CN104007222A - Method for detecting ephedra-perilla leaf cough relieving capsule - Google Patents
Method for detecting ephedra-perilla leaf cough relieving capsule Download PDFInfo
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Abstract
The invention relates to a method for detecting an ephedra-perilla leaf cough relieving capsule, which is used for controlling the quality of the ephedra-perilla leaf cough relieving capsule. The method comprises the steps: performing qualitative identification on five Chinese medicinal herbs including ephedra, perilla leaf, lumbricus, burdock and fructus schizandrae in the ephedra-perilla leaf cough relieving capsule by adopting a thin layer chromatography; and determining the content of ephedrine hydrochloride in the ephedra-perilla leaf cough relieving capsule by adopting a high performance liquid chromatography. The method provided by the invention is simple and convenient to operate, scientific, reasonable, good in repeatability, and capable of well controlling the quality of the ephedra-perilla leaf cough relieving capsule, effectively monitoring the production, and increasing the safety of medication of a patient.
Description
Technical field
The present invention relates to a kind of detection method of compound Chinese medicinal preparation, relate in particular to a kind of detection method of SuHuang ZhiKe capsule, for the quality control of SuHuang ZhiKe capsule.
Background technology
Asthma is a kind of common respiratory disease, is universally acknowledged difficult medical problem.Cough variant asthma (CVA) is wherein a kind of.The patient who approximately has 5-6% be take continuation cough as cardinal symptom, without any, pant or have difficulty in breathing symptom, this disease is multiple is born in night or morning, and be often irritable cough, be often misdiagnosed as bronchitis and cause many patients to lack rational early treatment and finally develop into serious asthma.
The reason that causes CVA has a lot, as subjective factors such as patient's heredodiathesis itself, immune state, Psychophysiological state, endocrine and health status, in addition, the environmental factor such as allergen, virus infections, occupational factor, weather, medicine, motion and diet is also to cause CVA that the major reason of development occurs.Current along with environmental pollution is day by day serious, the quickening of social life rhythm, the incidence of disease of CVA increases day by day, serious impact people's healthy and normal life.
The medicine for the treatment of CVA be take Western medicine as main at present, and this is the following three class medicines of main application wherein: fugitive beta 2 receptor activator, inhaled and LTRA.Fugitive beta 2 receptor activator, inhaled are effective to Most patients, and small number of patients is invalid to these two kinds of medicines, need auxiliary LTRA or the oral glucocorticoid of using.Its formulation mostly is aerosol, dry powder doses, solution.Patient uses inconvenience, and need continuously, rule use one week later can onset, but after drug withdrawal, be prone to bounce-back.Because the treating asthma cycle is longer, need Long-term taking medicine in addition, can produce some corresponding bad reactions, and after drug withdrawal, there will be state of an illness bounce-back, be unfavorable for the treatment of asthma.
In recent years, along with the continuous intensification to the understanding of CVA, people start be familiar with and treat CVA from traditional Chinese medicine angle, have obtained good effect.Professor CHAO En-xiang (CN1605349A) thinks that CVA belongs to the category of " wind is coughed ".It is a kind of common clinical manifestation form of cough that wind is coughed, be common in cough after common cold and cough type asthma, show as and continue or repeated relapsing cough, few phlegm, choke and cough (especially sucking cold air, edible cold drink or motion postemphasis), pharynx is itched, cough aggravation, especially to attach most importance to night, meet the feature of the traditional Chinese medical science " wind is apt to change ".SuHuang ZhiKe capsule is the compound Chinese medicinal preparation of a kind of CVA for the treatment of, and its prescription comes from professor CHAO En-xiang more than 40 years clinical practice accumulation and the achievement in research to respiratory disorder.This prescription is comprised of Chinese ephedra, perilla leaf, earthworm, honey-fried FOLIUM ERIABOTRYAE, perillaseed, cicada slough, Qian Hu, great burdock achene, the fruit of Chinese magnoliavine.Its epheday intermedia, earthworm, cicada slough, perilla leaf, the root of purple-flowered peucedanum are the medicine of its dispelling wind, loose wind, in order to cough-relieving, relieve sore throat, antipruritic; Perilla seed, the fruit of Chinese magnoliavine, spasmolysis emergency; Great burdock achene, loguat leaf moistening lung and clearing heat, all medicines share, and Xin Wen declares lung, dispelling wind spasmolysis, sensible sending down abnormally ascending, open-minded phlegm is relievingd asthma, and makes the loose phlegm of the wind contraction solution that disappears, and lung qi declare to fall, and mechanism of qi is unobstructed, the object of finally reach whole adjustment, treating both principal and secondary aspect of disease.Clinical testing shows the respond well of this medicine, and bad reaction is also little compared with at present conventional Western medicine.
But still there is no at present a cover system, effectively, easy, the detection method of feasible SuHuang ZhiKe capsule, this is unfavorable for the production of this product, also can affect medicine enterprise and carry out aborning the quality monitoring of this product, cannot guarantee patient's drug safety and marketing in the future, therefore, set up corresponding detection method standard imperative.
Summary of the invention
The object of the present invention is to provide a kind of detection method of SuHuang ZhiKe capsule, thereby improve SuHuang ZhiKe capsule quality controllability, guarantee the stable of product quality.
Specifically, the invention provides a kind of detection method of SuHuang ZhiKe capsule, it is characterized in that this detection method adopts the qualitative discriminating of thin-layered chromatography to SuHuang ZhiKe capsule epheday intermedia, perilla leaf, earthworm, great burdock achene, fruit of Chinese magnoliavine gomi herbs; And adopt high performance liquid chromatography to measure the content of ephedrine hydrochloride in SuHuang ZhiKe capsule.
In preferred embodiment of the present invention, the qualitative discriminating of SuHuang ZhiKe capsule epheday intermedia, perilla leaf, earthworm, great burdock achene, fruit of Chinese magnoliavine gomi herbs comprises the following steps:
A: Chinese ephedra: get SuHuang ZhiKe capsule content 3g, add strong ammonia solution 1ml moistening, add methenyl choloride 20ml, add hot reflux 1 hour, filter, filtrate evaporate to dryness, residue adds ethanol 1ml to be made to dissolve, as need testing solution.Separately get ephedrine hydrochloride reference substance, with methyl alcohol, dissolve and make every 1ml containing the solution of 1mg, in contrast product solution.According to thin-layered chromatography test, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with methenyl choloride-methyl alcohol-strong ammonia solution (20 ﹕ 5 ﹕ 0.5), be developping agent, launch, take out, dry, spray, with ninhydrin solution, is dried approximately 5 minutes at 105 ℃.In test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color.
B: perilla leaf: get SuHuang ZhiKe capsule content 10g, put in 500ml round-bottomed flask, add water 250ml and beaded glass number, connect volatile oil determination apparatus, from analyzer upper end, Jia Shui makes to be full of scale part, and till overflow enters flask, add again sherwood oil (60～90 ℃) 1.5ml, connect reflux condenser, be heated to boil, and keep micro-and boil approximately 2 hours, get petroleum ether layer as need testing solution.Separately get perilla leaf control medicinal material 0.7g, be made in the same way of control medicinal material solution.According to thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with sherwood oil (60～90 ℃)-ethyl acetate (19 ﹕ 1), be developping agent, launch, take out, dry, spray, with 5% vanillic aldehyde hydrochloric acid solution, is dried several minutes at 105 ℃.In test sample chromatogram with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.
C: earthworm: get SuHuang ZhiKe capsule content 5g, add chloroform 20ml, add hot reflux 1 hour, filter, filtrate evaporate to dryness, residue adds ethanol 1ml to be made to dissolve, as need testing solution.Separately get earthworm control medicinal material 0.5g, be made in the same way of control medicinal material solution.According to thin-layered chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate (9 ﹕ 1), be developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is put under ultraviolet lamp (365nm) and is inspected.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
D: great burdock achene: get great burdock achene control medicinal material 0.5g, add ethanol 20ml, ultrasonic processing 20 minutes, filters, and filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, in contrast medicinal material solution.Separately get arctiin reference substance, with ethanol, make every 1ml containing the solution of 5mg, in contrast product solution.According to thin-layered chromatography, test, draw [earthworm] and differentiate need testing solution 5 μ l and above-mentioned control medicinal material solution and each the 3 μ l of reference substance solution under item, put respectively on same silica gel g thin-layer plate, methenyl choloride-the Methanol-water (40 ﹕ 8 ﹕ 1) of take is developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 105 ℃ clear.In test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, the spot of aobvious same color.
E: the fruit of Chinese magnoliavine: get fruit of Chinese magnoliavine control medicinal material 0.5g, add methenyl choloride 10ml, ultrasonic processing 20 minutes, filters, and filtrate volatilizes, adds ethanol 1ml and makes to dissolve, in contrast medicinal material solution.Separately get schizandrin A reference substance, with methenyl choloride, make every 1ml containing the solution of 1mg, in contrast product solution.According to thin-layered chromatography, test, need testing solution 5 μ l under absorption [earthworm] discriminating item and above-mentioned control medicinal material solution, each 3 μ l of reference substance solution, put respectively on same silica GF254 thin layer plate, the upper solution of sherwood oil (30～60 ℃)-ethyl formate-formic acid (15 ﹕ 5 ﹕ 1) of take is developping agent, launch, take out, dry, put under ultraviolet lamp (254nm) and inspect.In test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, the spot of aobvious same color.
In another preferred embodiment of the present invention, adopt high-efficient liquid phase technique to carry out assay to the mode of the Herba Ephedrae application isocratic elution in SuHuang ZhiKe capsule.Every capsules contains Chinese ephedra (with ephedrine hydrochloride (C
10h
15nOHCl) meter) must not be lower than 2.0mg, its detection method is:
A, chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Acetonitrile-water-phosphoric acid-the triethylamine (1.5 ﹕ 98.3 ﹕ 0.1 ﹕ 0.1) of take is mobile phase; Detection wavelength is 205nm.Number of theoretical plate is pressed ephedrine hydrochloride peak and is calculated, and should be not less than 6000.
The preparation precision of b, reference substance solution takes ephedrine hydrochloride reference substance 10mg, put in 50ml volumetric flask, with 0.l mol/L dissolve with hydrochloric acid solution and be diluted to scale, shake up, precision measures 25ml, puts in 100ml volumetric flask, with 0.l mol/L hydrochloric acid solution, is diluted to scale, shake up, obtain (hydrochloric ephedrine 50 μ g in every 1ml).
This product content under this product content uniformity item is got in the preparation of c, need testing solution, and porphyrize, gets 0.3g, accurately weighed, to put in tool plug conical flask, precision adds 0.l mol/L hydrochloric acid solution 25ml, close plug, weighed weight, ultrasonic processing (power 100w, frequency 20KHZ) 30 minutes, take out, let cool, weighed weight again, supplies the weight of less loss with 0.l mol/L hydrochloric acid solution, filter, shake up, obtain.
D, determination method be accurate reference substance solution and each l0 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, with the content of ephedrine hydrochloride in calculated by peak area SuHuang ZhiKe capsule.
In another preferred embodiment of the present invention, the detection method of described SuHuang ZhiKe capsule also comprises following proterties discrimination method: the content of SuHuang ZhiKe capsule is tan particle; The micro-perfume (or spice) of gas, mildly bitter flavor.
In another preferred embodiment of the present invention, the detection method of described SuHuang ZhiKe capsule also comprises the inspection that meets every regulation relevant under capsule item (appendix I L of Chinese Pharmacopoeia version in 2005).
The advantage of detection method of the present invention is: 1, this law has been carried out thin-layer chromatography evaluation to the endemic element in SuHuang ZhiKe capsule simultaneously, can the comprehensive reaction SuHuang ZhiKe capsule of science in the existence of each taste medicine of monarch.2, high-efficient liquid phase technique adopts the mode of isocratic elution to measure the content of the effective constituent ephedrine hydrochloride in the monarch drug in a prescription-Herba Ephedrae in prescription, easy and simple to handle, scientific and reasonable.In a word, in the reaction prescription that the present invention can system, represent composition, and easy and simple to handle, scientific and reasonable, be conducive to SuHuang ZhiKe capsule quality control comprehensively.
Accompanying drawing explanation
Fig. 1 is Herba Ephedrae thin layer identification color spectrogram.
Fig. 2 is perilla leaf medicinal material thin layer identification color spectrogram.
Fig. 3 is earthworm medicinal material thin layer identification color spectrogram.
Fig. 4 is great burdock achene medicinal material thin layer identification color spectrogram.
Fig. 5 is schisandra chinensis medicinal material thin layer identification color spectrogram.
Fig. 6 is SuHuang ZhiKe capsule sample high-efficient liquid phase chromatogram.
Fig. 7 is ephedrine hydrochloride reference substance high-efficient liquid phase chromatogram.
Embodiment
By reading the following example, those skilled in the art will be better understood the present invention.These embodiment are only for explaining the present invention.
The experimental technique of unreceipted actual conditions in the embodiment of the present invention, conventionally according to normal condition, or the condition of advising according to raw material or commodity manufacturer.The reagent in unreceipted concrete source is the conventional reagent of market purchase.
Instrument: SPD-10Avp Ultraviolet Detector Japan Shimadzu company; Agilent 1200DAD high pressure liquid chromatograph (Sunfire C18150 * 4.6mm chromatographic column); HN1006 supersonic cleaning machine In South China ultrasonic device factory; HM202 electronic analytical balance Japan AND company.
Material: silica G is purchased from Qingdao Marine Chemical Co., Ltd.; Ephedrine hydrochloride, arctiin, schizandrin A reference substance are purchased from Nat'l Pharmaceutical & Biological Products Control Institute; Acetonitrile is that chromatographically pure is purchased from Di Ma company.All the other reagent are pure for analyzing.
Prescription: Chinese ephedra 556g, perilla leaf 556g, earthworm 556g, sweet loguat leaf 556g, stir-fry perilla seed 332g, cicada slough 444g, root of purple-flowered peucedanum 444g, stir-baked FRUCTUS ARCTII 556g, fruit of Chinese magnoliavine 444g.
Method for making: above nine taste medicines, perilla leaf, the root of purple-flowered peucedanum are soaked 1 hour, extract volatile oil 8 hours, collect volatile oil, and the another device of aqueous solution after distillation is collected; Volatile oil beta-cyclodextrin inclusion compound, dry, pulverize into fine powder below at 40 ℃.Chinese ephedra, the fruit of Chinese magnoliavine add 80% ethanol, add hot reflux three times, adding for the first time 8 times of amounts extracts 1.5 hours, add for the second time 6 times of amounts and extract 1.5 hours, add for the third time 6 times of amounts and extract 1.5 hours, filter, merging filtrate, reclaim ethanol, and be concentrated into the thick paste that relative density is 1.25～1.30 (50 ℃), standby.The five tastes boilings such as all the other earthworms three times, adding for the first time 10 times of water gagings decocts 1 hour, adding for the second time 8 times of water gagings decocts 1 hour, adding for the third time 8 times of water gagings decocts 1 hour, filter, aqueous solution after filtrate and above-mentioned distillation merges, being concentrated into relative density is 1.10 (50 ℃ of surveys), adding ethanol makes to reach 70% containing alcohol amount, refrigerate 24 hours, filter, filtrate recycling ethanol, and be condensed into the thick paste that relative density is 1.25～1.30 (50 ℃), merge with above-mentioned thick paste, 70 ℃ of following drying under reduced pressure become dry extract, dry extract is broken into fine powder, merge with above-mentioned fine powder, add appropriate amount of starch, mix, with 90～95% appropriate amount of ethanols, granulate, dry, cross after the whole grain of 40 mesh sieves, incapsulate, make 1000, obtain.
Proterties discrimination method is: this product is capsule, and content is tan particle; The micro-perfume (or spice) of gas, mildly bitter flavor.
During inspection, should meet every regulation relevant under capsule item (appendix I L of Chinese Pharmacopoeia version in 2005).
When thin layer is differentiated, respectively in SuHuang ZhiKe capsule: Chinese ephedra, perilla leaf, earthworm, great burdock achene, the fruit of Chinese magnoliavine detect, its method is:
A: Chinese ephedra: get SuHuang ZhiKe capsule content 3g, add strong ammonia solution 1ml moistening, add methenyl choloride 20ml, add hot reflux 1 hour, filter, filtrate evaporate to dryness, residue adds ethanol 1ml to be made to dissolve, as need testing solution.Separately get ephedrine hydrochloride reference substance, with methyl alcohol, dissolve and make every 1ml containing the solution of 1mg, in contrast product solution.According to thin-layered chromatography test, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with methenyl choloride-methyl alcohol-strong ammonia solution (20 ﹕ 5 ﹕ 0.5), be developping agent, launch, take out, dry, spray, with ninhydrin solution, is dried approximately 5 minutes at 105 ℃.In test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot (seeing Fig. 1) of aobvious same color.
B: perilla leaf: get SuHuang ZhiKe capsule content 10g, put in 500ml round-bottomed flask, add water 250ml and beaded glass number, connect volatile oil determination apparatus, from analyzer upper end, Jia Shui makes to be full of scale part, and till overflow enters flask, add again sherwood oil (60～90 ℃) 1.5ml, connect reflux condenser, be heated to boil, and keep micro-and boil approximately 2 hours, get petroleum ether layer as need testing solution.Separately get perilla leaf control medicinal material 0.7g, be made in the same way of control medicinal material solution.According to thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with sherwood oil (60～90 ℃)-ethyl acetate (19 ﹕ 1), be developping agent, launch, take out, dry, spray, with 5% vanillic aldehyde hydrochloric acid solution, is dried several minutes at 105 ℃.In test sample chromatogram with the corresponding position of control medicinal material chromatogram on, the spot (seeing Fig. 2) of aobvious same color.
C: earthworm: get SuHuang ZhiKe capsule content 5g, add chloroform 20ml, add hot reflux 1 hour, filter, filtrate evaporate to dryness, residue adds ethanol 1ml to be made to dissolve, as need testing solution.Separately get earthworm control medicinal material 0.5g, be made in the same way of control medicinal material solution.According to thin-layered chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate (9 ﹕ 1), be developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is put under ultraviolet lamp (365nm) and is inspected.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot (seeing Fig. 3) of aobvious same color.
D: great burdock achene: get great burdock achene control medicinal material 0.5g, add ethanol 20ml, ultrasonic processing 20 minutes, filters, and filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, in contrast medicinal material solution.Separately get arctiin reference substance, with ethanol, make every 1ml containing the solution of 5mg, in contrast product solution.According to thin-layered chromatography, test, draw [earthworm] and differentiate need testing solution 5 μ l and above-mentioned control medicinal material solution and each the 3 μ l of reference substance solution under item, put respectively on same silica gel g thin-layer plate, methenyl choloride-the Methanol-water (40 ﹕ 8 ﹕ 1) of take is developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 105 ℃ clear.In test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, the spot (seeing Fig. 4) of aobvious same color.
E: the fruit of Chinese magnoliavine: get fruit of Chinese magnoliavine control medicinal material 0.5g, add methenyl choloride 10ml, ultrasonic processing 20 minutes, filters, and filtrate volatilizes, adds ethanol 1ml and makes to dissolve, in contrast medicinal material solution.Separately get schizandrin A reference substance, with methenyl choloride, make every 1ml containing the solution of 1mg, in contrast product solution.According to thin-layered chromatography, test, need testing solution 5 μ l under absorption [earthworm] discriminating item and above-mentioned control medicinal material solution, each 3 μ l of reference substance solution, put respectively on same silica GF254 thin layer plate, the upper solution of sherwood oil (30～60 ℃)-ethyl formate-formic acid (15 ﹕ 5 ﹕ 1) of take is developping agent, launch, take out, dry, put under ultraviolet lamp (254nm) and inspect.In test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, the spot (seeing Fig. 5) of aobvious same color.
Adopt high-efficient liquid phase technique to carry out assay to the mode of the Chinese ephedra application isocratic elution in SuHuang ZhiKe capsule.Every capsules contains Chinese ephedra with ephedrine hydrochloride (C
10h
15nOHCl) meter, must not be lower than 2.0mg.Its detection method is:
A, chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Acetonitrile-water-phosphoric acid-the triethylamine (1.5 ﹕ 98.3 ﹕ 0.1 ﹕ 0.1) of take is mobile phase; Detection wavelength is 205nm.Number of theoretical plate is pressed ephedrine hydrochloride peak and is calculated, and should be not less than 6000.
The preparation precision of b, reference substance solution takes ephedrine hydrochloride reference substance 10mg, put in 50ml volumetric flask, with 0.l mol/L dissolve with hydrochloric acid solution and be diluted to scale, shake up, precision measures 25ml, puts in 100ml volumetric flask, with 0.l mol/L hydrochloric acid solution, is diluted to scale, shake up, obtain (hydrochloric ephedrine 50 μ g in every 1ml).
This product content under this product content uniformity item is got in the preparation of c, need testing solution, and porphyrize, gets 0.3g, accurately weighed, to put in tool plug conical flask, precision adds 0.l mol/L hydrochloric acid solution 25ml, close plug, weighed weight, ultrasonic processing (power 100w, frequency 20KHZ) 30 minutes, take out, let cool, weighed weight again, supplies the weight of less loss with 0.l mol/L hydrochloric acid solution, filter, shake up, obtain.
D, determination method be accurate reference substance solution and each l0 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, with the content (seeing Fig. 5, Fig. 6) of calculated by peak area ephedrine hydrochloride.
Claims (5)
1. a detection method for SuHuang ZhiKe capsule, is characterized in that this detection method adopts the qualitative discriminating of thin-layered chromatography to SuHuang ZhiKe capsule epheday intermedia, perilla leaf, earthworm, great burdock achene, fruit of Chinese magnoliavine gomi herbs; And adopt high performance liquid chromatography to measure the content of ephedrine hydrochloride in SuHuang ZhiKe capsule.
2. the detection method of SuHuang ZhiKe capsule according to claim 1, is characterized in that the qualitative discriminating of SuHuang ZhiKe capsule epheday intermedia, perilla leaf, earthworm, great burdock achene, fruit of Chinese magnoliavine five kinds of Chinese medicine comprises the following steps:
A, Chinese ephedra: get SuHuang ZhiKe capsule content 3g, add strong ammonia solution 1ml moistening, add methenyl choloride 20ml, add hot reflux 1 hour, filter, filtrate evaporate to dryness, residue adds ethanol 1ml to be made to dissolve, as need testing solution; Separately get ephedrine hydrochloride reference substance, with methyl alcohol, dissolve and make every 1ml containing the solution of 1mg, in contrast product solution; According to thin-layered chromatography test, draw need testing solution 5 μ l, reference substance solution 2 μ l, put respectively on same silica gel thin-layer plate, with methenyl choloride-methyl alcohol-strong ammonia solution, 20 ﹕ 5 ﹕ 0.5 are developping agent, launch, and take out, dry, spray, with ninhydrin solution, is dried approximately 5 minutes at 105 ℃; In test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
B, perilla leaf: get SuHuang ZhiKe capsule content 10g, put in round-bottomed flask, add water 250ml and beaded glass number, connect volatile oil determination apparatus, from analyzer upper end, Jia Shui makes to be full of scale part, and till overflow enters flask, add again sherwood oil 1.5ml, connect reflux condenser, be heated to boil, and keep micro-and boil approximately 2 hours, get petroleum ether layer as need testing solution; Separately get perilla leaf control medicinal material 0.7g, be made in the same way of control medicinal material solution; According to thin-layered chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, with sherwood oil-ethyl acetate 19 ﹕ 1, be developping agent, launch, take out, to dry, spray, with 5% vanillic aldehyde hydrochloric acid solution, is dried several minutes at 105 ℃; In test sample chromatogram with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color;
C, earthworm: get SuHuang ZhiKe capsule content 5g, add chloroform 20ml, add hot reflux 1 hour, filter, filtrate evaporate to dryness, residue adds ethanol 1ml to be made to dissolve, as need testing solution; Separately get earthworm control medicinal material 0.5g, be made in the same way of control medicinal material solution; According to thin-layered chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel thin-layer plate, with benzene-ethyl acetate 9 ﹕ 1, be developping agent, launch, take out, to dry, spray, with 10% ethanol solution of sulfuric acid, is put under ultraviolet lamp 365nm and is inspected; In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color;
D, great burdock achene: get great burdock achene control medicinal material 0.5g, add ethanol 20ml, ultrasonic processing 20 minutes, filters, and filtrate volatilizes, residue adds ethanol 1ml to be made to dissolve, in contrast medicinal material solution; Separately get arctiin reference substance, with ethanol, make every 1ml containing the solution of 5mg, in contrast product solution; According to thin-layered chromatography, test, draw C and differentiate need testing solution 5 μ l and above-mentioned control medicinal material solution and each the 3 μ l of reference substance solution under item, put respectively on same silica gel thin-layer plate, methenyl choloride-Methanol-water 40 ﹕ 8 ﹕ 1 of take are developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 105 ℃ clear; In test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, the spot of aobvious same color;
E, the fruit of Chinese magnoliavine: get fruit of Chinese magnoliavine control medicinal material 0.5g, add methenyl choloride 10ml, ultrasonic processing 20 minutes, filters, and filtrate volatilizes, add ethanol 1ml and make to dissolve, in contrast medicinal material solution; Separately get schizandrin A reference substance, with methenyl choloride, make every 1ml containing the solution of 1mg, in contrast product solution; According to thin-layered chromatography, test, draw C and differentiate respectively 3 μ l of a lower need testing solution 5 μ l and above-mentioned control medicinal material solution, reference substance solution, put respectively on same silica gel thin-layer plate, the upper solution of sherwood oil-ethyl formate-formic acid 15 ﹕ 5 ﹕ 1 of take is developping agent, launch, take out, dry, put under ultraviolet lamp 254nm and inspect; In test sample chromatogram, respectively with control medicinal material and the corresponding position of reference substance chromatogram on, the spot of aobvious same color.
3. the detection method of SuHuang ZhiKe capsule according to claim 1 and 2, is characterized in that in SuHuang ZhiKe capsule, the assay of ephedrine hydrochloride comprises the following steps:
A, chromatographic condition and system suitability: with octadecylsilane chemically bonded silica, be filling agent; Acetonitrile-water-phosphoric acid-triethylamine 1.5 ﹕ 98.3 ﹕ 0.1 ﹕ 0.1 of take are mobile phase; Detection wavelength is 205nm; Number of theoretical plate is pressed ephedrine hydrochloride peak and is calculated, and should be not less than 6000;
The preparation of b, reference substance solution: precision takes ephedrine hydrochloride reference substance 10mg, put in 50ml volumetric flask, with 0.l mol/L dissolve with hydrochloric acid solution and be diluted to scale, shake up, precision measures 25ml, puts in 100ml volumetric flask, with 0.l mol/L hydrochloric acid solution, be diluted to scale, shake up, obtain, hydrochloric ephedrine 50 μ g in every 1ml;
The preparation of c, need testing solution: get SuHuang ZhiKe capsule content, porphyrize, gets 0.3g, accurately weighed, to put in tool plug conical flask, precision adds 0.l mol/L hydrochloric acid solution 25ml, close plug, weighed weight, ultrasonic processing 30 minutes, take out, let cool, more weighed weight, with 0.l mol/L hydrochloric acid solution, supply the weight of less loss, filter, shake up, obtain;
D, determination method: precision is drawn reference substance solution and each l0 μ l of need testing solution respectively, injection liquid chromatography, measures, with the content of ephedrine hydrochloride in calculated by peak area SuHuang ZhiKe capsule; Every capsules contains Chinese ephedra in ephedrine hydrochloride, must not be lower than 2.0mg.
4. according to the detection method of the SuHuang ZhiKe capsule described in claim 1-3 any one, it is characterized in that the method also comprises following proterties discrimination method: the content of SuHuang ZhiKe capsule is tan particle; The micro-perfume (or spice) of gas, mildly bitter flavor.
5. according to the detection method of the SuHuang ZhiKe capsule described in claim 1-4 any one, it is characterized in that the method also comprises the inspection that meets every regulation relevant under appendix I L capsule item of Chinese Pharmacopoeia version in 2005.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792911A (en) * | 2015-05-13 | 2015-07-22 | 济南康众医药科技开发有限公司 | Method for identifying ephedra-monkshood-liquorice preparation |
| CN108490083A (en) * | 2018-03-02 | 2018-09-04 | 北京东方运嘉科技发展有限公司 | The quality determining method of SuHuang ZhiKe capsule |
| CN110687219A (en) * | 2019-08-23 | 2020-01-14 | 扬子江药业集团北京海燕药业有限公司 | Detection method of suhuang cough-relieving capsule fingerprint and application thereof |
| CN111983047A (en) * | 2020-07-03 | 2020-11-24 | 扬子江药业集团北京海燕药业有限公司 | Fingerprint detection method for volatile oil intermediate of perilla yellow cough-relieving capsule and application of fingerprint detection method |
| CN114224849A (en) * | 2022-01-26 | 2022-03-25 | 北京东方运嘉科技发展有限公司 | Suhuang cough relieving granules for children and preparation method thereof |
| CN114288340A (en) * | 2022-01-20 | 2022-04-08 | 北京大学 | Pharmaceutical composition for treating dandruff and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030157208A1 (en) * | 2001-12-20 | 2003-08-21 | Rui Wang | Cynomoriaceae extract and use in treating erectile dysfunction |
| CN1437982A (en) * | 2003-01-29 | 2003-08-27 | 黑龙江省中医研究院 | Medicinal composition for treating mycoplasma pneumonia and preparation method and quality-control method |
| CN1605349A (en) * | 2003-10-08 | 2005-04-13 | 晁恩祥 | Chinese traditional medicine for treating cough and variable asthma after cold and its preparation |
-
2014
- 2014-06-03 CN CN201410242575.4A patent/CN104007222A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030157208A1 (en) * | 2001-12-20 | 2003-08-21 | Rui Wang | Cynomoriaceae extract and use in treating erectile dysfunction |
| CN1437982A (en) * | 2003-01-29 | 2003-08-27 | 黑龙江省中医研究院 | Medicinal composition for treating mycoplasma pneumonia and preparation method and quality-control method |
| CN1605349A (en) * | 2003-10-08 | 2005-04-13 | 晁恩祥 | Chinese traditional medicine for treating cough and variable asthma after cold and its preparation |
Non-Patent Citations (4)
| Title |
|---|
| 余家奇 等: "抗感冒颗粒的制备及质量标准", 《时珍国医国药》 * |
| 国家药典委员会 编: "《中华人民共和国药典 2010年版 一部》", 31 January 2010 * |
| 毛颐晴 等: "高效液相色谱法测定咳喘宁口服液中麻黄碱的含量", 《江苏药学与临床研究》 * |
| 赵飞虎: "《豆丁网》", 25 August 2011 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792911A (en) * | 2015-05-13 | 2015-07-22 | 济南康众医药科技开发有限公司 | Method for identifying ephedra-monkshood-liquorice preparation |
| CN108490083A (en) * | 2018-03-02 | 2018-09-04 | 北京东方运嘉科技发展有限公司 | The quality determining method of SuHuang ZhiKe capsule |
| CN108490083B (en) * | 2018-03-02 | 2020-10-09 | 北京东方运嘉科技发展有限公司 | Quality detection method of Suhuang cough-relieving capsule |
| CN110687219A (en) * | 2019-08-23 | 2020-01-14 | 扬子江药业集团北京海燕药业有限公司 | Detection method of suhuang cough-relieving capsule fingerprint and application thereof |
| CN110687219B (en) * | 2019-08-23 | 2022-05-24 | 扬子江药业集团北京海燕药业有限公司 | Detection method of suhuang cough-relieving capsule fingerprint and application thereof |
| CN111983047A (en) * | 2020-07-03 | 2020-11-24 | 扬子江药业集团北京海燕药业有限公司 | Fingerprint detection method for volatile oil intermediate of perilla yellow cough-relieving capsule and application of fingerprint detection method |
| CN114288340A (en) * | 2022-01-20 | 2022-04-08 | 北京大学 | Pharmaceutical composition for treating dandruff and application thereof |
| CN114224849A (en) * | 2022-01-26 | 2022-03-25 | 北京东方运嘉科技发展有限公司 | Suhuang cough relieving granules for children and preparation method thereof |
| CN116270821A (en) * | 2022-01-26 | 2023-06-23 | 北京东方运嘉科技发展有限公司 | Perilla Huang Zhihai granule and preparation method and quality standard thereof |
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