CN109991359B - Quality control method of Chinese medicinal composition with cough relieving and phlegm eliminating effects - Google Patents
Quality control method of Chinese medicinal composition with cough relieving and phlegm eliminating effects Download PDFInfo
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Abstract
The invention relates to a quality control method of a specific traditional Chinese medicine composition for relieving cough and eliminating phlegm, and the traditional Chinese medicine composition is already disclosed. In particular to a quality control method of an identification method and a content determination method of the traditional Chinese medicine composition for relieving cough and eliminating phlegm. The applicant of the invention systematically researches the chemical components of the volatile oil in the product and carries out content measurement, thereby determining the quality control standard of the volatile oil, leading the quality of the product to reach the standard specifically and accurately, and establishing a model for researching the quality standard of the traditional Chinese medicine composition containing the volatile oil and the preparation thereof.
Description
Technical Field
The invention relates to a quality control method of a specific traditional Chinese medicine composition for relieving cough and eliminating phlegm.
Background
The invention relates to a traditional Chinese medicine composition which comprises 9 traditional Chinese medicines of Japanese ardisia herb, loquat leaf, ephedra herb, bitter apricot seed, mint, dried orange peel, bamboo shavings, heartleaf houttuynia herb and honey-fried licorice root. Has the functions of relieving cough and eliminating phlegm, and is used for treating the exterior syndrome, excess syndrome, heat syndrome and exterior cold and interior heat syndrome of cough and asthma. Can be used for treating acute bronchitis, acute episode of chronic bronchitis, etc.
The composition of the invention has already applied for Chinese invention patent on 24/3/2009 and is granted, and the patent numbers are: ZL 200910048132.0. Although the invention provides the preparation method of the composition, the quality control of the product prepared by the method is required to ensure the stability and controllability of the product quality, and the specificity of the quality control of the traditional Chinese medicine product is particularly required to have specificity.
Disclosure of Invention
The invention aims to disclose a quality control method of a traditional Chinese medicine composition with the functions of relieving cough and eliminating phlegm, which is realized by the following technical scheme:
a quality control method of Chinese medicinal composition with cough relieving and phlegm eliminating effects comprises quality control of identification method and content determination method.
A quality control method of Chinese medicinal composition with cough relieving and phlegm eliminating effects comprises adopting bergenin, folium Eriobotryae, ephedrine hydrochloride, hesperidin, benzaldehyde, methyl n-nonanone, Mentholum, and limonene as reference, and performing identification method quality control.
A quality control method of Chinese medicinal composition with cough relieving and phlegm eliminating effects comprises adopting bergenin, ephedrine hydrochloride, pseudoephedrine hydrochloride, and benzaldehyde as reference substances, and performing content determination and quality control.
Advantages of the invention
In qualitative aspect, thin layer identification of herba Ardisiae Japonicae, folium Eriobotryae, herba Ephedrae and pericarpium Citri Tangerinae, identification of volatile oil in semen Armeniacae amarum, herba Menthae and herba Houttuyniae, and identification of benzaldehyde in semen Armeniacae amarum are set as quality control standard; in terms of quantification, the determination of the representative components of the volatile oils in ephedra, Japanese ardisia, bitter apricot seed, peppermint and houttuynia cordata is subject to quality control standards. The composition has specificity and feasibility, and can effectively ensure the quality of the composition.
The quality of the Chinese medicinal composition is researched conventionally without controlling the quality of the volatile oil, and the applicant of the invention systematically researches the chemical components of the volatile oil in the product and performs content measurement, thereby determining the quality control standard of the volatile oil, ensuring that the quality of the product reaches the standard specifically and accurately, and establishing a model for researching the quality standards of the Chinese medicinal composition containing the volatile oil and the preparation thereof.
Detailed Description
Example 1 [ identification method ]
Taking 1ml of the product, adding 20ml of methanol, shaking up, filtering, and concentrating the filtrate to about 2ml to be used as a test solution. Adding methanol into bergenin control to obtain solution containing 0.5mg per 1ml, and making into control solution. According to thin layer chromatography test, sucking the above two solutions 5 μ l each, dropping on the same silica gel G thin layer plate, developing with chloroform-ethyl acetate-methanol (5:4:2) as developing agent, taking out, air drying, and spraying with mixed solution of 1% ferric trichloride-1% potassium ferricyanide (1: 1). Spots of the same color appear in the chromatogram of the test solution at positions corresponding to those in the chromatogram of the control solution.
Example 2 [ identification method ]
Collecting 5ml of the product, adding water saturated n-butanol, shaking for 4 times, extracting with 10ml of water, mixing n-butanol solutions, washing with ammonia solution for 2 times, 20ml of water, mixing n-butanol solutions, evaporating to dryness, dissolving the residue with 5ml of water, cooling, passing through D101 type macroporous adsorbent resin column (diameter 1.5cm, length 8 cm), eluting with 50ml of water, discarding water solution, eluting with diluted ethanol to colorless, collecting eluate, evaporating to dryness, dissolving the residue with 1ml of methanol to obtain sample solution. Taking 1g of loquat leaf as a control medicinal material, adding 100ml of water, decocting for 1 hour, filtering, and preparing the filtrate into a control medicinal material solution by the same method. Performing thin layer chromatography test, sucking the above two solutions 20 μ l each, dropping on the same silica gel G thin layer plate, developing with cyclohexane-ethyl acetate-glacial acetic acid (8: 4: 0.1) as developing agent, taking out, air drying, spraying with 5% vanillin sulfuric acid solution, and heating at 105 deg.C until the spots are clearly developed. Spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the control solution.
Example 3 [ identification method ]
Taking 10ml of the product, adding several drops of concentrated ammonia test solution, adding chloroform for extraction for 2 times, 10ml each time, mixing chloroform, evaporating to dryness, adding 1ml of methanol into residue for dissolving, filtering, and collecting filtrate as test solution. Adding methanol into ephedrine hydrochloride control to obtain solution containing 0.5mg per 1ml as control solution. Performing thin layer chromatography test, sucking the above two solutions 5 μ l each, dropping on the same silica gel G thin layer plate, developing with chloroform-methanol-concentrated ammonia solution (20:5: 0.5) as developing agent, taking out, air drying, spraying with ninhydrin solution, and heating at 105 deg.C until the spots are clearly developed. The same red spot appears on the chromatogram of the test solution at the position corresponding to the chromatogram of the control solution.
Example 4 [ identification method ]
Taking 20ml of the product, steaming the product on a water bath till the product is nearly dry, adding 10g of diatomite, grinding the mixture evenly, adding 30ml of ethanol, carrying out ultrasonic treatment for 20 minutes, cooling the mixture, filtering the mixture, and concentrating the filtrate to about 5ml to be used as a test solution; adding methanol into hesperidin control to obtain saturated solution as control solution. According to the thin layer chromatography test, sucking 10 μ l of each of the two solutions, respectively dropping on the same silica gel G thin layer plate prepared from 0.5% sodium hydroxide solution, developing with ethyl acetate-methanol-water (100:17:13) as developing agent, taking out, air drying, spraying with 1% aluminum trichloride methanol solution, drying with hot air, and inspecting under ultraviolet lamp (365 nm). The test chromatogram shows fluorescent spots of the same color at the positions corresponding to those of the control chromatogram.
Example 5 [ identification method ]
Taking 5ml of the product, placing the product in a 10ml measuring flask, adding ethyl acetate, carrying out ultrasonic treatment for 15min, shaking up, standing, and taking supernatant as a test solution. And adding ethyl acetate into benzaldehyde as control solution to obtain solution containing 1 mg/ml. The solution was precisely aspirated at 1. mu.l each, and the solution was injected into a gas chromatograph and measured by gas chromatography. Chromatographic conditions are as follows: a chromatographic column (30 m x 320 μm, 0.25 μm) using cross-linked bonded polyethylene glycol as a stationary phase; sample inlet temperature: 250 ℃; detector temperature: 270 ℃; split-flow sample introduction, split-flow ratio: 20: 1; carrier gas: nitrogen, flow rate: 1 ml/min; temperature programming: the temperature was maintained at 50 ℃ for 10min and then increased to 150 ℃ at a rate of 5 ℃/min. The test solutions peak at the same retention times as the control solutions, respectively.
Example 6 [ identification method ]
Taking 0.1ml of volatile oil in bitter almond, mint and houttuynia cordata, putting the volatile oil in a 10ml measuring flask, adding ethyl acetate to a constant volume, and shaking up uniformly to obtain a test solution. Taking benzaldehyde, methyl n-nonanone, menthol and limonene as reference substances, and adding ethyl acetate to obtain solutions containing 1mg of the reference substances per ml, and using the solutions as reference substance solutions. The solution was precisely aspirated at 1. mu.l each, and the solution was injected into a gas chromatograph and measured by gas chromatography. Chromatographic conditions are as follows: a chromatographic column (30 m x 320 μm, 0.25 μm) using cross-linked bonded polyethylene glycol as a stationary phase; sample inlet temperature: 250 ℃; detector temperature: 270 ℃; split-flow sample introduction, split-flow ratio: 20: 1; carrier gas: nitrogen, flow rate: 1 ml/min; temperature programming: the temperature was maintained at 50 ℃ for 10min and then increased to 150 ℃ at a rate of 5 ℃/min. The test solutions peak at the same retention times as the control solutions, respectively.
Example 7 [ determination of Ardisia japonica content ]
Octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system applicability tests; acetonitrile-water (12: 88) is used as a mobile phase; the flow rate is 1.0 ml/min; the detection wavelength was 275 nm. The theoretical plate number is not less than 3000 calculated according to bergenin peak.
Preparation of control solution A proper amount of bergenin control is precisely weighed, and added with methanol to obtain a solution containing 25 μ g of bergenin per 1 ml.
Preparation of a test solution, precisely measuring 1ml of the test solution, eluting on a neutral alumina column (100-200 meshes, 1g and 1cm in inner diameter) with methanol, collecting about 30ml of eluent, placing the eluent in a 50ml measuring flask, diluting to a scale with methanol, shaking uniformly, and filtering to obtain the test solution.
The determination method comprises precisely sucking 20 μ l of reference solution and test solution, injecting into liquid chromatograph, determining, and calculating to obtain product containing bergenin (C) per 1ml14H16O9) Calculated, the content of the active ingredient should not be less than 1.1 mg.
Example 8 [ determination of Ephedra ] herba Ephedrae content ]
Chromatographic conditions and system applicability test using octadecylsilane chemically bonded silica as filler, acetonitrile: 0.1% phosphoric acid (4: 96) as mobile phase, and the detection wavelength was 207 nm. The number of theoretical plates is not less than 3000 calculated according to the peak of ephedrine hydrochloride and pseudoephedrine hydrochloride.
Preparation of control solution 10mg of ephedrine hydrochloride control and 15mg of pseudoephedrine hydrochloride were weighed precisely, placed in 100ml measuring bottles, dissolved and diluted to scale with methanol, and shaken well. Precisely measuring 5ml of the ephedrine hydrochloride solution and 1ml of the pseudoephedrine hydrochloride solution respectively, placing into a 50ml measuring flask, diluting with mobile phase to scale, and shaking to obtain the final product (each 1ml contains 10 μ g of ephedrine hydrochloride and 3 μ g of pseudoephedrine hydrochloride).
Precisely measuring 1ml of the sample solution, placing in a separating funnel, adding 5ml of ammonia water, shaking, extracting with diethyl ether for 5 times (10 ml each time), mixing the diethyl ether solutions, adding 5ml of 5% methanol hydrochloride solution, shaking, recovering solvent in 40 deg.C water bath, dissolving the residue with mobile phase, quantitatively transferring to a 25ml measuring flask, adding mobile phase to dilute to scale, shaking, and filtering.
The determination method comprises precisely sucking 20 μ l of reference solution and test solution, respectively, injecting into liquid chromatograph, determining, and calculating to obtain a product containing ephedrine hydrochloride (C) for each 1ml of herba Ephedrae10H15NO & HCl) and pseudoephedrine hydrochloride (C)10H15NO & HCl) of not less than 0.30 mg.
Example 9 [ determination of volatile oil content ]
Chromatographic conditions are as follows: a chromatographic column (30 m x 320 μm, 0.25 μm) using cross-linked bonded polyethylene glycol as a stationary phase; sample inlet temperature: 250 ℃; detector temperature: 270 ℃; split-flow sample introduction, split-flow ratio: 20: 1; carrier gas: nitrogen, flow rate: 1 ml/min; temperature programming: the temperature was maintained at 50 ℃ for 10min and then increased to 150 ℃ at a rate of 5 ℃/min.
Preparation of reference solution 10mg of benzaldehyde reference substance was precisely weighed and placed in a 10ml measuring flask, and ethyl acetate was added to dissolve, and volume was determined, and shaking was performed to obtain the final product.
Preparing the sample solution by precisely measuring 0.5ml of volatile oil in semen Armeniacae amarum, herba Menthae and herba Houttuyniae, placing in a 50ml measuring flask, adding ethyl acetate to dissolve, fixing volume, and shaking.
The determination method comprises precisely sucking 1 μ l of reference solution and test solution respectively, injecting into gas chromatograph, and determining to obtain 1ml of benzaldehyde (C)7H6O) must not be less than 90 mg.
Claims (7)
1. A quality control method for Chinese medicinal composition with cough relieving and phlegm eliminating effects comprises herba Ardisiae Japonicae, folium Eriobotryae, herba Ephedrae, semen Armeniacae amarum, herba Menthae, pericarpium Citri Tangerinae, caulis Bambusae in Taenia, herba Houttuyniae, and radix Glycyrrhizae Preparata, and is characterized by quality control for identification method and content determination method;
the identification method comprises adopting bergenin, folium Eriobotryae, ephedrine hydrochloride, hesperidin, benzaldehyde, methyl-n-nonanone, Mentholum, and limonene as reference; the content determination method comprises adopting bergenin, ephedrine hydrochloride, pseudoephedrine hydrochloride, and benzaldehyde as reference substances;
the method using benzaldehyde as a reference substance comprises the following steps:
taking 5ml of the product, placing the product in a 10ml measuring flask, adding ethyl acetate, performing ultrasound for 15min, shaking up, standing, and taking supernatant as a test solution; adding ethyl acetate into benzaldehyde as control substance to obtain solution containing 1 mg/ml as control solution; precisely sucking 1 μ l of the above solutions, respectively, injecting into gas chromatograph, and measuring by gas chromatography;
chromatographic conditions are as follows: chromatographic column with cross-linked polyethylene glycol as stationary phase; sample inlet temperature: 250 ℃; detector temperature: 270 ℃; split-flow sample introduction, split-flow ratio: 20: 1; carrier gas: nitrogen, flow rate: 1 ml/min; temperature programming: keeping at 50 deg.C for 10min, and increasing to 150 deg.C at 5 deg.C/min; the sample solution peaks at the same retention time as the reference solution;
the method which adopts benzaldehyde, methyl-n-nonanone, menthol and limonene as reference substances comprises the following steps:
taking 0.1ml of volatile oil of bitter almond, mint and houttuynia cordata, putting the volatile oil into a 10ml measuring flask, adding ethyl acetate to a constant volume, and shaking up to be used as a test solution; taking benzaldehyde, methyl n-nonanone, menthol and limonene as reference substances, and adding ethyl acetate to obtain solutions containing 1mg of the reference substances per ml as reference substance solutions; precisely sucking 1 μ l of the above solutions, respectively, injecting into gas chromatograph, and measuring by gas chromatography;
chromatographic conditions are as follows: chromatographic column with cross-linked polyethylene glycol as stationary phase; sample inlet temperature: 250 ℃; detector temperature: 270 ℃; split-flow sample introduction, split-flow ratio: 20: 1; carrier gas: nitrogen, flow rate: 1 ml/min; temperature programming: keeping at 50 deg.C for 10min, and increasing to 150 deg.C at 5 deg.C/min; the test solution peaked at the same retention time as the control solution.
2. The quality control method of a Chinese medicinal composition with cough relieving and phlegm eliminating effects of claim 1, which is characterized in that bergenin is used as a reference substance, and the method comprises the following steps:
taking 1ml of the product, adding 20ml of methanol, shaking up, filtering, and concentrating the filtrate to about 2ml to be used as a test solution; adding methanol into bergenin reference to obtain a solution containing 0.5mg per 1ml as reference solution; according to a thin-layer chromatography test, sucking 5 mu l of each of the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, developing by taking trichloromethane-ethyl acetate-methanol as a developing agent in a ratio of 5:4:2, taking out, drying in the air, and spraying a mixed solution of 1% ferric trichloride and 1% potassium ferricyanide in a ratio of 1: 1; spots of the same color appear in the chromatogram of the test solution at positions corresponding to those in the chromatogram of the control solution.
3. The quality control method of a Chinese medicinal composition with cough relieving and phlegm eliminating effects as claimed in claim 1, which is characterized in that loquat leaves are used as reference, and the method comprises:
collecting 5ml of the product, adding water saturated n-butanol, shaking for 4 times, each time extracting for 10ml, mixing n-butanol solutions, washing with ammonia sample solution for 2 times, each time extracting for 20ml, mixing n-butanol solutions, evaporating to dryness, dissolving the residue with 5ml of water, cooling, passing through D101 type macroporous adsorbent resin column, eluting with 50ml of water, discarding water solution, eluting with diluted ethanol to colorless, collecting eluate, evaporating to dryness, dissolving the residue with 1ml of methanol to obtain sample solution; taking 1g of loquat leaf as a reference medicinal material, adding 100ml of water, decocting for 1 hour, filtering, and preparing the filtrate into a reference medicinal material solution by the same method; performing thin layer chromatography test, sucking the two solutions 20 μ l each, dropping on the same silica gel G thin layer plate, developing with cyclohexane-ethyl acetate-glacial acetic acid at a ratio of 8:4:0.1 as developing agent, taking out, air drying, spraying with 5% vanillin sulfuric acid solution, and heating at 105 deg.C until the spots are clearly developed; spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the control solution.
4. The quality control method of a Chinese medicinal composition with cough relieving and phlegm eliminating effects of claim 1, which is characterized in that ephedrine hydrochloride is used as a reference substance, and the method comprises:
taking 10ml of the product, adding several drops of concentrated ammonia test solution, adding chloroform for extraction for 2 times, 10ml each time, mixing chloroform, evaporating to dryness, adding 1ml of methanol into residue for dissolving, filtering, and collecting filtrate as test solution; adding methanol into ephedrine hydrochloride reference to obtain 0.5mg solution per 1ml as reference solution; performing thin-layer chromatography test, sucking the above two solutions 5 μ l each, dropping on the same silica gel G thin-layer plate respectively, developing with chloroform-methanol-concentrated ammonia solution at a ratio of 20:5:0.5 as developing agent, taking out, air drying, spraying with ninhydrin solution, heating at 105 deg.C until the spots are clearly developed; the same red spot appears on the chromatogram of the test solution at the position corresponding to the chromatogram of the control solution.
5. The quality control method of a Chinese medicinal composition with cough relieving and phlegm eliminating effects of claim 1, which is characterized in that hesperidin is used as a reference substance, and the method comprises the following steps:
taking 20ml of the product, steaming the product on a water bath till the product is nearly dry, adding 10g of diatomite, grinding the mixture evenly, adding 30ml of ethanol, carrying out ultrasonic treatment for 20 minutes, cooling the mixture, filtering the mixture, and concentrating the filtrate to about 5ml to be used as a test solution; adding methanol into hesperidin control to obtain saturated solution as control solution; performing thin-layer chromatography test, sucking 10 μ l of each of the two solutions, respectively dropping on the same silica gel G thin-layer plate prepared from 0.5% sodium hydroxide solution, developing with ethyl acetate-methanol-water at a ratio of 100:17:13 as developing agent, taking out, air drying, spraying with 1% aluminum trichloride methanol solution, drying with hot air, and inspecting under ultraviolet lamp; the test chromatogram shows fluorescent spots of the same color at the positions corresponding to those of the control chromatogram.
6. The quality control method of a Chinese medicinal composition with cough relieving and phlegm eliminating effects of claim 1, which is characterized in that bergenin is used as a reference substance to determine the content of Japanese ardisia herb, and the method comprises the following steps:
octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-water in a ratio of 12:88 is taken as a mobile phase; the flow rate is 1.0 ml/min; the detection wavelength is 275 nm; the theoretical plate number is not less than 3000 calculated according to bergenin peak;
preparation of control solutions: precisely weighing bergenin reference, and adding methanol to obtain solution containing 25 μ g of bergenin per 1 ml;
preparation of a test solution: precisely measuring 1ml of the product, loading on neutral alumina column, eluting with methanol, collecting about 30ml of eluate, placing in a 50ml measuring flask, diluting with methanol to scale, shaking, and filtering to obtain the final product;
the determination method comprises the following steps: precisely sucking 20 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, measuring, and calculating to obtain product containing herba Ardisiae Japonicae (calculated as bergenin) per 1ml not less than 1.1 mg.
7. The quality control method of a Chinese medicinal composition with cough relieving and phlegm eliminating effects of claim 1, which is characterized in that ephedrine hydrochloride and pseudoephedrine hydrochloride are used as reference substances to determine herba Ephedrae content, and the method comprises:
octadecylsilane chemically bonded silica is used as a filling agent, and the ratio of the filler to the octadecylsilane chemically bonded silica is 4: 96 acetonitrile-0.1% phosphoric acid is used as a mobile phase, and the detection wavelength is 207 nm; the number of theoretical plates is not less than 3000 calculated according to the peak of ephedrine hydrochloride and pseudoephedrine hydrochloride;
preparation of control solutions: precisely weighing ephedrine hydrochloride and pseudoephedrine hydrochloride reference substances, and adding methanol to obtain solutions containing ephedrine hydrochloride 10ug and pseudoephedrine hydrochloride 3ug per 1ml respectively;
preparation of a test solution: precisely measuring 1ml of the product, placing in a separating funnel, adding 5ml of ammonia water, shaking, adding diethyl ether for extraction for 5 times, 10ml each time, combining the diethyl ether solution, adding 5ml of 5% methanol hydrochloride solution, shaking, recovering solvent in 40 deg.C water bath, dissolving the residue with mobile phase, quantitatively transferring to a 25ml measuring flask, adding the mobile phase for dilution to scale, shaking, and filtering to obtain the final product;
the determination method comprises the following steps: precisely sucking 20 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, measuring, and calculating to obtain a product containing herba Ephedrae (1 ml) not less than 0.30mg calculated based on ephedrine hydrochloride and pseudoephedrine hydrochloride.
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