CN1785219A - Quality control method of composite prepn. of dry mango tree leaves extract - Google Patents
Quality control method of composite prepn. of dry mango tree leaves extract Download PDFInfo
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- CN1785219A CN1785219A CN 200510125224 CN200510125224A CN1785219A CN 1785219 A CN1785219 A CN 1785219A CN 200510125224 CN200510125224 CN 200510125224 CN 200510125224 A CN200510125224 A CN 200510125224A CN 1785219 A CN1785219 A CN 1785219A
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Abstract
A compound medicine in the form of tablet, capsule or softgel is prepared from the dried extract of mango leaf, sodium houttuyfonate and chlorphenamine maleate. Its quality control method features that a thin-layer chromatography is used to identify said three components and an efficient liquid-phase chromatographe is used to measure their contents.
Description
Technical field
The present invention relates to a kind of method of quality control of Chinese and western drugs compound preparation, particularly relate to the new method of quality control of the tablet made with Folium mango dry extractum, Sodium Houttuyfonate and chlorphenamine maleate prescription, capsule, soft capsule.
Background technology
The Folium mango dry extractum compound preparation mainly is made up of Folium mango dry extractum, Sodium Houttuyfonate and chlorphenamine maleate, has the effect of dispersing lung-QI and dissipating phlegm, relieving cough and asthma.Be used for the treatment of cough, asthma, excessive phlegm.
The medicine made from this prescription at present has MANGGUO ZHIKE PIAN, and its quality standard records in the 5th the 50th page of Ministry of Health of the People's Republic of China's " Chinese traditional patent formulation preparation ".The clinical for many years use determined curative effect of MANGGUO ZHIKE PIAN listing, side effect are little, are a kind of Chinese and western drugs compound preparations of comparatively ideal treatment cough.But this drug standard is too simple, and the control product quality is by the ministry standard WS of Ministry of Health of the People's Republic of China
3-B-0919-91 carries out, and does not have comparatively ideal qualitative method in the standard, does not more formulate the assay item, therefore control of quality and stable curative effect and the incidence rate that reduces side effect effectively.Particularly contain two chemical medicines of Sodium Houttuyfonate and chlorphenamine maleate in this compound preparation, all untoward reaction may take place at any time.So, the composition in the preparation is carried out qualitative and quantitatively is necessary.Owing to influence each other between the compound preparation composition of Chinese and Western with disturb too greatly, it is bigger to formulate truly feasible qualitative and quantitative approach difficulty.
In recent years, there is the people that composition contained in the said preparation was carried out some researchs, comprises the research of qualitative-and-quantitative method, but more to the research of the contained chimonin of Folium mango dry extractum, and very few to the research of two chemical medicines.Main research has: content for Chlorphenamine Maleate in the tlc scanning determination MANGGUO ZHIKE PIAN. the journal .2001.4 of Colleges Of Traditional Chinese Medicine Of Guangxi (4): 100～101; The thin layer of Folium mangiferae is differentiated in the MANGGUO ZHIKE PIAN. basic unit's Chinese medicine magazine, 1999,13 (1): 8; The improvement of discrimination method in the MANGGUO ZHIKE PIAN quality standard. Chinese drug standard, 2001,2 (4): 51; The RP-HPLC method is measured the content of chimonin in the Folium mangiferae. CHINA JOURNAL OF CHINESE MATERIA MEDICA .2003,28 (9): 839～841; The HPLC method is measured the content of Mengiferin in the MANGGUO ZHIKE PIAN. Chinese patent medicine, 1997,03:14～15.More than repeatability and the stability of condition determination in practice formulated of these institutes be not very desirable, the sensitivity and the degree of accuracy that particularly adopt thin-layer chromatogram scanner to measure chlorphenamine maleate content in the MANGGUO ZHIKE PIAN are not fine, so these methods fail to take in the quality standard of said preparation always.
Summary of the invention
The objective of the invention is in order to overcome deficiency of the prior art, a kind of method of quality control of new Folium mango dry extractum compound preparation is provided, it is characterized in that, this method comprises that thin layer chromatography differentiates and determination.
The method of quality control of a kind of Folium mango dry extractum compound preparation provided by the invention, it is characterized in that, described thin layer chromatography is differentiated, concrete technical scheme is: differentiate in this compound preparation as positive control with the gallic acid reference substance and contain Folium mango dry extractum, differentiate as positive control with corresponding reference substance and contain Sodium Houttuyfonate in this compound preparation and contain chlorphenamine maleate.
(1) differentiate that as positive control the chromatographic condition and the discrimination method that contain Folium mango dry extractum in this compound preparation are with the gallic acid reference substance:
This compound preparation content 2g is got in the preparation of need testing solution, and porphyrize adds water 50ml, and heating is 30 minutes in boiling water bath, stirs constantly, takes out, and puts coldly, filters, and filtrate evaporate to dryness, residue add the 1ml dissolve with methanol, filter, promptly;
The gallic acid reference substance is got in the preparation of reference substance solution, adds methanol and makes the solution that 1ml contains gallic acid 0.5mg, in contrast product solution;
The discrimination method point sample in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethyl acetate-formic acid (6: 2: 2) is developing solvent, launch, spray is with 2% ferric chloride alcoholic solution, in 105 ℃ of heating colour developing in 2 minutes behind the airing.
(2) differentiate that as positive control the chromatographic condition and the discrimination method that contain Sodium Houttuyfonate in this compound preparation are with the Sodium Houttuyfonate reference substance:
This compound preparation content 2g is got in the preparation of need testing solution, and porphyrize adds methanol 20ml and ground 10 minutes, filters, and filtrate evaporate to dryness, residue add the 1ml dissolve with methanol, filter, promptly;
The Sodium Houttuyfonate reference substance is got in the preparation of reference substance solution, adds methanol and makes the solution that 1ml contains 3mg, in contrast product solution;
The discrimination method point sample in same be the silica gel G F of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, be developing solvent, launch, dry under the rearmounted 254nm ultra-violet lamp and inspect with chloroform-methanol-strong ammonia solution (20: 1: 0.2).
(3) differentiate that as positive control the chromatographic condition and the discrimination method that contain chlorphenamine maleate in this compound preparation are with the chlorphenamine maleate reference substance:
This compound preparation content 3g is got in the preparation of need testing solution, and porphyrize adds water 30ml, and jolting number minute with 2%NaOH adjust pH to 11, adds chloroform 30ml and extracts, and gets the chloroform layer, and evaporate to dryness, residue add the 1ml dissolve with methanol, filter, promptly;
The chlorphenamine maleate reference substance is got in the preparation of reference substance solution, adds methanol and makes the solution that 1ml contains chlorphenamine maleate 1mg, in contrast product solution;
The discrimination method point sample in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with methanol-strong ammonia solution (20: 0.15), launch, dry in the rearmounted iodine vapor smoked to colour developing.
The method of quality control of a kind of Folium mango dry extractum compound preparation provided by the invention, it is characterized in that, described determination is with chimonin, Sodium Houttuyfonate and content for Chlorphenamine Maleate in this compound preparation of high effective liquid chromatography for measuring, and has determined content limit.
Described chimonin belongs to polyphenol compound, molecular formula: C
19H
18O
11
Sodium Houttuyfonate belongs to the sodium sulfite addition product of decanoylacetaldehyde, and the original name Sodium Houttuyfonate records in first of the Sanitation Ministry medicine standard chemistry medicine, back income Chinese Pharmacopoeia nineteen ninety-five version, and Sodium Houttuyfonate just by name, molecular formula:
C
12H
23NaO
5S
Chlorphenamine maleate records in one one of Chinese Pharmacopoeia version in 2005, original name chlorphenamine.Molecular formula:
C
16H
19ClN
2·C
4H
4O
4
(1) chimonin content assaying method
The chromatographic condition chromatographic column is filler with the octadecylsilane chemically bonded silica, and mobile phase is methanol-0.3% phosphoric acid solution-triethylamine (28: 72: 0.25), and the detection wavelength is 258nm;
It is an amount of that the preparation precision of reference substance solution takes by weighing the chimonin reference substance, adds methanol and make the solution that every 1ml contains 50 μ g, promptly;
The about 0.5g of Folium mango dry extractum compound preparation content is got in the preparation of need testing solution, porphyrize, and weight decided in accurate title, put in the tool plug conical flask, the accurate 70% methanol solution 20ml that adds claims to decide weight, reflux 1.5 hours, take out, put and claim again to decide weight after cold, supply the weight of minimizing with 70% methanol, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of assay method inject high performance liquid chromatograph, measure, promptly.
(2) Sodium Houttuyfonate content assaying method
The chromatographic condition chromatographic column is filler with the octadecylsilane chemically bonded silica, and mobile phase is methanol-water-tetraethyl ammonium hydroxide (65: 35: 0.3), and the detection wavelength is 283nm, column temperature: 35 ℃;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Sodium Houttuyfonate reference substance, adds methanol and make the solution that every 1ml contains 70 μ g, promptly;
The preparation of need testing solution takes by weighing Folium mango dry extractum compound preparation content 0.2g, porphyrize, and accurate the title, decide, and puts in the 100ml measuring bottle, add methanol 60ml, supersound process 20 minutes is taken out, put cold back with methanol constant volume to scale, shake up, filter, get subsequent filtrate, promptly;
Assay method: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject high performance liquid chromatograph, measure, promptly.
(3) chlorphenamine maleate content assay method:
The chromatographic condition chromatographic column is filler with the octadecylsilane chemically bonded silica, and mobile phase is 0.005mol/L dodecyl sodium sulfate methanol solution-phosphate buffered solution (55: 45), detects wavelength 262nm, 40 ℃ of column temperatures;
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorphenamine maleate reference substance, adds methanol and make the solution that every 1ml contains chlorphenamine maleate 0.1mg, promptly;
The preparation of need testing solution takes by weighing Folium mango dry extractum compound preparation content 1.0g, porphyrize, and accurate the title, decide, and the accurate methanol solution 20ml that adds claims to decide weight, supersound process 30 minutes is taken out, and puts coldly, claims to decide weight again, supplies the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly;
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of assay method inject high performance liquid chromatograph, measure, promptly.
The technological progress that the present invention obtains is:
1, formulated the thin layer chromatography discrimination method of said preparation, this method specificity is strong, favorable reproducibility.
2, the content of each composition in the utilization high performance liquid chromatography energy fast detecting preparation, can overcome the big deficiency of other assay method measurement deviation, the accuracy height has stronger practicality to the production and the quality control of said preparation, has guaranteed the safe, effective and stable and controllable for quality of product.
3, the present invention is applicable to the quality control of the multiple dosage form of this compound preparation.
Description of drawings
Fig. 1. be the high-efficient liquid phase chromatogram of measuring chimonin content in the MANGGUO ZHIKE PIAN
Fig. 2. be the high-efficient liquid phase chromatogram of measuring houttuynine sodium bisulfite sodium content in the MANGGUO ZHIKE PIAN
Fig. 3. be the high-efficient liquid phase chromatogram of measuring chlorphenamine maleate content in the MANGGUO ZHIKE PIAN
Fig. 4. be the high-efficient liquid phase chromatogram of measuring chimonin content in the MANGGUO ZHIKE JIAONANG
Fig. 5. be the high-efficient liquid phase chromatogram of measuring houttuynine sodium bisulfite sodium content in the MANGGUO ZHIKE JIAONANG
Fig. 6. be the high-efficient liquid phase chromatogram of measuring chlorphenamine maleate content in the MANGGUO ZHIKE JIAONANG
1 is the peak type of corresponding composition in the accompanying drawing.
The specific embodiment
Embodiment one:
MANGGUO ZHIKE PIAN
1, contains Folium mango dry extractum in the discriminating MANGGUO ZHIKE PIAN
Get this product 2g that removes behind the coating, porphyrize adds water 50ml, puts in the water-bath heating 30 minutes, stirs constantly, takes out, and puts coldly, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, filters, and filtrate is as need testing solution.Other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethyl acetate-formic acid (6: 2: 2) is developing solvent, launch, take out, dry, spray is with 2% ferric chloride alcoholic solution, in 105 ℃ of heating 2 minutes.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
2, contain Sodium Houttuyfonate in the discriminating MANGGUO ZHIKE PIAN
Get this product 2g that removes behind the coating, add methanol 20ml, ground 10 minutes, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, filters, and filtrate is as need testing solution.Other gets the Sodium Houttuyfonate reference substance, adds methanol and makes the solution that every 1ml contains 3mg, in contrast product solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica gel G F of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, be developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect with chloroform-methanol-ammonia (20: 1: 0.2).In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
3, contain chlorphenamine maleate in the discriminating MANGGUO ZHIKE PIAN
Get this product 3g that removes behind the coating, add water 30ml, jolting number minute is regulated pH value to 11 with 2% sodium hydroxide solution, adds chloroform 30ml extraction, divides and gets the chloroform layer, and evaporate to dryness, residue add methanol 1ml makes dissolving, filters, and filtrate is as need testing solution.Other gets the chlorphenamine maleate reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw above-mentioned reference substance solution 5 μ l, need testing solution 10 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with methanol-strong ammonia solution (20: 0.15) is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the iodine vapor.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
4, chimonin assay in the MANGGUO ZHIKE PIAN
Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).Fig. 1 is a chromatogram.
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With methanol-0.3% phosphoric acid solution-triethylamine (28: 72: 0.25) is mobile phase; The detection wavelength is 258nm.Number of theoretical plate calculates by the chimonin peak should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the chimonin reference substance, adds methanol and make the solution that every 1ml contains 50 μ g, promptly.
The preparation of need testing solution: get 20 of this product, remove coating, porphyrize, mixing is got 0.5g, and accurate the title decides, put in the tool plug conical flask, the accurate 70% methanol solution 20ml that adds claims to decide weight, reflux 1.5 hours is taken out, and puts cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with 70% methanol, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph, measure, promptly.
Every of this product contains Folium mango dry extractum with chimonin (C
19H
18O
11) calculate, be no less than 0.70mg.
5, Sodium Houttuyfonate assay in the MANGGUO ZHIKE PIAN
Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).Fig. 2 is a chromatogram.
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With methanol-water-tetraethyl ammonium hydroxide (65: 35: 0.3) is mobile phase; The detection wavelength is 283nm; Column temperature: 35 ℃.Number of theoretical plate calculates by the Sodium Houttuyfonate peak should be not less than 5000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the Sodium Houttuyfonate reference substance, adds methanol and make the solution that every 1ml contains 70 μ g, promptly.
The preparation of need testing solution: get 10 of this product, remove coating, porphyrize, mixing is got 0.2g, and accurate the title, decide, put in the measuring bottle of 100ml, add 60ml methanol, supersound process 20 minutes is taken out, put cold after,, shake up to scale with methanol constant volume, filter, get subsequent filtrate, promptly.
Algoscopy: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject high performance liquid chromatograph and measure, promptly.
Every of this product contains Sodium Houttuyfonate (C
12H
23NaO
5S), should be 80.0%～120.0% of labelled amount.
6, chlorphenamine maleate content is measured in the MANGGUO ZHIKE PIAN
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).Fig. 3 is a chromatogram.
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With 0.005moL/L dodecyl sodium sulfate methanol solution-phosphate buffered solution (potassium dihydrogen phosphate 6.8g adds water to 1000mL, contains 1% triethylamine, and transferring PH with phosphoric acid is 3.0～3.2) (55: 45) is mobile phase; The detection wavelength is 262nm; Column temperature: 40 ℃.Number of theoretical plate calculates by the chlorphenamine maleate peak should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the chlorphenamine maleate reference substance, adds methanol and make the solution that every 1ml contains chlorphenamine maleate 100 μ g, promptly.
The preparation of need testing solution: get 20 of this product, remove coating, porphyrize, mixing is got 1.0g, and accurate the title, decide, the accurate methanol solution 20ml that adds claims decide weight, and supersound process 30 minutes is taken out, and puts coldly, and weight decided in title again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
Algoscopy: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject high performance liquid chromatograph and measure, promptly.
Every of this product contains chlorphenamine maleate (C
16H
19ClN
2C
4H
4O
4), should be 80.0%～120.0% of labelled amount.
Embodiment two:
MANGGUO ZHIKE JIAONANG
(1) contains Folium mango dry extractum in the discriminating MANGGUO ZHIKE JIAONANG
Get this product content 2g, porphyrize adds water 50ml, puts in the water-bath heating 30 minutes, stirs constantly, takes out, and puts coldly, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, filters, and filtrate is as need testing solution.Other gets the gallic acid reference substance, adds methanol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethyl acetate-formic acid (6: 2: 2) is developing solvent, launch, take out, dry, spray is with 2% ferric chloride alcoholic solution, in 105 ℃ of heating 2 minutes.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
2, contain Sodium Houttuyfonate in the discriminating MANGGUO ZHIKE JIAONANG
Get this product content 2g, add methanol 20ml, ground 10 minutes, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, filters, and filtrate is as need testing solution.Other gets the Sodium Houttuyfonate reference substance, adds methanol and makes the solution that every 1ml contains 3mg, in contrast product solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be the silica gel G F of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, be developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect with chloroform-methanol-ammonia (20: 1: 0.2).In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
3, contain chlorphenamine maleate in the discriminating MANGGUO ZHIKE JIAONANG
Get this product content 3g, add water 30ml, jolting number minute is regulated pH value to 11 with 2% sodium hydroxide solution, adds chloroform 30ml extraction, divides and gets the chloroform layer, and evaporate to dryness, residue add methanol 1ml makes dissolving, filters, and filtrate is as need testing solution.Other gets the chlorphenamine maleate reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw above-mentioned reference substance solution 5 μ l, need testing solution 10 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with methanol-strong ammonia solution (20: 0.15) is developing solvent, launch, take out, dry, it is smoked clear to the speckle colour developing to put in the iodine vapor.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
4, chimonin assay in the MANGGUO ZHIKE JIAONANG
Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).Fig. 4 is a chromatogram.
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With methanol-0.3% phosphoric acid solution-triethylamine (28: 72: 0.25) is mobile phase; The detection wavelength is 258nm.Number of theoretical plate calculates by the chimonin peak should be not less than 3000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the chimonin reference substance, adds methanol and make the solution that every 1ml contains 50 μ g, promptly.
20 of this product are got in the preparation of need testing solution, get content, mixing, porphyrize is got 0.5g, and accurate the title decides, put in the tool plug conical flask, the accurate 70% methanol solution 20ml that adds claims to decide weight, reflux 1.5 hours is taken out, and puts cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with 70% methanol, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph and measure, promptly.
Every of this product contains Folium mango dry extractum with chimonin (C
19H
18O
11) calculate, be no less than 0.70mg.
5, Sodium Houttuyfonate assay in the MANGGUO ZHIKE JIAONANG
Measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).Fig. 5 is a chromatogram.
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; With methanol-water-tetraethyl ammonium hydroxide (65: 35: 0.3) is mobile phase; The detection wavelength is 283nm; Column temperature: 35 ℃.Number of theoretical plate calculates by the Sodium Houttuyfonate peak should be not less than 5000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the Sodium Houttuyfonate reference substance, adds methanol and make the solution that every 1ml contains 70 μ g, promptly.
10 of this product are got in the preparation of need testing solution, get content, mixing, and porphyrize is got 0.2g, and accurate the title, decide, put in the measuring bottle of 100ml, add 60ml methanol, supersound process 20 minutes is taken out, put cold after,, shake up to scale with methanol constant volume, filter, get subsequent filtrate, promptly.
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph and measure, promptly.
Every of this product contains Sodium Houttuyfonate (C
12H
23NaO
5S), should be 80.0%～120.0% of labelled amount.
6, chlorphenamine maleate content is measured in the MANGGUO ZHIKE JIAONANG
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).Fig. 6 is a chromatogram.
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With 0.005moL/L dodecyl sodium sulfate methanol solution-phosphate buffered solution (potassium dihydrogen phosphate 6.8g adds water to 1000mL, contains 1% triethylamine, and transferring PH with phosphoric acid is 3.0～3.2) (55: 45) is mobile phase; The detection wavelength is 262nm; Column temperature: 40 ℃.Number of theoretical plate calculates by the chlorphenamine maleate peak should be not less than 3000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorphenamine maleate reference substance, adds methanol and make the solution that every 1ml contains chlorphenamine maleate 100 μ g, promptly.
20 of this product are got in the preparation of need testing solution, get content, mixing, and porphyrize is got 1.0g, and accurate the title, decide, the accurate methanol solution 20ml that adds claims decide weight, and supersound process 30 minutes is taken out, and puts coldly, and weight decided in title again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph and measure, promptly.
Every of this product contains chlorphenamine maleate (C
16H
19ClN
2C4H
4O
4), should be 80.0%～120.0% of labelled amount.
Claims (12)
1, the method for quality control of Folium mango dry extractum compound preparation is characterized in that this method comprises thin layer chromatography discriminating and determination.
2, the method for claim 1, it is characterized in that, described thin layer chromatography is differentiated, be to adopt the gallic acid reference substance to differentiate in this compound preparation to contain Folium mango dry extractum, adopt corresponding reference substance to differentiate and contain Sodium Houttuyfonate in this compound preparation and contain chlorphenamine maleate as positive control as positive control.
3, the method for claim 2 is characterized in that, described thin layer chromatography differentiates that the method that contains Folium mango dry extractum in this compound preparation is:
This compound preparation content 2g is got in the preparation of need testing solution, and porphyrize adds water 50ml, and heating is 30 minutes in boiling water bath, stirs constantly, takes out, and puts coldly, filters, and filtrate evaporate to dryness, residue add the 1ml dissolve with methanol, filter, promptly;
The gallic acid reference substance is got in the preparation of reference substance solution, adds methanol and makes the solution that 1ml contains gallic acid 0.5mg, in contrast product solution;
The detection method point sample in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform-ethyl acetate-formic acid (6: 2: 2) is developing solvent, launch, spray is with 2% ferric chloride alcoholic solution, in 105 ℃ of heating colour developing in 2 minutes behind the airing.
4, the method for claim 2 is characterized in that, described thin layer chromatography differentiates that the method that contains Sodium Houttuyfonate in this compound preparation is:
This compound preparation content 2g is got in the preparation of need testing solution, and porphyrize adds methanol 20ml and ground 10 minutes, filters, and filtrate evaporate to dryness, residue add the 1ml dissolve with methanol, filter, promptly;
The Sodium Houttuyfonate reference substance is got in the preparation of reference substance solution, adds methanol and makes the solution that 1ml contains Sodium Houttuyfonate 3mg, in contrast product solution;
The detection method point sample in same be the silica gel G F of adhesive with the sodium carboxymethyl cellulose
254On the lamellae, be developing solvent, launch, dry under the rearmounted 254nm ultra-violet lamp and inspect with chloroform-methanol-strong ammonia solution (20: 1: 0.2).
5, the method for claim 2 is characterized in that, described thin layer chromatography differentiates that the method that contains chlorphenamine maleate in this compound preparation is:
This compound preparation content 3g is got in the preparation of need testing solution, and porphyrize adds water 30ml, and jolting number minute with 2%NaOH adjust pH to 11, adds chloroform 30ml and extracts, and divides and gets the chloroform layer, and evaporate to dryness, residue add the 1ml dissolve with methanol, filter, promptly;
The chlorphenamine maleate reference substance is got in the preparation of reference substance solution, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution;
The detection method point sample in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with methanol-strong ammonia solution (20: 0.15), launch, dry in the rearmounted iodine vapor smoked to colour developing.
6, the method for claim 1 is characterized in that, described determination is the chimonin content that adopts in this compound preparation of high effective liquid chromatography for measuring, houttuynine sodium bisulfite sodium content and chlorphenamine maleate content.
7, the method for claim 6 is characterized in that, the chimonin HPLC method is in this compound preparation of described mensuration:
The chromatographic condition chromatographic column is filler with the octadecylsilane chemically bonded silica, and mobile phase is methanol-0.3% phosphoric acid solution-triethylamine (28: 72: 0.25), and the detection wavelength is 258nm;
It is an amount of that the preparation precision of reference substance solution takes by weighing the chimonin reference substance, adds methanol and make the solution that every 1ml contains 50 μ g, promptly;
The about 0.5g of this compound preparation content is got in the preparation of need testing solution, porphyrize, and weight decided in accurate title, put in the tool plug conical flask, the accurate 70% methanol solution 20ml that adds claims to decide weight, reflux 1.5 hours, take out, put and claim again to decide weight after cold, supply the weight of minimizing with 70% methanol, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of assay method inject high performance liquid chromatograph, measure, promptly.
8, the method for claim 6 is characterized in that, the Sodium Houttuyfonate HPLC method is in this compound preparation of described mensuration:
The chromatographic condition chromatographic column is filler with the octadecylsilane chemically bonded silica, and mobile phase is methanol-water-tetraethyl ammonium hydroxide (65: 35: 0.3), and the detection wavelength is 283nm, column temperature: 35 ℃;
It is an amount of that the preparation precision of reference substance solution takes by weighing the Sodium Houttuyfonate reference substance, adds methanol and make the solution that every 1ml contains 70 μ g, promptly;
The preparation of need testing solution takes by weighing this compound preparation content 0.2g, and porphyrize accurate claims surely, puts in the 100ml measuring bottle, adds methanol 60ml, and supersound process 20 minutes is taken out, put cold back with methanol constant volume to scale, shake up, filter, get subsequent filtrate, promptly;
Assay method: accurate reference substance solution and each 10 μ l of need testing solution of drawing, inject high performance liquid chromatograph, measure, promptly.
9, the method for claim 6 is characterized in that, the high performance liquid chromatography of chlorphenamine maleate content is in this compound preparation of described mensuration:
The chromatographic condition chromatographic column is filler with the octadecylsilane chemically bonded silica, and mobile phase is 0.005mol/L dodecyl sodium sulfate methanol solution-phosphate buffered solution (55: 45), and the detection wavelength is 262nm, 40 ℃ of column temperatures;
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorphenamine maleate reference substance, adds methanol and make the solution that every 1ml contains chlorphenamine maleate 0.1mg, promptly;
The preparation of need testing solution takes by weighing this compound preparation content 1.0g, porphyrize, and accurate the title, decide, and the accurate methanol solution 20ml that adds claims to decide weight, supersound process 30 minutes is taken out, and puts coldly, claims to decide weight again, supplies the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly;
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of assay method inject high performance liquid chromatograph, measure, promptly.
10, the method for claim 9, described phosphate buffered solution compound method is: get potassium dihydrogen phosphate 6.8g, add water to 1000mL (containing 1% triethylamine), transferring pH value with phosphoric acid is 3.0～3.2, promptly.
11, the method for claim 1 can detect the various dosage forms of mainly being made by Folium mango dry extractum 92～98 weight portions, Sodium Houttuyfonate 2～8 weight portions, chlorphenamine maleate 0.1～0.4 weight portion prescription.
12, the method for claim 11, described dosage form are capsule, hard capsule, soft capsule, tablet, Film coated tablets, coated tablet, enteric coated tablet, effervescent tablet, dispersible tablet, slow releasing tablet.
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| CNB2005101252246A CN100402048C (en) | 2005-11-19 | 2005-11-19 | Quality control method of composite prepn. of dry mango tree leaves extract |
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| CNB2005101252246A CN100402048C (en) | 2005-11-19 | 2005-11-19 | Quality control method of composite prepn. of dry mango tree leaves extract |
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| CN100402048C CN100402048C (en) | 2008-07-16 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101181357B (en) * | 2007-11-30 | 2010-11-03 | 广西药用植物园制药厂 | Detection method of chlorphenamine Maleate of ketelin lozenge |
| CN105866285A (en) * | 2016-04-26 | 2016-08-17 | 广西壮族自治区梧州食品药品检验所 | Method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in manner of liquid mass spectrum serial connection |
| CN110780007A (en) * | 2019-12-11 | 2020-02-11 | 广西中医药大学制药厂 | Method for evaluating 6 component contents of mango cough relieving tablet by HPLC (high performance liquid chromatography) method |
| CN115420834A (en) * | 2022-09-29 | 2022-12-02 | 广西中医药大学百年乐制药有限公司 | Establishment of mango cough relieving tablet fingerprint and component content determination method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102854282B (en) * | 2012-09-12 | 2014-12-03 | 广州白云山敬修堂药业股份有限公司 | Detection method of traditional Chinese medicine compound preparation used for treating laryngopathy |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559503A (en) * | 2004-02-18 | 2005-01-05 | 徐小彬 | Mango couth suppressing capsule and method of preparatuion long effect capsule |
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2005
- 2005-11-19 CN CNB2005101252246A patent/CN100402048C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101181357B (en) * | 2007-11-30 | 2010-11-03 | 广西药用植物园制药厂 | Detection method of chlorphenamine Maleate of ketelin lozenge |
| CN105866285A (en) * | 2016-04-26 | 2016-08-17 | 广西壮族自治区梧州食品药品检验所 | Method for measuring mangiferin and bergenin in heat-clearing cough-relieving syrup in manner of liquid mass spectrum serial connection |
| CN110780007A (en) * | 2019-12-11 | 2020-02-11 | 广西中医药大学制药厂 | Method for evaluating 6 component contents of mango cough relieving tablet by HPLC (high performance liquid chromatography) method |
| CN110780007B (en) * | 2019-12-11 | 2022-07-08 | 广西中医药大学制药厂 | Method for evaluating 6 component contents of mango cough relieving tablet by HPLC (high performance liquid chromatography) method |
| CN115420834A (en) * | 2022-09-29 | 2022-12-02 | 广西中医药大学百年乐制药有限公司 | Establishment of mango cough relieving tablet fingerprint and component content determination method |
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| CN100402048C (en) | 2008-07-16 |
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