CN101637506A - Method for detecting compound herba solidaginis spray - Google Patents
Method for detecting compound herba solidaginis spray Download PDFInfo
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- CN101637506A CN101637506A CN200910306184A CN200910306184A CN101637506A CN 101637506 A CN101637506 A CN 101637506A CN 200910306184 A CN200910306184 A CN 200910306184A CN 200910306184 A CN200910306184 A CN 200910306184A CN 101637506 A CN101637506 A CN 101637506A
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Abstract
The invention discloses a method for detecting the quality of compound herba solidaginis spray, which revises a method for detecting the content of compound herba solidaginis spray on the basis of theoriginal quality standard so that a detecting result is more accurate.
Description
Technical field
The invention belongs to the pharmaceutical technology field, relate to a kind of detection method of spray, particularly a kind of detection method for the treatment of the spray (adopted name or nomenclature of drug compound herba solidaginis spray) of upper respiratory tract infection.
Background technology
Compound herba solidaginis spray has heat-clearing and toxic substances removing, dispelling wind-heat, and the function of clearing throat is used for upper respiratory tract infection, acute and chronic pharyngitis, aphtha of the mouth and tongue, gingival swelling and pain, diseases such as halitosis.In the quality standard of existing compound herba solidaginis spray, content assaying method is perfect inadequately, may make testing result not accurate enough, influences the curative effect of medicine.For guaranteeing this product quality and help supervision, management, tackle the preparation method of need testing solution in the content assaying method of this product and revise, thereby guarantee product quality this product quality.
Summary of the invention
The objective of the invention is: the detection method that a kind of compound herba solidaginis spray is provided.The present invention has revised the preparation method of need testing solution in the content assaying method on the initial quality standard base.The present invention has remedied the deficiency of proper mass control procedure, has improved the quality monitoring level of product.
Purpose of the present invention can realize by following technical proposal: the detection method of compound herba solidaginis spray, according to listed as parts by weight, compound herba solidaginis spray is to make the 1000ml spray with Herba Solidaginis 167g, Flos Lonicerae 278g, Rhizoma Osmundae 167g, Fructus Forsythiae 167g, Herba Menthae 111g, Herba Schizonepetae 111g, Herba Blumeae Balsamiferae 111g; It is characterized in that this detection method may further comprise the steps:
Character: this product (compound herba solidaginis spray) is that brownish red is to tan supernatant liquid; Bitter in the mouth is little sweet, the refrigerant sense of tool;
Differentiate: (1) gets this product 10ml, and evaporate to dryness, residue add ethanol 25ml, and supersound process makes dissolving, filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets the chlorogenic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same polyamide thin film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp of 365nm and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(2) get this product 50ml, steam near and do, add water 15ml, regulate pH value to 1～2 with hydrochloric acid, extract 2 times with the ether jolting, each 40ml merges ether solution, volatilizes, and residue adds dehydrated alcohol 2ml makes dissolving, as need testing solution; Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.2mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 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 cyclohexane extraction-acetone of 5: 2: 1-ethyl acetate is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, puts under the uviol lamp of 365nm and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
In the above-mentioned compound herba solidaginis spray quality determining method, this detection method also comprises:
Inspection should meet following relevant every regulation;
Relative density should be not less than 1.02;
PH value should be 3.5～5.5;
Jet test is whenever pressed average emitted dose for every bottle and be should be 0.06g～0.15g;
Other should meet every regulation relevant under the spray item;
Assay is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With 10: 90 acetonitriles-0.4% phosphoric acid solution is mobile phase; The detection wavelength is 327nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the chlorogenic acid reference substance, and accurate the title decides, and adds 50% methanol and makes the solution that every 1ml contains 50 μ g, promptly;
The preparation of need testing solution: precision is measured this product 10ml, and evaporate to dryness, residue add methanol 10ml, use 250W, the supersound process of 40KHz 20 minutes filters, with methanol about 10ml gradation washing container and filter, merging filtrate and washing liquid, evaporate to dryness, residue add water 15ml makes dissolving, regulate pH value to 3～4 with dilute hydrochloric acid, extract 5 times each 25ml, combined ethyl acetate liquid with the ethyl acetate jolting, evaporate to dryness, residue adds 50% methanol makes dissolving, is transferred in the measuring bottle of 50ml, adds 50% methanol and is diluted to scale, shake up, filter, get subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
The every 1ml of this product contains Flos Lonicerae and Herba Solidaginis with chlorogenic acid (C
16H
18O
9) meter, must not be less than 0.40mg.
In the aforesaid compound herba solidaginis spray quality determining method, described compound herba solidaginis spray is made according to following method:
Get above seven flavor medicine material, soaked 2～3 hours, add thermal distillation, collect Aromatic water, standby 1～4 ℃ temperature lower seal cold preservation, extracting solution device is in addition preserved; Medicinal residues decoct with water secondary, 1.5 hours for the first time, 1 hour for the second time, decocting liquid and said extracted liquid merged, and filtered, filtrate be condensed into relative density be 1.10～1.13 and temperature be 45 ℃ clear paste, add ethanol and make and contain the alcohol amount and reach 70%, stir, left standstill 24 hours, filter, reclaim ethanol and be condensed into relative density be 1.20 and temperature be 45 ℃ clear paste; Add Aromatic water, mixing, cold preservation filters, and filtrate adds steviosin, potassium sorbate, and mixing adds water to ormal weight, fill, promptly.
Compared with prior art, the present invention has revised the content assaying method of compound herba solidaginis spray on initial quality control basis, make testing result more accurate.The present invention has remedied the deficiency of proper mass control procedure, has improved the quality monitoring level of product.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment, but not as the foundation of the present invention being done any restriction.
Embodiment.The detection method of this compound herba solidaginis spray, according to listed as parts by weight, compound herba solidaginis spray is to make the 1000ml spray with Herba Solidaginis 167g, Flos Lonicerae 278g, Rhizoma Osmundae 167g, Fructus Forsythiae 167g, Herba Menthae 111g, Herba Schizonepetae 111g, Herba Blumeae Balsamiferae 111g; This detection method may further comprise the steps:
Character: this product is that brownish red is to tan supernatant liquid; Bitter in the mouth is little sweet, the refrigerant sense of tool.
Differentiate: (1) gets this product 10ml, and evaporate to dryness, residue add ethanol 25ml, and supersound process makes dissolving, filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution.Other gets the chlorogenic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same polyamide thin film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(2) get this product 50ml, steam near and do, add water 15ml, regulate pH value to 1～2 with hydrochloric acid, extract 2 times with the ether jolting, each 40ml merges ether solution, volatilizes, and residue adds dehydrated alcohol 2ml makes dissolving, as need testing solution.Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.2mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 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 cyclohexane extraction-acetone-ethyl acetate (5: 2: 1) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, puts under the uviol lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
This detection method also comprises:
Check:
Relative density: should be not less than 1.02 (appendix VIIA of Chinese Pharmacopoeia version in 2005).
PH value: should be 3.5～5.5 (appendix VIIG of Chinese Pharmacopoeia version in 2005).
Jet test: whenever press average emitted dose for every bottle and should be 0.06g～0.15g (an appendix I of Chinese Pharmacopoeia version in 2005 Z)
Other: should meet every regulation relevant under the spray item (an appendix I of Chinese Pharmacopoeia version in 2005 Z).
Assay: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-0.4% phosphoric acid solution (10: 90) is a mobile phase; The detection wavelength is 327nm.Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 2000.
The preparation of reference substance solution: it is an amount of to get the chlorogenic acid reference substance, and accurate the title decides, and adds 50% methanol and makes the solution that every 1ml contains 50 μ g, promptly.
The preparation of need testing solution: precision is measured this product 10ml, and evaporate to dryness, residue add methanol 10ml, (250W 40KHz) 20 minutes, filters supersound process, with methanol about 10ml gradation washing container and filter, merging filtrate and washing liquid, evaporate to dryness, residue add water 15ml makes dissolving, regulate pH value to 3～4 with dilute hydrochloric acid, extract 5 times each 25ml, combined ethyl acetate liquid with the ethyl acetate jolting, evaporate to dryness, residue adds 50% methanol makes dissolving, is transferred in the measuring bottle of 50ml, adds 50% methanol and is diluted to scale, shake up, filter, get subsequent filtrate, promptly.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
The every 1ml of this product contains Flos Lonicerae and Herba Solidaginis with chlorogenic acid (C
16H
18O
9) meter, must not be less than 0.40mg.
Compound herba solidaginis spray is made according to following method:
Get above seven flavor medicine material, soaked 2～3 hours, add thermal distillation, collect Aromatic water, sealing cold preservation (1～4 ℃), standby, extracting solution device is in addition preserved; Medicinal residues decoct with water secondary, 1.5 hours for the first time, 1 hour for the second time, decocting liquid and said extracted liquid merged, and filtered, filtrate is condensed into the clear paste that relative density is 1.10～1.13 (45 ℃), add ethanol and make and contain the alcohol amount and reach 70%, stir, left standstill 24 hours, filter, reclaim ethanol and be condensed into the clear paste that relative density is 1.20 (45 ℃); Add Aromatic water, mixing, cold preservation filters, and filtrate adds steviosin, potassium sorbate, and mixing adds water to ormal weight, fill, promptly.
Claims (3)
1. the quality determining method of compound herba solidaginis spray, according to listed as parts by weight, compound herba solidaginis spray is to make the 1000ml spray with Herba Solidaginis 167g, Flos Lonicerae 278g, Rhizoma Osmundae 167g, Fructus Forsythiae 167g, Herba Menthae 111g, Herba Schizonepetae 111g, Herba Blumeae Balsamiferae 111g; It is characterized in that this detection method may further comprise the steps:
Character: this product is that brownish red is to tan supernatant liquid; Bitter in the mouth is little sweet, the refrigerant sense of tool;
Differentiate: (1) gets this product 10ml, and evaporate to dryness, residue add ethanol 25ml, and supersound process makes dissolving, filters, and filtrate evaporate to dryness, residue add ethanol 2ml makes dissolving, as need testing solution; Other gets the chlorogenic acid reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to thin layer chromatography test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same polyamide thin film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp of 365nm and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(2) get this product 50ml, steam near and do, add water 15ml, regulate pH value to 1～2 with hydrochloric acid, extract 2 times with the ether jolting, each 40ml merges ether solution, volatilizes, and residue adds dehydrated alcohol 2ml makes dissolving, as need testing solution; Other evens up pier fruit acid reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 0.2mg, in contrast product solution; Test according to thin layer chromatography, draw each 10 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 cyclohexane extraction-acetone of 5: 2: 1-ethyl acetate is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 110 ℃, puts under the uviol lamp of 365nm and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
2. the quality determining method of compound herba solidaginis spray according to claim 1 is characterized in that, this detection method also comprises:
Inspection should meet following relevant every regulation;
Relative density should be not less than 1.02;
PH value should be 3.5～5.5;
Jet test is whenever pressed average emitted dose for every bottle and be should be 0.06g～0.15g;
Other should meet every regulation relevant under the spray item;
Assay is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With 10: 90 acetonitriles-0.4% phosphoric acid solution is mobile phase; The detection wavelength is 327nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the chlorogenic acid reference substance, and accurate the title decides, and adds 50% methanol and makes the solution that every 1ml contains 50 μ g, promptly;
The preparation of need testing solution: precision is measured this product 10ml, and evaporate to dryness, residue add methanol 10ml, use 250W, the supersound process of 40KHz 20 minutes filters, with methanol about 10ml gradation washing container and filter, merging filtrate and washing liquid, evaporate to dryness, residue add water 15ml makes dissolving, regulate pH value to 3～4 with dilute hydrochloric acid, extract 5 times each 25ml, combined ethyl acetate liquid with the ethyl acetate jolting, evaporate to dryness, residue adds 50% methanol makes dissolving, is transferred in the measuring bottle of 50ml, adds 50% methanol and is diluted to scale, shake up, filter, get subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
The every 1ml of this product contains Flos Lonicerae and Herba Solidaginis in chlorogenic acid (C16H18O9), must not be less than 0.40mg.
3. detection method according to claim 1 and 2 is characterized in that, described compound herba solidaginis spray is made according to following method:
Get above seven flavor medicine material, soaked 2～3 hours, add thermal distillation, collect Aromatic water, standby 1～4 ℃ temperature lower seal cold preservation, extracting solution device is in addition preserved; Medicinal residues decoct with water secondary, 1.5 hours for the first time, 1 hour for the second time, decocting liquid and said extracted liquid merged, and filtered, it is 1.10～1.13 clear paste that filtrate is condensed into 45 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 70%, stir, left standstill 24 hours, filter, reclaiming ethanol and being condensed into 45 ℃ of relative densities is 1.20 clear paste; Add Aromatic water, mixing, cold preservation filters, and filtrate adds steviosin, potassium sorbate, and mixing adds water to ormal weight, fill, promptly.
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|---|---|---|---|
| CN200910306184A CN101637506A (en) | 2009-08-27 | 2009-08-27 | Method for detecting compound herba solidaginis spray |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103518912A (en) * | 2013-10-22 | 2014-01-22 | 张家界航空工业职业技术学院 | Traditional Chinese medicinal health-protection tea for treating chronic pharyngitis and preparation method of traditional Chinese medicinal health-protection tea |
| CN113262244A (en) * | 2021-06-02 | 2021-08-17 | 无锡简玺生物科技有限公司 | Enzymolysis extraction method of solidago virgaurea and application of product of solidago virgaurea |
-
2009
- 2009-08-27 CN CN200910306184A patent/CN101637506A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103518912A (en) * | 2013-10-22 | 2014-01-22 | 张家界航空工业职业技术学院 | Traditional Chinese medicinal health-protection tea for treating chronic pharyngitis and preparation method of traditional Chinese medicinal health-protection tea |
| CN113262244A (en) * | 2021-06-02 | 2021-08-17 | 无锡简玺生物科技有限公司 | Enzymolysis extraction method of solidago virgaurea and application of product of solidago virgaurea |
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Application publication date: 20100203 |