and Extraction skin at first, and precision takes by weighing the about 1g of the peaceful emulsifiable paste of skin to be measured; Add the 15ml solvent, said solvent is mixed with volume ratio 1:9 by HCL and the methyl alcohol of 0.1mol/L, and 80 ℃ of heated and stirred of water-bath are to clarification; Put refrigerator and cooled but to be lower than room temperature filtration, washing three times, use the said solvent of 10ml at every turn, merging filtrate adds said solvent dilution to scale to the 50ml volumetric flask; Shake up; Precision is measured said dilution 2.5ml in the 25ml volumetric flask, and solubilizer shakes up to scale; Next adopts ultraviolet-visible pectrophotometer, measures econazole nitrate content at the 231nm place with three order derivative methods;
Gentamicin sulphate is differentiated; Specifically be to get the peaceful emulsifiable paste 0.5g of skin to be measured (sulfur acid gentamicin 5mg) to add water 10ml dissolving; The boiling water bath breakdown of emulsion; The water-saturated n-butanol solution 1ml and the pyridine 0.5ml that add 0.1wt% (mass percent concentration) triketohydrindene hydrate while hot, 100 ℃ of water-bath heating 5min develop the color;
Dexamethasone sodium phosphate is differentiated, specifically is to get the peaceful emulsifiable paste 10g of skin to be measured (containing dexamethasone sodium phosphate 6mg), adding 10ml methyl alcohol, and 80 ℃ of water-baths dissolvings, filtered while hot, the Rotary Evaporators evaporate to dryness is used in filtrating cooling back, develops the color in the residue adding 1ml sulfuric acid.
The present invention has following beneficial effect:
The quality determining method of the peaceful cream preparation of the antimycotic skin of the present invention is easy to operate, cost is low; It is easy, identified antimycotic effective constituent econazole nitrate and the content thereof in the preparation quickly; Especially, adopted econazole nitrate methyl alcohol as extracting solvent, fully having reduced the interference of impurity in the liquid to be measured in measuring; In ether, launch, effect is very good, the inclusion-free spot occurs.But in the econazole nitrate assay, adopt not only breakdown of emulsion but also can extract econazole nitrate of specific solvent.The detection method recovery of the present invention is high, and all more than 99 percent, average recovery rate is 100.3%, favorable reproducibility at every turn; Simultaneously high, the inventive method r=0.9999 of degree of accuracy is approximate 1, and to compare degree of accuracy suitable with the HPLC method.In a word, detection method of the present invention is accurate, specificity, good reproducibility, and easy to operate, cost is low, and the present invention provides a kind of easy alternative method for many school, hospital and small test chambers that do not have condition.
Description of drawings
Fig. 1 is a ultraviolet zeroth order spectrogram, the blank matrix of the peaceful emulsifiable paste c of a econazole nitrate b skin; Horizontal ordinate unit's wave number (nm) is respectively 200.0,220.0,240.0,260.0,280.0,300.0, and ordinate is an amplitude, is respectively-0.025,1.000,2.000,2.500.
Fig. 2 is econazole nitrate three order derivative spectrograms, the blank matrix of the peaceful emulsifiable paste c of a econazole nitrate b skin; Horizontal ordinate unit's wave number (nm) is respectively 200.0,220.0,240.0,260.0,280.0,300.0, and ordinate is the derivative of amplitude, is respectively-0.025 ,-0.020 ,-0.010,0.000,0.010,0.020,0.025.
Embodiment
Through embodiment the present invention is carried out concrete description below; Be necessary to be pointed out that at this following examples only are used for the present invention is further specified; Can not be interpreted as the restriction to protection domain of the present invention, the technician in this field can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
Embodiment 1
The quality determining method of the peaceful emulsifiable paste of a kind of skin, carry out according to the following steps:
(1) thin-layer chromatography is differentiated econazole nitrate: get the peaceful emulsifiable paste sample of skin 2g, methyl alcohol 20ml, 80 ℃ of heated and stirred of water-bath, ice bath cooling; Filter, the filtrating evaporate to dryness adds the 2ml dissolve with methanol as supplying examination; Precision takes by weighing 20mg econazole nitrate sample, and the 2ml dissolve with methanol is obtained the 5ul point in silica gel g plate as contrast liquid; Ether launches, the iodine vapor colour developing, and contrast liquid and test liquid principal spot are at same position;
(2) differentiate gentamicin sulphate: get the peaceful emulsifiable paste sample of skin 0.5g (being equivalent to gentamicin sulphate 5mg) and add water 10ml dissolving; The boiling water bath breakdown of emulsion; The water-saturated n-butanol solution 1ml and the pyridine 0.5ml that add the 0.1wt% triketohydrindene hydrate while hot, 100 ℃ of water-bath heating 5min, solution shows bluish violet;
(3) differentiate dexamethasone sodium phosphate: sample thief 10g (being equivalent to dexamethasone sodium phosphate 6mg), add 10ml methyl alcohol, 80 ℃ of water-bath dissolvings, filtered while hot, the Rotary Evaporators evaporate to dryness is used in filtrating cooling back, and residue adds 1ml sulfuric acid and shows brownish red.
(4) three rank spectroscopic methodology reciprocal is surveyed econazole nitrate content:
1. the preparation of solution
The preparation of need testing solution: precision takes by weighing the about 1g of sample, adds 15ml solvent (0.1mol/L HCL-methyl alcohol 1:9 is in volume ratio); 80 ℃ of heated and stirred of water-bath are put refrigerator and cooled and are but filtered, wash three times, each 10ml solvent to being lower than room temperature to clarification; Merging filtrate is to the 50ml volumetric flask, and solubilizer shakes up to scale; Precision is measured dilution 2.5ml in the 25ml volumetric flask, and solubilizer shakes up to scale.
The preparation of blank liquid: the blank sample solution that does not contain econazole nitrate by preparation method's preparation of above-mentioned need testing solution.
The preparation of reference substance solution: precision takes by weighing econazole nitrate 10.2mg, dissolves in accordance with the law and dilute as for 50ml volumetric flask with the solution of 0.1mol/L HCL-methyl alcohol 1:9 (volume ratio), and precision is measured the 2.5ml dilution to the 25ml volumetric flask.
2. spectrum condition and system suitability experiment
Instrument and reagent: UV-2501PC (day island proper Tianjin) analyzes pure methyl alcohol, normal butyl alcohol, hydrochloric acid.The peaceful emulsifiable paste of skin (production of new bridge hospital pharmacy).Econazole nitrate (lot number 030208, Xuzhou En Hua group).
3. assay
3.1 selection of experiment conditions
The preparation of test liquid: precision takes by weighing the about 1g of sample, adds 15ml solvent (0.1mol/L HCL-methyl alcohol 1:9), and 80 ℃ of heated and stirred of water-bath are to clarification; Put refrigerator and cooled and but filter, wash three times to being lower than room temperature, each 10ml solvent, merging filtrate is to the 50ml volumetric flask; Solubilizer shakes up to scale, and precision is measured dilution 2.5ml in the 25ml volumetric flask; Solubilizer shakes up to scale.
The preparation of contrast liquid: precision takes by weighing econazole nitrate 10.2mg, dissolves in accordance with the law and dilute as for 50ml volumetric flask with the solution of 0.1mol/L HCL-methyl alcohol 1:9, and precision is measured the 2.5ml dilution to the 25ml volumetric flask.
The preparation of blank solution: precision takes by weighing the about 1g of the emulsifiable paste that does not contain econazole nitrate, adds 15ml solvent (0.1mol/L HCL-methyl alcohol 1:9), and 80 ℃ of heated and stirred of water-bath and refrigerator and cooled are but to being lower than room temperature; Filter; Wash three times, each 10ml solvent, set room temperature is dissolved in the 50ml volumetric flask; Precision is measured the 2.5ml dilution in 25ml volumetric flask constant volume, shakes up.
3.2 measuring selection test liquid, contrast liquid, the blank solution of wavelength is blank with 0.1mol/L hydrochloric acid-methyl alcohol respectively, in the interscan of 300 ~ 200nm wavelength coverage, gets zeroth order, three rank spectrograms are seen Fig. 1, Fig. 2.Visible by Fig. 1, in the zeroth order ultraviolet spectrogram, blank matrix is disturbed bigger to the absorption of econazole nitrate.Econazole nitrate has peak swing to three order derivative spectrograms at the 231nm place, and blank matrix does not almost have amplitude, can get rid of the influence of blank matrix, therefore is selected in the 231nm place and surveys econazole nitrate content with three order derivative methods.
3.3 the drafting of typical curve
The smart econazole nitrate 10.2mg that is dried to constant weight that takes by weighing, the dissolving of 0.1mol/L hydrochloric acid-methyl alcohol (1:9) solution, constant volume is in the 50ml volumetric flask, and precision is measured dilution 1.5ml respectively; 2ml, 2.5ml, 3ml; 3.5ml constant volume is to the 25ml volumetric flask, making concentration is 12.24ug/ml; 16.32ug/ml, 20.4ug/m, 24.48ug/ml; 28.56ug/ml solution, measure three order derivative spectral amplitudes values at the 231nm place, concentration and three order derivative values have extraordinary linear dependence C=(D-0.00010)/0.000221 r=0.9999 to be similar to 1.
3.4 the mensuration of the recovery
Precision takes by weighing several parts of variable concentrations econazole nitrates, joins precision and takes by weighing among the blank emulsifiable paste 1g that does not contain econazole nitrate, after the cooling of heating mixing, is cooled to the emulsifiable paste moulding; Add 15ml solvent (0.1mol/L HCL-methyl alcohol 1:9), 80 ℃ of heated and stirred of water-bath are to clarification, take out to put refrigerator and cooled and but filter to room temperature; Wash three times (choose at every turn after the filtration matrix again the solubilizer breakdown of emulsion filter), each 10ml solvent, merging filtrate; Set room temperature is dissolved in the 50ml volumetric flask, precision measure the 2.5ml dilution in 25ml volumetric flask solubilizer to scale, shake up; Measure three order derivative spectrum 231nm place amplitudes, the substitution typical curve calculates content in accordance with the law, and the result sees table 1:
Table Spectazole determination of recovery rates result (n=3)
Figure BDA00001903625900071
3.5 sample determination
The peaceful emulsifiable paste of skin of three parts of different lot numbers of preparation, the finished product of each lot number is by the method detection level under the recovery item, and the result sees table 2:
Econazole nitrate assay result (n=2) in the peaceful emulsifiable paste of table 2 skin
Figure BDA00001903625900072
4 stability experiments
Select 45,50,55 ℃ of three temperature respectively,, only find that outward appearance does not change in the time of 45 ℃, therefore select 45 ℃ for measuring temperature respectively at sealing baking in the baking oven 10 hours.
In 45 ℃ of baking ovens, toast 0,4,8,12 respectively, 16 hours, record data were measured content, are respectively 100%, 98%, 95%, 93%, 93%, and stability is not good enough, and can not put for a long time summer.
4.1 in 55 ℃ of baking ovens, toasted 6 hours continuously, in 0 ℃ of refrigerator, to place for 1 week, the oil and water separation phenomenon does not appear.
4.2 2500 rev/mins of high speed centrifugations of hydro-extractor half an hour, emulsifiable paste does not separate, but the particle little rough.
Experiment shows, the peaceful emulsifiable paste of a certain amount of skin increase to reduce or increases the content of matrix and changes gentamicin sulphate, the amount of dexamethasone sodium phosphate, and peak value is constant basically, explains that this law can eliminate interference.Extract is more stable, places after 48 hours and is measuring wavelength survey absorption value, and absorption value does not have significant change, and the peaceful emulsifiable paste of skin to be measured can satisfy the requirement of hospital preparation.

Claims (4)

1. the quality determining method of the peaceful emulsifiable paste of skin comprises discriminating and Determination on content thereof to antimycotic effective constituent econazole nitrate, it is characterized in that: tlc identification method is adopted in the discriminating to said econazole nitrate, specifically is to get the peaceful emulsifiable paste 2g of skin to be measured; Methyl alcohol 20ml, 80 ℃ of heated and stirred of water-bath, ice bath cooling; Filter, the filtrating evaporate to dryness adds the 2ml dissolve with methanol as test liquid; Precision takes by weighing 20mg econazole nitrate sample, and the 2ml dissolve with methanol is obtained the 5ul point in silica gel plate as contrast liquid; Ether launches, and the iodine vapor colour developing compares;
Said is to adopt three rank spectroscopic methodologies reciprocal to the econazole nitrate Determination on content, the econazole nitrate in the peaceful emulsifiable paste of separation and Extraction skin at first, and precision takes by weighing the about 1g of the peaceful emulsifiable paste of skin to be measured; Add the 15ml solvent, said solvent is mixed with volume ratio 1:9 by HCL and the methyl alcohol of 0.1mol/L, and 80 ℃ of heated and stirred of water-bath are to clarification; Put refrigerator and cooled but to be lower than room temperature filtration, washing three times, use the said solvent of 10ml at every turn, merging filtrate adds said solvent dilution to scale to the 50ml volumetric flask; Shake up; Precision is measured said dilution 2.5ml in the 25ml volumetric flask, and solubilizer shakes up to scale; Next adopts ultraviolet-visible pectrophotometer, measures econazole nitrate content at the 231nm place with three order derivative methods.
2. the quality determining method of the peaceful emulsifiable paste of skin according to claim 1; It is characterized in that: said quality determining method also comprises the discriminating to antibacterium effective constituent gentamicin sulphate; Specifically be to get the peaceful emulsifiable paste 0.5g of skin to be measured to add water 10ml dissolving, the boiling water bath breakdown of emulsion adds the water-saturated n-butanol solution 1ml and the pyridine 0.5ml of 0.1wt% (mass percent concentration) triketohydrindene hydrate while hot; 100 ℃ of water-bath heating 5min develop the color.
3. the quality determining method of the peaceful emulsifiable paste of skin according to claim 1 or claim 2; It is characterized in that: said quality determining method also comprises to be differentiated the dexamethasone sodium phosphate, specifically is to get the peaceful emulsifiable paste 10g of skin to be measured (containing dexamethasone sodium phosphate 6mg), adds 10ml methyl alcohol; 80 ℃ of water-bath dissolvings; Filtered while hot, the Rotary Evaporators evaporate to dryness is used in filtrating cooling back, develops the color in the residue adding 1ml sulfuric acid.
4. the quality determining method of the peaceful emulsifiable paste of skin is discriminating and the Determination on content thereof to antimycotic effective constituent econazole nitrate, antibacterium effective constituent gentamicin sulphate is differentiated, and dexamethasone sodium phosphate composition is differentiated; It is characterized in that: tlc identification method is adopted in the discriminating to said econazole nitrate, specifically is to get the peaceful emulsifiable paste 2g of skin to be measured, methyl alcohol 20ml, 80 ℃ of heated and stirred of water-bath; The ice bath cooling is filtered, and the filtrating evaporate to dryness adds the 2ml dissolve with methanol as test liquid; Precision takes by weighing 20mg econazole nitrate sample, and the 2ml dissolve with methanol is obtained the 5ul point in silica gel plate as contrast liquid; Ether launches, and the iodine vapor colour developing compares; Said is to adopt three rank spectroscopic methodologies reciprocal to the econazole nitrate Determination on content, the econazole nitrate in the peaceful emulsifiable paste of separation and Extraction skin at first, and precision takes by weighing the about 1g of the peaceful emulsifiable paste of skin to be measured; Add the 15ml solvent, said solvent is mixed with volume ratio 1:9 by HCL and the methyl alcohol of 0.1mol/L, and 80 ℃ of heated and stirred of water-bath are to clarification; Put refrigerator and cooled but to be lower than room temperature filtration, washing three times, use the said solvent of 10ml at every turn, merging filtrate adds said solvent dilution to scale to the 50ml volumetric flask; Shake up; Precision is measured said dilution 2.5ml in the 25ml volumetric flask, and solubilizer shakes up to scale; Next adopts ultraviolet-visible pectrophotometer, measures econazole nitrate content at the 231nm place with three order derivative methods;
Gentamicin sulphate is differentiated; Specifically be to get the peaceful emulsifiable paste 0.5g of skin to be measured (sulfur acid gentamicin 5mg) to add water 10ml dissolving; The boiling water bath breakdown of emulsion; The water-saturated n-butanol solution 1ml and the pyridine 0.5ml that add 0.1wt% (mass percent concentration) triketohydrindene hydrate while hot, 100 ℃ of water-bath heating 5min develop the color;
Dexamethasone sodium phosphate is differentiated, specifically is to get the peaceful emulsifiable paste 10g of skin to be measured (containing dexamethasone sodium phosphate 6mg), adding 10ml methyl alcohol, and 80 ℃ of water-baths dissolvings, filtered while hot, the Rotary Evaporators evaporate to dryness is used in filtrating cooling back, develops the color in the residue adding 1ml sulfuric acid.
CN2012102494914A 2012-07-18 2012-07-18 Quality detection method for antifungal cream Pending CN102735791A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105136697A (en) * 2015-08-18 2015-12-09 安徽城市药业有限责任公司 Dexamethasone sodium phosphate injection intermediate testing method

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Application publication date: 20121017