CN114720620B

CN114720620B - Quality detection method of Shangxiaoting capsule

Info

Publication number: CN114720620B
Application number: CN202210204316.7A
Authority: CN
Inventors: 何艳; 胡小祥; 刘冠琼; 徐杨玉
Original assignee: Chenzhou Food And Drug Testing Center; Xiangnan University
Current assignee: Chenzhou Food And Drug Testing Center; Xiangnan University
Priority date: 2022-03-02
Filing date: 2022-03-02
Publication date: 2023-06-16
Anticipated expiration: 2042-03-02
Also published as: CN114720620A

Abstract

The invention relates to the technical field of medicine analysis, in particular to a quality detection method of a Shangxiaoting capsule, which comprises the steps of identifying angelica dahurica, identifying ephedrine hydrochloride and identifying glycyrrhizic acid, and can rapidly and accurately detect the ephedrine hydrochloride in the Shangxiaoting capsule and has the advantage of low toxicity; the quality detection method can identify glycyrrhizic acid in the Shangxiaoting capsule, and effectively improves the detection comprehensiveness of the Shangxiaoting capsule; the quality detection method has the advantages of easy operation and good repeatability.

Description

Quality detection method of Shangxiaoting capsule

Technical Field

The invention relates to the technical field of medicine analysis, in particular to a quality detection method of a Shangning capsule.

Background

The Shangfengting capsule is prepared from 6 medicinal materials including ephedra herb, fineleaf schizonepeta herb, dahurian angelica root, swordlike atractylodes rhizome (fried), tangerine peel, liquoric root group and the like, has the effect of dispersing wind-cold, and is clinically used for treating diseases such as exogenous wind-cold, aversion to cold, fever, serious limb acid, upper respiratory tract infection and the like. Herba Ephedrae in the recipe dispels wind-cold, and relieves cough and asthma as monarch drug; herba Schizonepetae for relieving exterior syndrome and dispelling pathogenic wind, radix Angelicae Dahuricae for relieving exterior syndrome, relieving pain, eliminating dampness, relieving stuffy nose, rhizoma Atractylodis for invigorating spleen and eliminating dampness, the three medicines are ministerial medicines for helping ephedra to relieve exterior syndrome, dispel cold, relieve pain and unblock orifices; dried orange peel, pericarpium citri reticulatae, dried dampness and phlegm, and relieving cough are adjuvant drugs; liquorice regulates the medicines, and phlegm-resolving and cough-relieving medicines are guiding medicines; the medicines are combined together to play the roles of dispersing wind-cold, relieving cough and asthma and inducing resuscitation. The Shangfengting capsule has the use popularity and the quality of the Shangxiaoting capsule needs to be strictly controlled.

The current quality standard of the Shangfengting capsule is thirteenth book and pharmacopoeia page (2002) No. 004 of "health department medicine standard Chinese medicine prescription preparation", the standard only carries chemical reaction, ephedrine hydrochloride and angelica dahurica thin layer chromatography identification and capsule inspection items, and has no other medicine identification and content measurement items, thus the standard is simple, and the quality of the whole medicine cannot be effectively and comprehensively controlled. Although the existing literature reports ephedrine hydrochloride determination methods, the existing ephedrine hydrochloride has more impurities, larger interference and harsh method requirements, and does not have good universal applicability. Moreover, although the existing TLC identification method of ephedrine hydrochloride has the problems of high toxicity and long time consumption.

In addition, although the existing research on quality control of the Shangning capsule is mainly content measurement, the mobile phase in each content measurement method mostly adopts gradient elution, the measurement process consumes long time, and the requirements on experimental conditions are high, so the durability and the applicability are not strong.

Disclosure of Invention

The invention aims to avoid the defects in the prior art and provide a quality detection method of a Shangfengting capsule, which can rapidly and accurately detect ephedrine hydrochloride in the Shangfengting capsule and has the advantage of low toxicity; the quality detection method can identify glycyrrhizic acid in the Shangxiaoting capsule, and improves detection comprehensiveness of the Shangxiaoting capsule; the quality detection method has the advantages of easy operation and good repeatability.

In order to achieve the above purpose, the present invention provides the following technical solutions:

the quality detection method of the Shangxiaoting capsule comprises the steps of identifying angelica dahurica, identifying ephedrine hydrochloride and identifying glycyrrhizic acid, wherein the quality detection method of the Shangxiaoting capsule comprises the steps of identifying the angelica dahurica, identifying ephedrine hydrochloride and identifying glycyrrhizic acid,

identification by TLCRadix angelicae, comprising: adding petroleum ether into the content of the capsule to be tested to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution, filtering the mixed solution, collecting filtrate, volatilizing the filtrate to a certain volume, and taking the volatilized filtrate as a solution to be tested of the angelica dahurica; adding petroleum ether into radix Angelicae Dahuricae as reference material to obtain mixed solution, performing ultrasonic treatment on the obtained mixed solution, standing, and collecting supernatant as radix Angelicae Dahuricae reference solution; respectively dispensing the solution to be detected and the reference solution of radix Angelicae Dahuricae on the same silica gel GF ₂₅₄ The thin layer plate is unfolded by using a petroleum ether-diethyl ether mixed solvent as an unfolding agent, and then taken out and dried; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 365nm ultraviolet lamp to see if the chromatogram of the radix Angelicae Dahuricae solution to be tested and the chromatogram of the radix Angelicae Dahuricae reference solution show fluorescent spots of the same color at corresponding positions; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 254nm ultraviolet lamp, and observing whether the chromatogram of the radix Angelicae Dahuricae solution to be detected and the chromatogram of the radix Angelicae Dahuricae reference solution show spots with the same color at corresponding positions; if the chromatogram of the solution to be detected of the angelica dahurica has fluorescent spots with the same color and spots with the same color as those of the solution of the angelica dahurica reference substance, the capsule to be detected of the common cold stop contains the angelica dahurica;

identifying ephedrine hydrochloride by TLC identification method, which comprises taking the content of the capsule to be detected, grinding, adding ethanol and ammonia test solution to obtain mixed solution, carrying out ultrasonic treatment on the mixed solution, filtering, collecting filtrate, evaporating filtrate to dryness, adding methanol into the evaporated filtrate residue to dissolve the residue, and taking the dissolved filtrate residue as ephedrine hydrochloride to be detected; preparing a negative sample without ephedra components, taking the negative sample, grinding, adding ethanol and ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution, filtering, collecting filtrate, evaporating filtrate to dryness, adding methanol into the evaporated filtrate residue to dissolve the filtrate residue, and taking the dissolved filtrate residue as a negative sample solution; taking ephedrine hydrochloride as reference substance, adding methanol to obtain solution, and taking the solution as ephedrine hydrochloride reference substance solution; the ephedrine hydrochloride solution to be detected, the negative sample solution and the ephedrine hydrochloride reference substance solution are respectively spotted on the same silica gel G plate, the mixed solution of chloroform-methanol-concentrated ammonia solution is taken as a developing agent, after the developing agent is developed, the mixed solution is taken out and dried, the mixed solution is sprayed with ninhydrin solution, and the mixed solution is heated until spots are clear in color development, the positions of the ephedrine hydrochloride solution to be detected, the negative sample solution and the ephedrine hydrochloride reference substance solution on the silica gel G plate are observed, for example, the color spectrum of the ephedrine hydrochloride solution to be detected and the color spectrum of the ephedrine hydrochloride reference substance solution show fluorescent spots with the same color on the corresponding positions, and if the negative sample solution is negative and has no interference, the cold stopping capsule to be detected contains ephedrine hydrochloride;

Identifying glycyrrhizic acid by adopting an HPLC identification method, which comprises taking the content of a capsule for treating injury and wind, grinding, adding ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution, filtering, collecting filtrate, steaming the filtrate until no ethanol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 with hydrochloric acid, extracting the aqueous solution with ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residue, adding 70% methanol into the residue to dissolve the residue, and fixing the volume to obtain the glycyrrhizic acid solution for treating injury and wind; preparing a negative sample without liquorice, weighing the negative sample, grinding, adding ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution, filtering, collecting filtrate, steaming the filtrate until no alcohol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 with hydrochloric acid, then extracting the aqueous solution with ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residues, adding 70% methanol into the residues to dissolve, and fixing the volume to obtain a negative sample solution; adding methanol into ammonium glycyrrhizate as reference substance to obtain ammonium glycyrrhizate reference substance solution; octadecylsilane chemically bonded silica is used as a filler, methanol-0.1% phosphoric acid is used as a mobile phase, the flow rate, detection wavelength and sample injection amount are adjusted, chromatographic peaks are observed, and if the retention time of the chromatographic peaks of the solution to be detected of glycyrrhizic acid is the same as that of the chromatographic peaks of the solution of ammonium glycyrrhizinate control, and negative interference is avoided, the capsule to be detected of the common cold stop contains liquorice.

In some embodiments of the present invention, in some embodiments,

identification of dahurian angelica root by TLC identification method, which comprises: taking 4-5 g of the content of the Shangfengting capsule to be detected, adding 15-30 mL of petroleum ether at 60-90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 15-30 min, filtering the mixed solution, collecting filtrate, volatilizing the filtrate to 0.5-1.5 mL, and taking the volatilized filtrate as a solution to be detected of angelica dahurica; taking 0.05-0.2 g of radix angelicae as a reference medicine, adding 15-30 mL of petroleum ether at 60-90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 15-30 min, standing, and taking supernatant as a radix angelicae reference substance solution; according to the thin layer chromatography of the four-part rule 0502 of the pharmacopoeia of the people's republic of China in 2020 edition, respectively sucking 8-15 mu L of the solution to be detected of the angelica dahurica and 8-15 mu L of the solution of the angelica dahurica reference substance, and respectively dispensing the solution to be detected of the angelica dahurica and the solution of the angelica dahurica reference substance on the same silica gel GF ₂₅₄ On the thin layer plate, the mixed solvent of petroleum ether and diethyl ether is used as developing agent, wherein the weight ratio of petroleum ether to diethyl ether is 0.5-1.2:1, the temperature of petroleum ether is 60-90 ℃, and the solution is prepared on silica gel GF ₂₅₄ After being unfolded on the thin layer plate, the thin layer plate is taken out and dried; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 365nm ultraviolet lamp to see if the chromatogram of the radix Angelicae Dahuricae solution to be tested and the chromatogram of the radix Angelicae Dahuricae reference solution show fluorescent spots of the same color at corresponding positions; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 254nm ultraviolet lamp, and observing whether the chromatogram of the radix Angelicae Dahuricae solution to be detected and the chromatogram of the radix Angelicae Dahuricae reference solution show spots with the same color at corresponding positions; if the chromatogram of the solution to be tested of the angelica dahurica has fluorescent spots with the same color and spots with the same color as those of the solution of the angelica dahurica reference substance, the capsule to be tested of the common cold stop contains the angelica dahurica.

In some embodiments of the present invention, in some embodiments,

identification of dahurian angelica root by TLC identification method, which comprises: taking 3.5g of the content of the Shangfengting capsule to be detected, adding 20mL of petroleum ether at 60-90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 20min, and filtering the mixed solutionCollecting filtrate, volatilizing the filtrate to 1mL, and taking the volatilized filtrate as a solution to be detected of the angelica dahurica; taking 0.1g of radix angelicae as a reference medicine, adding 20mL of petroleum ether at 60-90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 20min, standing, and taking supernatant as a radix angelicae reference solution; respectively sucking 10 μl of radix Angelicae Dahuricae solution to be detected and radix Angelicae Dahuricae reference substance solution according to thin layer chromatography of four-part rule 0502 of the 2020 edition of the pharmacopoeia of the people's republic of China, Will beThe solution to be detected of the angelica dahurica and the solution of the angelica dahurica reference substance are respectively spotted on the same silica gel GF ₂₅₄ On the thin layer plate, the mixed solvent of petroleum ether and diethyl ether is used as developing agent, wherein the weight ratio of petroleum ether to diethyl ether is 1:1, the temperature of petroleum ether is 60-90 ℃, and the solution is heated in silica gel GF ₂₅₄ After being unfolded on the thin layer plate, the thin layer plate is taken out and dried; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 365nm ultraviolet lamp to see if the chromatogram of the radix Angelicae Dahuricae solution to be tested and the chromatogram of the radix Angelicae Dahuricae reference solution show fluorescent spots of the same color at corresponding positions; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 254nm ultraviolet lamp, and observing whether the chromatogram of the radix Angelicae Dahuricae solution to be detected and the chromatogram of the radix Angelicae Dahuricae reference solution show spots with the same color at corresponding positions; if the chromatogram of the solution to be tested of the angelica dahurica has fluorescent spots with the same color and spots with the same color as those of the solution of the angelica dahurica reference substance, the capsule to be tested of the common cold stop contains the angelica dahurica.

In some embodiments of the present invention, in some embodiments,

identifying ephedrine hydrochloride by TLC identification method, which comprises taking 0.5-2 g of the content of Shangfengting capsule to be detected, grinding, adding 8-15 mL of ethanol and 3 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 5-15 min, filtering, collecting filtrate, evaporating the filtrate, adding 0.5-1.5 mL of methanol into the evaporated filtrate residue to dissolve the filtrate, and taking the dissolved filtrate residue as ephedrine hydrochloride to be detected; preparing a negative sample without ephedra component, taking 0.5-1.5 g of the negative sample, adding 8-15 mL of ethanol and 2-4 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 8-15 min, filtering, collecting filtrate, evaporating the filtrate to dryness, and evaporating the filtrate to dryness Adding 0.5-1.5 mL of methanol into the filtrate residue to dissolve the filtrate residue, and taking the dissolved filtrate residue as a negative sample solution; taking ephedrine hydrochloride as a reference substance, adding methanol to prepare a solution containing 0.5-1.5 mg ephedrine hydrochloride per 1mL, wherein the solution is used as an ephedrine hydrochloride reference substance solution; according to the thin layer chromatography of the four-part rule 0502 of the pharmacopoeia of the people's republic of China in 2020 edition, absorbing 5-15 mu L of ephedrine hydrochloride to be detected solution, negative sample solution and ephedrine hydrochloride reference substance solution respectively, respectively dispensing the ephedrine hydrochloride to be detected solution, the negative sample solution and the ephedrine hydrochloride reference substance solution on the same silica gel G plate, taking a mixed solution of chloroform-methanol-concentrated ammonia solution as a developing solvent, wherein the weight ratio of the chloroform, the methanol and the concentrated ammonia solution is 15-25:4-6:0.2-1, and standing for the solution on the silica gel GF ₂₅₄ After the thin layer plate is unfolded, taking out, airing, spraying ninhydrin test solution, heating until spots are clear in color development, and observing the positions of ephedrine hydrochloride to-be-detected solution, negative sample solution and ephedrine hydrochloride reference substance solution on the silica gel G plate; observing the spot positions, for example, the color spectrum of the ephedrine hydrochloride to be detected and the color spectrum of the ephedrine hydrochloride reference substance solution show fluorescence spots with the same color at the corresponding positions, and the negative sample solution is negative without interference, so that the capsule to be detected contains ephedrine hydrochloride.

In some embodiments of the present invention, in some embodiments,

identifying ephedrine hydrochloride by TLC identification method, which comprises taking 1g of the content of Shangfengting capsule to be detected, grinding, adding 10mL of ethanol and 3 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 10min, filtering, collecting filtrate, evaporating the filtrate, adding 1mL of methanol into the evaporated filtrate residue to dissolve the residue, and taking the dissolved filtrate residue as ephedrine hydrochloride to be detected solution; preparing a negative sample without ephedra components, taking 1g of the negative sample, adding 10mL of ethanol and 3 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 10min, filtering, collecting filtrate, evaporating the filtrate to dryness, adding 1mL of methanol into the evaporated filtrate residue to dissolve the filtrate residue, and taking the dissolved filtrate residue as a negative sample solution; taking ephedrine hydrochloride as reference substance, adding methanol to obtain solution containing ephedrine hydrochloride 1 mg/1 mL, and dissolvingThe solution is used as ephedrine hydrochloride reference substance solution; according to the thin layer chromatography of the four-part rule 0502 of the pharmacopoeia of the people's republic of China in 2020 edition, absorbing 10 mu L of ephedrine hydrochloride to be detected solution, negative sample solution and ephedrine hydrochloride reference substance solution respectively, respectively dispensing the ephedrine hydrochloride to be detected solution, the negative sample solution and the ephedrine hydrochloride reference substance solution on the same silica gel G plate, and taking a mixed solution of chloroform-methanol-concentrated ammonia solution as a developing agent, wherein the weight ratio of the chloroform, the methanol and the concentrated ammonia solution is 20:5:0.5, and standing for the solution to be in the silica gel GF ₂₅₄ After the thin layer plate is unfolded, taking out, airing, spraying ninhydrin test solution, heating until spots are clear in color development, and observing the positions of ephedrine hydrochloride to-be-detected solution, negative sample solution and ephedrine hydrochloride reference substance solution on the silica gel G plate; observing the spot positions, for example, the color spectrum of the ephedrine hydrochloride to be detected and the color spectrum of the ephedrine hydrochloride reference substance solution show fluorescence spots with the same color at the corresponding positions, and the negative sample solution is negative without interference, so that the capsule to be detected contains ephedrine hydrochloride.

In some embodiments of the present invention, in some embodiments,

identifying the glycyrrhizic acid by adopting an HPLC identification method, which comprises taking 0.5-1.5 g of the content of the Shangfengting capsule to be detected, grinding, adding 30-50 mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 20-40 min, filtering, collecting filtrate, steaming the filtrate until no alcohol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 15-30 mL of ethyl acetate each time, discarding the ethyl acetate solution, collecting the aqueous solution, regulating the pH value of the aqueous solution to 2 by hydrochloric acid, extracting the aqueous solution by using the ethyl acetate solution, merging the ethyl acetate solution after extracting the aqueous solution, evaporating the ethyl acetate solution to obtain residues, adding 70% methanol into the residues to dissolve the residues, and fixing the volume to 10mL to obtain the glycyrrhizic acid to be detected; preparing a negative sample without liquorice, weighing 0.5-1.5 g of the negative sample, grinding, adding 30-45 mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 25-40 min, filtering, collecting filtrate, steaming the filtrate until no alcohol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 15-30 mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 with hydrochloric acid, extracting the aqueous solution with the ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residues, adding 70% methanol into the residues to dissolve the residues, and fixing the volume to 10mL to obtain a negative sample solution; in addition, taking ammonium glycyrrhizate as an ammonium glycyrrhizate reference substance, adding 70% methanol to prepare a solution L containing 0.5-1.5 mg of glycyrrhizic acid per 1 mL; according to the performance liquid chromatography of the four-part rule 0512 test of the pharmacopoeia of the people's republic of China in 2020 edition, octadecylsilane chemically bonded silica is used as a filler, methanol-0.1% phosphoric acid is used as a mobile phase, wherein the weight ratio of the methanol to the 0.1% phosphoric acid is 50-70:3, the flow rate is 1.0mL/min, the detection wavelength is 252nm, the sample injection amount is 10 mu L, and the chromatographic peak is observed, if the retention time of the chromatographic peak of a glycyrrhizic acid solution to be detected is the same as the retention time of the chromatographic peak of an ammonium glycyrrhizinate reference substance and the negative and non-interference is the same, the cold stop capsule to be detected contains liquorice.

In some embodiments of the present invention, in some embodiments,

identifying glycyrrhizic acid by adopting an HPLC identification method, which comprises taking 1g of the content of the Shangfengting capsule to be detected, grinding, adding 40mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 30min, filtering, collecting filtrate, steaming the filtrate until no ethanol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 25mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 by hydrochloric acid, extracting the aqueous solution with the ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residues, adding 70% methanol into the residues to dissolve the residues, and fixing the volume to 10mL to obtain a glycyrrhizic acid solution to be detected; preparing a negative sample without liquorice, weighing 1g of the negative sample, grinding, adding 40mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 30min, filtering, collecting filtrate, steaming the filtrate until no ethanol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 25mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 with hydrochloric acid, extracting the aqueous solution with ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residue, adding 70% methanol into the residue to dissolve, and fixing the volume to 10mL to obtain a negative sample solution; taking ammonium glycyrrhizate as ammonium glycyrrhizate reference substance, adding 70% methanol to prepare solution L containing 1mg of glycyrrhizic acid per 1 mL; according to the performance liquid chromatography of the four-part rule 0512 test of the pharmacopoeia of the people's republic of China in 2020 edition, octadecylsilane chemically bonded silica is used as a filler, methanol-0.1% phosphoric acid is used as a mobile phase, wherein the weight ratio of the methanol to the 0.1% phosphoric acid is 65:3, the flow rate is 1.0mL/min, the detection wavelength is 252nm, the sample injection amount is 10 mu L, and the chromatographic peak is observed, if the retention time of the chromatographic peak of the glycyrrhizic acid to be detected solution is the same as that of the chromatographic peak of the ammonium glycyrrhizinate reference substance, and the negative is not interfered, the capsule to be detected contains liquorice.

In some embodiments of the present invention, in some embodiments,

the quality detection method of the Shangxiaoting capsule also comprises the content determination of ephedrine hydrochloride and pseudoephedrine hydrochloride, and comprises the following steps:

setting chromatographic conditions and system adaptability test: the chromatographic column conditions were: agiLent ZORBAX SB-C ₁₈ The dimensions are 250mm by 4.6mm,5 μm; mobile phase: acetonitrile-0.1% phosphoric acid, containing 0.1% NH4CL, wherein the weight ratio of acetonitrile-0.1% phosphoric acid is 4:96, the flow rate is 1.0mL/min, the column temperature is 30 ℃, and the detection wavelength is 210nm;

preparation of a mixed control solution: respectively weighing ephedrine hydrochloride reference substance 10.68mg and pseudoephedrine hydrochloride reference substance 9.91mg, placing into 50mL volumetric flask, adding water to dissolve, fixing volume to scale, and shaking to obtain mixed reference substance stock solution; measuring 1mL, 2mL, 4mL, 6mL, 8mL and 10mL of mixed reference stock solution respectively, adding water to the scales in volumetric flasks with 10mL to 10mL, and obtaining mixed reference solution with 6 series of concentrations;

preparation of test solution: taking the content of the Shangguang capsule, grinding, taking 1-1.5 g, placing in a distillation flask, adding 10mL of water, carrying out ultrasonic treatment for 10min, adding 150mL of 20% NaOH solution, carrying out heating distillation, introducing the distillate into a 100mL measuring flask filled with 8mL of 0.5moL/L hydrochloric acid solution, stopping collecting when the distillate is about 90mL, cooling, adding water to a scale, shaking uniformly, filtering the filtrate with a 0.45 mu m filter membrane, and taking the filtrate to obtain a sample solution;

Preparation of negative sample solution: preparing a negative sample without ephedrine hydrochloride and without pseudoephedrine hydrochloride, taking the negative sample, grinding, taking 1-1.5 g, placing in a distillation flask, adding 10mL of water, carrying out ultrasonic treatment for 10min, adding 150mL of 20% NaOH solution, carrying out heating distillation, introducing distillate into a 100mL measuring flask containing 8mL of 0.5moL/L hydrochloric acid solution, stopping collecting when the distillate is about 90mL, cooling, adding water to a scale, shaking uniformly, filtering the filtrate with a 0.45 mu m filter membrane, and taking a subsequent filtrate to obtain a negative sample solution;

and (3) measuring: respectively sucking 10 μl of reference solution, sample solution and negative sample solution, and injecting into high performance liquid chromatograph, measuring, and judging whether the contents of ephedrine hydrochloride and pseudoephedrine hydrochloride exceed the limit standard according to the peak area obtained by external standard method.

In the content measurement of ephedrine hydrochloride and pseudoephedrine hydrochloride, a content measurement method of ephedrine hydrochloride and pseudoephedrine hydrochloride in the Shangning capsule is established, the chemical structure of ephedrine alkaloids belongs to organic amines, the molecular weight is smaller and the ephedrine alkaloids are easy to volatilize, the invention adopts NaOH saturated aqueous solution for distillation to effectively extract free ephedrine and pseudoephedrine, and the ephedrine alkaloids are easy to dissolve in water after salifying, so that distillate is led into hydrochloric acid solution to be used as a sample solution; the method for measuring the content of ephedrine hydrochloride and pseudoephedrine hydrochloride is simple and easy to operate, has little impurity interference, is suitable for chromatographic columns and instruments of different factories and different experimenters, and has the advantages of simplicity, convenience, good repeatability, strong durability, wide adaptability and higher quality control system.

In some embodiments of the present invention, in some embodiments,

the quality detection method of the Shangxiao capsule also comprises the content measurement of imperatorin, which comprises the following steps:

chromatographic conditions and system adaptation test: the chromatographic column conditions are AgiLent ZORBAX SB-C18, the size is 250mm×4.6mm,5 μm; mobile phase: acetonitrile-water, the weight ratio of acetonitrile to water being 47:53; flow rate: 1.0mL/min; column temperature is 30 ℃; detection wavelength: 300nm;

preparation of a control solution: weighing imperatorin reference substance 10.29mg, placing in 50mL volumetric flask, adding methanol to dissolve, fixing volume to scale, shaking to obtain reference substance stock solution; respectively weighing a proper amount of control stock solution, and diluting with methanol to obtain a series of control solutions with different mass concentrations of 2.037 mug/mL, 4.074 mug/mL, 8.148 mug/mL, 12.22 mug/mL, 16.30 mug/mL and 20.37 mug/mL;

preparation of test solution: taking the content of the Shangguang capsule, grinding, weighing 1g of powder, placing into a conical flask, precisely adding 25mL of methanol, weighing, performing ultrasonic treatment, cooling, weighing again, supplementing the reduced weight with methanol, shaking uniformly, filtering, and filtering the filtrate with a 0.45 μm filter membrane to obtain a sample solution;

preparation of negative sample solution: preparing a negative sample without imperatorin, taking the negative sample, grinding, weighing 1g of powder, placing in a conical flask, precisely adding 25mL of methanol, weighing, performing ultrasonic treatment, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and filtering the filtrate with a 0.45 mu m filter membrane to obtain a negative sample solution;

And (3) measuring: respectively sucking 10 μl of reference solution, sample solution and negative sample solution, injecting into high performance liquid chromatograph, measuring, and judging whether the imperatorin content exceeds the limit standard according to the peak area obtained by external standard method.

Wherein "% (g/ml)" means that the solution contains several grams of solute per 100 ml; the percentage of ethanol refers to the ratio of the capacities at 20 ℃.

As imperatorin is furocoumarin, is soluble in water, methanol, ethanol and alkali liquor, has low boiling point of methanol, is cheap and easy to obtain, can reduce interference of large-polarity impurities in the extract on content measurement, has high chromatographic peak response value and stable baseline, and can monitor the content of the Shangqiangting capsule better by detecting imperatorin. In the content measurement of imperatorin, the mobile phase system for measuring the content of imperatorin is methanol-water, the water phase does not contain inorganic salt, the loss of a high performance liquid chromatograph is reduced, and the mobile phase system is an optimal mobile phase system and is a higher quality control system.

The quality detection method of the Shangning capsule has the beneficial effects that:

(1) According to the quality detection method of the Shangxiaoting capsule, when ephedrine hydrochloride is identified, ethanol and ammonia test solution are adopted, the ethanol solubility is good, so that dissolved water-soluble impurities are less, and compared with the prior art that diethyl ether and chloroform are adopted, the toxicity of the solvent used by the method is low; the ammonia test solution plays a role in infiltration, so that alkaloids are converted into a free state, and the free-state alkaloids are mostly insoluble in water and are dissolved in an organic reagent, namely, the ammonia test solution converts ephedrine in a sample into the free state, so that the ephedrine can be dissolved in ethanol, the purity of substances to be detected in the extracting solution is increased, the detection interference is reduced, the detection precision is effectively improved, and the detection time is shortened.

(2) The quality detection method of the Shangxiaoting capsule increases the detection of glycyrrhizic acid, so that the quality of the Shangxiaoting capsule is monitored more comprehensively; when detecting glycyrrhizic acid, because glycyrrhizic acid has carboxyl and phenolic hydroxyl groups, has strong hydrophilicity, is easily dissolved in a solvent with strong polarity and is not easily dissolved in an organic solvent with weak polarity, the invention adopts ethanol to completely extract glycyrrhizic acid in liquorice, the ethanol is evaporated to dryness, then ethyl acetate with weak polarity is used for extraction, because the solubility of glycyrrhizic acid in water is larger than that of ethyl acetate, the ethyl acetate can remove most of impurities, especially the influence of fat-soluble impurity components on chromatographic peak separation of glycyrrhizic acid, then the pH value of the extracted aqueous solution is adjusted to 2, so that glycyrrhizic acid is precipitated, and then the glycyrrhizic acid yellow precipitate is extracted by using ethyl acetate.

(3) The quality detection method of the Shangxiaoting capsule improves the quality control standard of the Shangxiaoting capsule, selects and analyzes the effective components in the monarch drug ephedra and the ministerial drug angelica dahurica, optimizes the TLC identification method of ephedrine hydrochloride, and increases the HPLC identification of glycyrrhizic acid.

Drawings

FIG. 1 is a TLC chart for identifying ephedrine hydrochloride in example 1, wherein reference numerals 1 to 3 in the chart represent ephedrine hydrochloride to-be-detected solutions, reference numeral 4 represents negative sample solutions, and reference numeral 5 represents ephedrine hydrochloride reference solution.

FIG. 2 is an HPLC chromatogram for identifying glycyrrhizic acid in example 1, wherein FIG. 1 represents glycyrrhizic acid in the figure (a) is an ammonium glycyrrhizinate control HPLC chromatogram, FIG. b is an HPLC chromatogram of glycyrrhizic acid to be detected solution, and FIG. c is a negative sample solution HPLC chromatogram.

Fig. 3 is an HPLC chromatogram of example 1 for detecting ephedrine hydrochloride and pseudoephedrine hydrochloride, wherein fig. (a) is a mixed control solution HPLC chromatogram, fig. (b) is a test solution HPLC chromatogram, and fig. (c) is a negative sample solution HPLC chromatogram, reference numeral 1 in the figure represents ephedrine hydrochloride, and reference numeral 2 in the figure represents pseudoephedrine hydrochloride.

Fig. 4 is an HPLC chromatogram of imperatorin in example 1, wherein fig. 1 represents imperatorin in the figure (a) is a control solution HPLC chromatogram, fig. 2 is a test solution HPLC chromatogram, and fig. c is a negative sample solution HPLC chromatogram.

Detailed Description

Preferred embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While the preferred embodiments of the present invention are shown in the drawings, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.

The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.

It should be understood that although the terms "number 1", "number 2" and the like may be used to describe various information in the present invention, such information should not be limited to these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the invention. Thus, a feature defined as "number 1", "number 2" may include one or more of the feature, either explicitly or implicitly. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.

For the convenience of description of the detection method of the present invention, the following capsule for treating common cold is selected in a unified way:

Capsule for treating injury and wind-stopping

Herba Ephedrae 606.1g herba Schizonepetae 606.1g radix Angelicae Dahuricae 606.1g rhizoma Atractylodis (parched) 606.1g pericarpium Citri Tangerinae 606.1g Glycyrrhrizae radix 303.05g

[ PREPARATION METHOD ] pulverizing above six ingredients, radix Angelicae Dahuricae 250g into fine powder; extracting volatile oil from herba Schizonepetae, pericarpium Citri Tangerinae and the rest radix Angelicae Dahuricae;

decocting the residue and herba Ephedrae with water twice each for 1.5 hr, mixing decoctions, filtering, concentrating the filtrate to relative density

1.1, adding ethanol to ethanol content of 60%, standing, collecting supernatant, recovering ethanol, and concentrating to relative density

1.30 to 1.33, adding radix angelicae fine powder, mixing, drying, granulating, spraying volatile oil, and encapsulating

1000 grains, and the preparation method is obtained.

[ PROBLEMS ] the product is capsule, and the content is brown yellow to brown granule; slightly fragrant smell, sweet and slightly bitter taste.

[ Functions and indications ] dispel wind-cold. Can be used for treating wind-cold type common cold, aversion to cold, fever, headache, nasal obstruction, nasal discharge,

heavy limb soreness, itching throat, cough with clear and thin sputum, pale red tongue with thin and white coating, and superficial and tight pulse; and upper respiratory tract infection, cold and rhinitis.

[ usage and dosage ] 3 granules at a time and 3 times a day are orally taken.

[ Note ] the infant, the elderly and the weak, and the pregnant woman should be taken under the guidance of a physician.

[ Specification ] 0.35g of the powder is packed per granule.

[ storage ] seal.

Example 1

The quality detection method of the Shangxiaoting capsule disclosed by the embodiment comprises the steps of identifying angelica dahurica, identifying ephedrine hydrochloride and identifying glycyrrhizic acid,

identification of dahurian angelica root by TLC identification method, which comprises: taking 3.5g of the content of the Shangfengting capsule to be detected, adding 20mL of petroleum ether at 80 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 20min, filtering the mixed solution, collecting filtrate, volatilizing the filtrate to 1mL, and taking the volatilized filtrate as a solution to be detected of the angelica dahurica; taking 0.1g of radix angelicae as a reference medicine, adding 20mL of petroleum ether at 60-90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 20min, standing, and taking supernatant as a radix angelicae reference solution; respectively sucking 10 μl of radix Angelicae Dahuricae solution to be detected and radix Angelicae Dahuricae reference substance solution according to thin layer chromatography of four-part rule 0502 of the 2020 edition of the pharmacopoeia of the people's republic of China,will beThe solution to be detected of the angelica dahurica and the solution of the angelica dahurica reference substance are respectively spotted on the same silica gel GF ₂₅₄ On the thin layer plate, the mixed solvent of petroleum ether and diethyl ether is used as developing agent, wherein the weight ratio of petroleum ether to diethyl ether is 1:1, the temperature of petroleum ether is 60-90 ℃, and the solution is heated in silica gel GF ₂₅₄ After being unfolded on the thin layer plate, the thin layer plate is taken out and dried; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 365nm ultraviolet lamp to see if the chromatogram of the radix Angelicae Dahuricae solution to be tested and the chromatogram of the radix Angelicae Dahuricae reference solution show fluorescent spots of the same color at corresponding positions; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 254nm ultraviolet lamp, and observing whether the chromatogram of the radix Angelicae Dahuricae solution to be detected and the chromatogram of the radix Angelicae Dahuricae reference solution show spots with the same color at corresponding positions; if the chromatogram of the solution to be tested of the angelica dahurica has fluorescent spots with the same color and spots with the same color as those of the solution of the angelica dahurica reference substance, the capsule to be tested of the common cold stop contains the angelica dahurica.

Identification of the salts by TLC identificationTaking 1g of the content of a capsule for treating injury, grinding, adding 10mL of ethanol and 3 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 10min, filtering, collecting filtrate, evaporating the filtrate, adding 1mL of methanol into the evaporated filtrate residue to dissolve the residue, and taking the dissolved filtrate residue as a ephedrine hydrochloride solution to be detected; preparing a negative sample without ephedra components, taking 1g of the negative sample, adding 10mL of ethanol and 3 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 10min, filtering, collecting filtrate, evaporating the filtrate to dryness, adding 1mL of methanol into the evaporated filtrate residue to dissolve the filtrate residue, and taking the dissolved filtrate residue as a negative sample solution; taking ephedrine hydrochloride as reference substance, adding methanol to prepare 1mg ephedrine hydrochloride solution per 1mL, and taking the solution as ephedrine hydrochloride reference substance solution; according to the thin layer chromatography of the four-part rule 0502 of the pharmacopoeia of the people's republic of China in 2020 edition, absorbing 10 mu L of ephedrine hydrochloride to be detected solution, negative sample solution and ephedrine hydrochloride reference substance solution respectively, respectively dispensing the ephedrine hydrochloride to be detected solution, the negative sample solution and the ephedrine hydrochloride reference substance solution on the same silica gel G plate, and taking a mixed solution of chloroform-methanol-concentrated ammonia solution as a developing agent, wherein the weight ratio of the chloroform, the methanol and the concentrated ammonia solution is 20:5:0.5, and standing for the solution to be in the silica gel GF ₂₅₄ After the thin layer plate is unfolded, taking out, airing, spraying ninhydrin test solution, heating until spots are clear in color development, and observing the positions of ephedrine hydrochloride to-be-detected solution, negative sample solution and ephedrine hydrochloride reference substance solution on the silica gel G plate; observing the spot positions, for example, the color spectrum of the ephedrine hydrochloride to be detected and the color spectrum of the ephedrine hydrochloride reference substance solution show fluorescence spots with the same color at the corresponding positions, and the negative sample solution is negative without interference, so that the capsule to be detected contains ephedrine hydrochloride.

In this embodiment, the quality detection method of the capsule for treating common cold further includes content determination of ephedrine hydrochloride and pseudoephedrine hydrochloride, which includes:

In this embodiment, the quality detection method of the capsule for treating common cold further includes content determination of imperatorin, which includes:

Example 2

identification of dahurian angelica root by TLC identification method, which comprises: taking 4g of the content of the Shangfengting capsule to be detected, adding 15mL of petroleum ether at 60 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 150min, filtering the mixed solution, collecting filtrate, volatilizing the filtrate to 0.5mL, and taking the volatilized filtrate as a solution to be detected of the angelica dahurica; taking 0.05g of radix angelicae as a reference medicine, adding 15mL of petroleum ether at 60 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 15min, standing, and taking supernatant as a radix angelicae reference substance solution; respectively sucking 8 μl of radix Angelicae Dahuricae solution to be tested and radix Angelicae Dahuricae reference solution according to thin layer chromatography of four-part rule 0502 in the 2020 edition of the pharmacopoeia of the people's republic of China, and comparing radix Angelicae Dahuricae solution to be tested and radix Angelicae DahuricaeThe photographic solution is respectively spotted on the same silica gel GF ₂₅₄ On the thin layer plate, a mixed solvent of petroleum ether and diethyl ether is used as a developing agent, wherein the weight ratio of petroleum ether to diethyl ether is 0.5:1, the temperature of the petroleum ether is 60 ℃, and the solution is heated in silica gel GF ₂₅₄ After being unfolded on the thin layer plate, the thin layer plate is taken out and dried; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 365nm ultraviolet lamp to see if the chromatogram of the radix Angelicae Dahuricae solution to be tested and the chromatogram of the radix Angelicae Dahuricae reference solution show fluorescent spots of the same color at corresponding positions; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 254nm ultraviolet lamp, and observing whether the chromatogram of the radix Angelicae Dahuricae solution to be detected and the chromatogram of the radix Angelicae Dahuricae reference solution show spots with the same color at corresponding positions; if the chromatogram of the solution to be tested of the angelica dahurica has fluorescent spots with the same color and spots with the same color as those of the solution of the angelica dahurica reference substance, the capsule to be tested of the common cold stop contains the angelica dahurica.

Identifying ephedrine hydrochloride by TLC identification method, which comprises taking 0.5g of the content of Shangfengting capsule to be detected, grinding, adding 8mL of ethanol and 3 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 5min, filtering, collecting filtrate, evaporating the filtrate, adding 0.5mL of methanol into the evaporated filtrate residue to dissolve the residue, and taking the dissolved filtrate residue as ephedrine hydrochloride to be detected; preparing a negative sample without ephedra components, taking 0.5g of the negative sample, adding 8mL of ethanol and 2 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 8min, filtering, collecting filtrate, evaporating the filtrate to dryness, adding 0.5mL of methanol into the evaporated filtrate residue to dissolve the filtrate residue, and taking the dissolved filtrate residue as a negative sample solution; taking ephedrine hydrochloride as reference substance, adding methanol to obtain solution containing ephedrine hydrochloride 0.5mg per 1mL, and taking the solution as ephedrine hydrochloride reference substance solution; according to thin layer chromatography of four-part rule 0502 of the pharmacopoeia of the people's republic of China in 2020 edition, absorbing 5 μl of ephedrine hydrochloride to be detected solution, negative sample solution and ephedrine hydrochloride reference substance solution, respectively dispensing the ephedrine hydrochloride to be detected solution, the negative sample solution and the ephedrine hydrochloride reference substance solution on the same silica gel G plate, and taking mixed solution of chloroform-methanol-concentrated ammonia as exhibition solution Opening agent, wherein the weight ratio of chloroform, methanol and concentrated ammonia solution is 15:4:0.2, and the solution is prepared on silica gel GF ₂₅₄ After the thin layer plate is unfolded, taking out, airing, spraying ninhydrin test solution, heating until spots are clear in color development, and observing the positions of ephedrine hydrochloride to-be-detected solution, negative sample solution and ephedrine hydrochloride reference substance solution on the silica gel G plate; observing the spot positions, for example, the color spectrum of the ephedrine hydrochloride to be detected and the color spectrum of the ephedrine hydrochloride reference substance solution show fluorescence spots with the same color at the corresponding positions, and the negative sample solution is negative without interference, so that the capsule to be detected contains ephedrine hydrochloride.

Identifying glycyrrhizic acid by adopting an HPLC identification method, which comprises taking 0.5g of the content of the Shangfengting capsule to be detected, grinding, adding 30mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 20min, filtering, collecting filtrate, steaming the filtrate until no ethanol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 15mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 by hydrochloric acid, extracting the aqueous solution with the ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residue, adding 70% methanol into the residue to dissolve the residue, and fixing the volume to 10mL to obtain glycyrrhizic acid to be detected; preparing a negative sample without liquorice, weighing 0.5g of the negative sample, grinding, adding 30mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 25min, filtering, collecting filtrate, steaming the filtrate until no ethanol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 15mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 with hydrochloric acid, extracting the aqueous solution with ethyl acetate liquid, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residue, adding 70% methanol into the residue to dissolve the residue, and fixing the volume to 10mL to obtain a negative sample solution; taking ammonium glycyrrhizate as ammonium glycyrrhizate reference substance, adding 70% methanol to prepare solution L containing 0.5mg of glycyrrhizic acid per 1 mL; according to the performance liquid chromatography of the four-part rule 0512 test of the pharmacopoeia of the people's republic of China in 2020 edition, octadecylsilane chemically bonded silica is used as a filler, methanol-0.1% phosphoric acid is used as a mobile phase, wherein the weight ratio of the methanol to the 0.1% phosphoric acid is 50:3, the flow rate is 1.0mL/min, the detection wavelength is 252nm, the sample injection amount is 10 mu L, and the chromatographic peak is observed, if the retention time of the chromatographic peak of a glycyrrhizic acid solution to be detected is the same as the retention time of the chromatographic peak of an ammonium glycyrrhizinate reference substance, and the negative noninterference indicates that the capsule to be detected contains liquorice.

Example 3

identification of dahurian angelica root by TLC identification method, which comprises: taking 5g of the content of the Shangfengting capsule to be detected, adding 30mL of petroleum ether at 90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 30min, filtering the mixed solution, collecting filtrate, volatilizing the filtrate to 1.5mL, and taking the volatilized filtrate as a solution to be detected of the angelica dahurica; taking 0.2g of radix angelicae as a reference medicine, adding 30mL of petroleum ether at 90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 30min, standing, and taking supernatant as a radix angelicae reference substance solution; respectively sucking 15 μl of radix Angelicae Dahuricae solution to be tested and radix Angelicae Dahuricae reference solution according to thin layer chromatography of four-part rule 0502 in the 2020 edition of the pharmacopoeia of the people's republic of China, and respectively dispensing radix Angelicae Dahuricae solution to be tested and radix Angelicae Dahuricae reference solution on the same silica gel GF ₂₅₄ On the thin layer plate, a mixed solvent of petroleum ether and diethyl ether is used as a developing agent, wherein the weight ratio of petroleum ether to diethyl ether is 1.2:1, the temperature of the petroleum ether is 90 ℃, and the solution is heated in silica gel GF ₂₅₄ After being unfolded on the thin layer plate, the thin layer plate is taken out and dried; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 365nm ultraviolet lamp to see if the chromatogram of the radix Angelicae Dahuricae solution to be tested and the chromatogram of the radix Angelicae Dahuricae reference solution show fluorescent spots of the same color at corresponding positions; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 254nm ultraviolet lamp, and observing whether the chromatogram of the radix Angelicae Dahuricae solution to be detected and the chromatogram of the radix Angelicae Dahuricae reference solution show spots with the same color at corresponding positions; if the chromatogram of the solution to be tested of the angelica dahurica has fluorescent spots with the same color and spots with the same color as those of the solution of the angelica dahurica reference substance, the capsule to be tested of the common cold stop contains the angelica dahurica.

The ephedrine hydrochloride is identified by TLC identification method, which comprises taking 2g of the content of SHANGFENGTING capsule to be detected, grinding, adding 15mL of ethanol and 3 drops of ammonia test solution to obtain mixed solution, performing ultrasonic treatment for 15min, and sievingFiltering, collecting filtrate, evaporating to dryness, adding 1.5mL of methanol into the evaporated filtrate residue to dissolve the filtrate residue, and taking the dissolved filtrate residue as ephedrine hydrochloride solution to be detected; preparing a negative sample without ephedra components, taking 1.5g of the negative sample, adding 15mL of ethanol and 4 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 15min, filtering, collecting filtrate, evaporating the filtrate to dryness, adding 1.5mL of methanol into the evaporated filtrate residue to dissolve the filtrate residue, and taking the dissolved filtrate residue as a negative sample solution; taking ephedrine hydrochloride as reference substance, adding methanol to prepare into solution containing ephedrine hydrochloride 1.5 mg/1 mL, and taking the solution as ephedrine hydrochloride reference substance solution; according to the thin layer chromatography of the four-part rule 0502 of the pharmacopoeia of the people's republic of China in 2020 edition, absorbing 15 mu L of ephedrine hydrochloride to be detected solution, negative sample solution and ephedrine hydrochloride reference substance solution, respectively dispensing the ephedrine hydrochloride to be detected solution, the negative sample solution and the ephedrine hydrochloride reference substance solution on the same silica gel G plate, and taking a mixed solution of chloroform-methanol-concentrated ammonia solution as a developing agent, wherein the weight ratio of the chloroform to the methanol to the concentrated ammonia solution is 25:6:1, and standing for the solution on the silica gel GF ₂₅₄ After the thin layer plate is unfolded, taking out, airing, spraying ninhydrin test solution, heating until spots are clear in color development, and observing the positions of ephedrine hydrochloride to-be-detected solution, negative sample solution and ephedrine hydrochloride reference substance solution on the silica gel G plate; observing the spot positions, for example, the color spectrum of the ephedrine hydrochloride to be detected and the color spectrum of the ephedrine hydrochloride reference substance solution show fluorescence spots with the same color at the corresponding positions, and the negative sample solution is negative without interference, so that the capsule to be detected contains ephedrine hydrochloride.

Identifying glycyrrhizic acid by adopting an HPLC identification method, which comprises taking 1.5g of the content of the Shangfengting capsule to be detected, grinding, adding 50mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 40min, filtering, collecting filtrate, steaming the filtrate until no ethanol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 30mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 by hydrochloric acid, extracting the aqueous solution with the ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residue, adding 70% methanol into the residue to dissolve the residue, and fixing the volume to 10mL to obtain glycyrrhizic acid to be detected; preparing a negative sample without liquorice, weighing 1.5g of the negative sample, grinding, adding 45mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 40min, filtering, collecting filtrate, steaming the filtrate until no ethanol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 30mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 with hydrochloric acid, extracting the aqueous solution with ethyl acetate liquid, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residue, adding 70% methanol into the residue to dissolve the residue, and fixing the volume to 10mL to obtain a negative sample solution; taking ammonium glycyrrhizate as ammonium glycyrrhizate reference substance, adding 70% methanol to prepare solution L containing 1.5mg of glycyrrhizic acid per 1 mL; according to the performance liquid chromatography of the four-part rule 0512 test of the pharmacopoeia of the people's republic of China in 2020 edition, octadecylsilane chemically bonded silica is used as a filler, methanol-0.1% phosphoric acid is used as a mobile phase, wherein the weight ratio of the methanol to the 0.1% phosphoric acid is 70:3, the flow rate is 1.0mL/min, the detection wavelength is 252nm, the sample injection amount is 10 mu L, and the chromatographic peak is observed, if the retention time of the chromatographic peak of a glycyrrhizic acid solution to be detected is the same as the retention time of the chromatographic peak of an ammonium glycyrrhizinate reference substance, and the negative noninterference indicates that the capsule to be detected contains liquorice.

preparation of test solution: taking the content of the Shangguang capsule, grinding, taking 1.5g, placing in a distillation flask, adding 10mL of water, carrying out ultrasonic treatment for 10min, adding 150mL of 20% NaOH solution, carrying out heating distillation, introducing the distillate into a 100mL measuring flask filled with 8mL of 0.5moL/L hydrochloric acid solution, stopping collecting when the distillate is about 90mL, cooling, adding water to a scale, shaking uniformly, filtering the filtrate with a 0.45 mu m filter membrane, and taking the subsequent filtrate to obtain a sample solution;

Preparation of negative sample solution: preparing a negative sample without ephedrine hydrochloride and without pseudoephedrine hydrochloride, taking the negative sample, grinding, taking 1g, placing in a distillation flask, adding 10mL of water, carrying out ultrasonic treatment for 10min, adding 150mL of 20% NaOH solution, carrying out heating distillation, introducing distillate into a 100mL measuring flask containing 8mL of 0.5moL/L hydrochloric acid solution, stopping collecting when the distillate is about 90mL, cooling, adding water to a scale, shaking uniformly, filtering the filtrate with a 0.45 mu m filter membrane, and taking a subsequent filtrate to obtain a negative sample solution;

Quality detection effect:

1. the pre-test analyzes the influence of ethanol and methanol as the extraction solvent on TLC identification of ephedrine hydrochloride, and the TLC chromatogram effect of the ethanol as the extraction solvent is superior to that of methanol, but the ephedrine hydrochloride spot color is lighter overall. When the concentrated ammonia test solution is added into the ethanol in a dropwise manner, the color of ephedrine hydrochloride spots is obviously deepened, the judgment is easy, but when the concentrated ammonia test solution is added more, the solution of the test sample is more viscous and the sample application volume is smaller, so that the ratio of the ethanol extraction solvent to the concentrated ammonia test solution is searched in the pre-experiment. FIG. 1 is a TLC chart for identifying ephedrine hydrochloride in example 1, as can be seen from FIG. 1: it was found that 3 drops of concentrated ammonia solution were added dropwise to 10ml of ethanol to give an optimal ratio. Meanwhile, analysis was performed on different temperatures (10-35 ℃), different humidities (30-75%) and different thin layer plate manufacturers (from Qingdao ocean chemical industry Co., ltd., tobacco stand chemical industry institute, german Merck Co.). The ephedrine hydrochloride spot can achieve good separation effect in TLC chromatograms under various conditions, and no interference spot appears in each negative sample.

2. Glycyrrhizic acid has carboxyl and phenolic hydroxyl groups, is high in hydrophilicity, is easily dissolved in a solvent with high polarity, and is not easily dissolved in an organic solvent with low polarity. The glycyrrhizic acid chromatographic peak was found to have good separation and negative without interference. AT the same time, the HPLC identification was subjected to a durability test to examine different high performance liquid chromatographs (Agilent 1260, waters e2695, shimadzu LC-20 AT) and different chromatographic columns (Agilent ZORBAX SB-C) ₁₈ 、Waters sunfire C ₁₈ 、Thermo AcclaimTM C ₁₈ The specification is 250mm multiplied by 4.6mm,5 μm), different phosphoric acid concentrations (0.05%, 0.1%, 0.15%,), different flow rates (0.9, 1.0, 1.1 ml/min), different temperatures (25, 30, 35 ℃) on glycyrrhizic acid separation. FIG. 2 is an HPLC chromatogram for identifying glycyrrhizic acid in example 1, as can be seen from FIG. 2: as a result, glycyrrhizic acid has good separation effect under all conditions, and negative effect is not interfered.

3. Fig. 3 is an HPLC chromatogram for example 1 detection of ephedrine hydrochloride and pseudoephedrine hydrochloride, as can be seen from fig. 3: and respectively taking a mixed reference substance solution, a sample solution and a negative sample solution, carrying out sample injection measurement according to chromatographic conditions, recording a chromatogram, wherein under the chromatographic conditions, the chromatographic peak of ephedrine hydrochloride and the chromatographic peak of pseudoephedrine hydrochloride in the sample are basically consistent with the chromatographic peak retention time of the mixed reference substance, the separation degree between the sample solution and adjacent components is greater than 1.5, and chromatographic peaks do not appear at the same position of the retention time of each component peak, so that the negative sample has no interference on measurement. Intermediate precision and durability tests were performed simultaneously to examine different personnel (A, B), different HPLC (Agilent 1260, waters e2695, shimadzu LC-20 AT), different columns (Agilent ZORBAX SB-C) ₁₈ 、Waters sunfire C ₁₈ 、Thermo AcclaimTM C ₁₈ The specification is 250mm multiplied by 4.6mm,5 μm), different phosphoric acid concentrations (0.05%, 0.1%, 0.15%,), different flow rates (0.8, 1.0, 1.2 ml/min), and different temperatures (25, 30, 35 ℃) to the content measurement of ephedrine hydrochloride and pseudoephedrine hydrochloride. As a result, the RSD of the ephedrine hydrochloride content measurement result is less than or equal to 2.05%, and the RSD of the pseudoephedrine hydrochloride content measurement result is less than or equal to 2.21%, which shows that the method has good durability and general applicability.

4. FIG. 4Is the HPLC chromatogram of imperatorin, example 1, as can be seen from fig. 4: taking reference substance solution, sample solution and negative sample solution respectively, sampling and measuring according to chromatographic conditions, and recording chromatograms. The imperatorin chromatographic peak in the test sample is basically consistent with the chromatographic peak retention time of the reference substance, and can achieve baseline separation with other components, the separation degree is more than 1.5, and the negative sample has no interference at the corresponding position. Intermediate precision and durability tests were performed simultaneously to examine different personnel (A, B), different HPLC (Agilent 1260, waters e2695, shimadzu LC-20 AT), different columns (Agilent ZORBAX SB-C) ₁₈ 、Waters sunfire C ₁₈ 、Thermo AcclaimTM C ₁₈ The effect of different flow rates (0.8, 1.0, 1.2 ml/min) and different temperatures (25, 30, 35 ℃) on the imperatorin content measurement was measured with the specification of 250mm×4.6mm,5 μm. As a result, the RSD of the results of the imperatorin content measurement is less than or equal to 1.94%, which shows that the method has good durability and general applicability.

5. According to the assay of example 1, the amounts of ephedrine hydrochloride, pseudoephedrine hydrochloride and imperatorin were determined for 17 batches of samples. Table 1 shows the contents of ephedrine hydrochloride, pseudoephedra hydrochloride and imperatorin in 17 batches,

TABLE 1 determination of ephedrine hydrochloride, pseudoephedrine hydrochloride and imperatorin content in 17 batches of samples

Remarks: 17 samples were from Yunnan white drug powder group Co., ltd

As can be seen from Table 1, the content measurement results of 17 batches of Shangxiaoting capsules show that the content range of ephedrine hydrochloride is 0.4711-0.9618 mg/granule, the average value is 0.6410 mg/granule, the content range of pseudoephedrine hydrochloride is 0.2547-0.5996 mg/granule, the average value is 0.3603 mg/granule, and the total amount average value is 1.001 mg/granule; the content of imperatorin is 61.78-123.8 mug/granule, and the average value is 89.11 mug/granule. Considering comprehensively, the limit is regulated according to 70% of the average value of the content measurement results obtained by 17 batches of samples, wherein each capsule sample of the Shangning capsule contains ephedra, calculated by the total amount of ephedrine hydrochloride and pseudoephedrine hydrochloride, of not less than 0.7mg, contains dahurian angelica, calculated by Hu Suji European, of not less than 60 mug, and whether the product content is qualified can be obtained by judging the content obtained by 17 batches of samples.

The relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present application unless it is specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective parts shown in the drawings are not drawn in actual scale for convenience of description. Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further discussion thereof is necessary in subsequent figures.

The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A quality detection method of a Shangxiaoting capsule comprises ephedra, schizonepeta, dahurian angelica root, rhizoma atractylodis, dried orange peel and liquorice, and is characterized in that: the quality detection method of the Shangtongting capsule comprises the steps of identifying angelica dahurica, identifying ephedrine hydrochloride and identifying glycyrrhizic acid, wherein,

identification of dahurian angelica root by TLC identification method, which comprises: taking 4-5 g of the content of the Shangfengting capsule to be detected, adding 15-30 mL of petroleum ether at 60-90 ℃ to obtain a mixed solution, and carrying out ultrasonic treatment on the obtained mixed solution for 15-30 min, filtering the mixed solution and collecting filtrate, volatilizing the filtrate to 0.5-1.5 mL, and taking the volatilized filtrate as a solution to be detected of the angelica dahurica; taking 0.05-0.2 g of radix angelicae as a reference medicine, adding 15-30 mL of petroleum ether at 60-90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 15-30 min, standing, and taking a supernatant as a radix angelicae reference substance solution; according to the thin layer chromatography of the four-part rule 0502 of the pharmacopoeia of the people's republic of China in 2020 edition, respectively sucking 8-15 mu L of the solution to be detected of the angelica dahurica and 8-15 mu L of the solution of the angelica dahurica reference substance, and respectively dispensing the solution to be detected of the angelica dahurica and the solution of the angelica dahurica reference substance on the same silica gel GF ₂₅₄ On the thin layer plate, the mixed solvent of petroleum ether and diethyl ether is used as developing agent, wherein the weight ratio of petroleum ether to diethyl ether is 0.5-1.2:1, the temperature of petroleum ether is 60-90 ℃, and the solution is prepared on silica gel GF ₂₅₄ After being unfolded on the thin layer plate, the thin layer plate is taken out and dried; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 365nm ultraviolet lamp to see if the chromatogram of the radix Angelicae Dahuricae solution to be tested and the chromatogram of the radix Angelicae Dahuricae reference solution show the first fluorescent spots with the same color at the corresponding positions; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 254nm ultraviolet lamp, and observing whether the chromatogram of the radix Angelicae Dahuricae solution to be detected and the chromatogram of the radix Angelicae Dahuricae reference solution show second fluorescent spots with the same color at corresponding positions; if the chromatogram of the solution to be detected of the angelica dahurica has the first fluorescent spots with the same color and the chromatogram of the solution to be detected of the angelica dahurica has the second fluorescent spots with the same color, the capsule to be detected of the common cold stop contains the angelica dahurica;

identifying ephedrine hydrochloride by TLC identification method, which comprises taking 0.5-2 g of the content of Shangfengting capsule to be detected, grinding, adding 8-15 mL of ethanol and 3 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 5-15 min, filtering, collecting filtrate, evaporating the filtrate, adding 0.5-1.5 mL of methanol into the evaporated filtrate residue to dissolve the filtrate, and taking the dissolved filtrate residue as ephedrine hydrochloride to be detected; preparing a negative sample without ephedra component, taking 0.5-1.5 g of the negative sample, adding 8-15 mL of ethanol and 2-4 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 8-15 min, filtering, collecting filtrate, Evaporating the solution to dryness, adding 0.5-1.5 mL of methanol into the evaporated filtrate residue to dissolve the solution, and taking the dissolved filtrate residue as a negative sample solution; taking ephedrine hydrochloride as a reference substance, adding methanol to prepare a solution containing 0.5-1.5 mg ephedrine hydrochloride per 1mL, wherein the solution is used as an ephedrine hydrochloride reference substance solution; according to the thin layer chromatography of the four-part rule 0502 of the pharmacopoeia of the people's republic of China in 2020 edition, absorbing 5-15 mu L of ephedrine hydrochloride to be detected solution, negative sample solution and ephedrine hydrochloride reference substance solution, respectively and respectively dispensing the ephedrine hydrochloride to be detected solution, the negative sample solution and the ephedrine hydrochloride reference substance solution on the same silica gel GF ₂₅₄ On the thin-layer plate, a mixed solution of chloroform-methanol-concentrated ammonia solution is used as a developing agent, wherein the weight ratio of the chloroform to the methanol to the concentrated ammonia solution is 15-25:4-6:0.2-1, and the solution is prepared on silica gel GF ₂₅₄ After the thin layer plate is unfolded, the thin layer plate is taken out, dried and sprayed with ninhydrin test solution, heated until the spots are clear in color development, and the ephedrine hydrochloride solution to be tested, the negative sample solution and the ephedrine hydrochloride reference substance solution are observed to be in silica gel GF ₂₅₄ A location on the lamina plate; observing the positions of spots, for example, the color spectrum of the ephedrine hydrochloride to be detected and the color spectrum of the ephedrine hydrochloride reference substance solution show fluorescent spots with the same color at the corresponding positions, and if the negative sample solution is negative and has no interference, the capsule to be detected contains ephedrine hydrochloride;

Identifying the glycyrrhizic acid by adopting an HPLC identification method, which comprises taking 0.5-1.5 g of the content of the Shangfengting capsule to be detected, grinding, adding 30-50 mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 20-40 min, filtering, collecting filtrate, steaming the filtrate until no alcohol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 15-30 mL of ethyl acetate each time, discarding the ethyl acetate solution, collecting the aqueous solution, regulating the pH value of the aqueous solution to 2 by hydrochloric acid, extracting the aqueous solution by using the ethyl acetate solution, merging the ethyl acetate solution after extracting the aqueous solution, evaporating the ethyl acetate solution to obtain residues, adding 70% methanol into the residues to dissolve the residues, and fixing the volume to 10mL to obtain the glycyrrhizic acid to be detected; preparing a negative sample without liquorice, weighing 0.5-1.5 g of the negative sample, grinding, adding 30-45 mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 25-40 min, filtering, collecting filtrate, steaming the filtrate until no alcohol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 15-30 mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 with hydrochloric acid, extracting the aqueous solution with the ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residues, adding 70% methanol into the residues to dissolve the residues, and fixing the volume to 10mL to obtain a negative sample solution; in addition, ammonium glycyrrhizate is taken as an ammonium glycyrrhizate reference substance, and 70% methanol is added to prepare a reference substance solution containing 0.5-1.5 mg of glycyrrhizic acid per 1 mL; according to the high performance liquid chromatography of the four-part rule 0512 test of the pharmacopoeia of the people's republic of China in 2020 edition, octadecylsilane chemically bonded silica is used as a filler, methanol-0.1% phosphoric acid is used as a mobile phase, wherein the weight ratio of the methanol to the 0.1% phosphoric acid is 50-70:3, the flow rate is 1.0mL/min, the detection wavelength is 252nm, the sample injection amount is 10 mu L, and the chromatographic peak is observed, if the retention time of the chromatographic peak of a glycyrrhizic acid solution to be detected is the same as the retention time of the chromatographic peak of an ammonium glycyrrhizinate reference solution, and if negative interference does not exist, the cold stop capsule to be detected contains liquorice.

2. The quality detection method of the Shangxiaoting capsule according to claim 1, which is characterized in that:

identification of dahurian angelica root by TLC identification method, which comprises: taking 3.5g of the content of the Shangfengting capsule to be detected, adding 20mL of petroleum ether at 60-90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 20min, filtering the mixed solution, collecting filtrate, volatilizing the filtrate to 1mL, and taking the volatilized filtrate as a solution to be detected of angelica dahurica; taking 0.1g of radix angelicae as a reference medicine, adding 20mL of petroleum ether at 60-90 ℃ to obtain a mixed solution, carrying out ultrasonic treatment on the obtained mixed solution for 20min, standing, and taking supernatant as a radix angelicae reference solution; respectively sucking 10 μl of radix Angelicae Dahuricae solution to be tested and radix Angelicae Dahuricae reference solution according to thin layer chromatography of four-part rule 0502 in the 2020 edition of the pharmacopoeia of the people's republic of China, and respectively dispensing radix Angelicae Dahuricae solution to be tested and radix Angelicae Dahuricae reference solution on the same silica gel GF ₂₅₄ On the thin layer plate, the mixed solvent of petroleum ether and diethyl ether is used as developing agent, wherein the weight ratio of petroleum ether to diethyl ether is 1:1, the temperature of petroleum ether is 60-90 ℃, and the solution is heated in silica gel GF ₂₅₄ After being unfolded on the thin layer plate, the thin layer plate is taken out and dried; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 365nm ultraviolet lamp to see if the chromatogram of the radix Angelicae Dahuricae solution to be tested and the chromatogram of the radix Angelicae Dahuricae reference solution show the first fluorescent spots with the same color at the corresponding positions; drying the dried silica gel GF ₂₅₄ Inspecting the thin-layer plate under 254nm ultraviolet lamp, and observing whether the chromatogram of the radix Angelicae Dahuricae solution to be detected and the chromatogram of the radix Angelicae Dahuricae reference solution show second fluorescent spots with the same color at corresponding positions; if the chromatogram of the solution to be tested of the angelica dahurica has the first fluorescent spots with the same color and the chromatogram of the solution to be tested of the angelica dahurica reference substance has the second fluorescent spots with the same color, the capsule to be tested of the common cold stop contains the angelica dahurica.

3. The quality detection method of the Shangxiaoting capsule according to claim 1, which is characterized in that:

identifying ephedrine hydrochloride by TLC identification method, which comprises taking 1g of the content of Shangfengting capsule to be detected, grinding, adding 10mL of ethanol and 3 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 10min, filtering, collecting filtrate, evaporating the filtrate, adding 1mL of methanol into the evaporated filtrate residue to dissolve the residue, and taking the dissolved filtrate residue as ephedrine hydrochloride to be detected solution; preparing a negative sample without ephedra components, taking 1g of the negative sample, adding 10mL of ethanol and 3 drops of ammonia test solution to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 10min, filtering, collecting filtrate, evaporating the filtrate to dryness, adding 1mL of methanol into the evaporated filtrate residue to dissolve the filtrate residue, and taking the dissolved filtrate residue as a negative sample solution; taking ephedrine hydrochloride as reference substance, adding methanol to prepare 1mg ephedrine hydrochloride solution per 1mL, and taking the solution as ephedrine hydrochloride reference substance solution; absorbing ephedrine hydrochloride solution to be detected, negative sample solution and ephedrine hydrochloride reference solution by thin layer chromatography of 0502 of four-part rule of 2020 edition of pharmacopoeia of the people's republic of China by 10 μl each The ephedrine hydrochloride solution to be measured, the negative sample solution and the ephedrine hydrochloride reference solution are respectively spotted on the same silica gel GF ₂₅₄ On the thin-layer plate, a mixed solution of chloroform-methanol-concentrated ammonia solution is used as a developing agent, wherein the weight ratio of the chloroform to the methanol to the concentrated ammonia solution is 20:5:0.5, and the solution is prepared on silica gel GF ₂₅₄ After the thin layer plate is unfolded, the thin layer plate is taken out, dried and sprayed with ninhydrin test solution, heated until the spots are clear in color development, and the ephedrine hydrochloride solution to be tested, the negative sample solution and the ephedrine hydrochloride reference substance solution are observed to be in silica gel GF ₂₅₄ A location on the lamina plate; observing the spot positions, for example, the color spectrum of the ephedrine hydrochloride to be detected and the color spectrum of the ephedrine hydrochloride reference substance solution show fluorescence spots with the same color at the corresponding positions, and the negative sample solution is negative without interference, so that the capsule to be detected contains ephedrine hydrochloride.

4. The quality detection method of the Shangxiaoting capsule according to claim 1, which is characterized in that:

identifying glycyrrhizic acid by adopting an HPLC identification method, which comprises taking 1g of the content of the Shangfengting capsule to be detected, grinding, adding 40mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 30min, filtering, collecting filtrate, steaming the filtrate until no ethanol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 25mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 by hydrochloric acid, extracting the aqueous solution with the ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residues, adding 70% methanol into the residues to dissolve the residues, and fixing the volume to 10mL to obtain a glycyrrhizic acid solution to be detected; preparing a negative sample without liquorice, weighing 1g of the negative sample, grinding, adding 40mL of ethanol to obtain a mixed solution, carrying out ultrasonic treatment on the mixed solution for 30min, filtering, collecting filtrate, steaming the filtrate until no ethanol smell exists, then adding water to obtain an aqueous solution, extracting the aqueous solution with ethyl acetate for 3 times, using 25mL of ethyl acetate each time, discarding ethyl acetate liquid, collecting the aqueous solution, regulating the pH of the aqueous solution to 2 with hydrochloric acid, extracting the aqueous solution with ethyl acetate solution, merging the ethyl acetate liquid after extracting the aqueous solution, evaporating the ethyl acetate liquid to obtain residue, adding 70% methanol into the residue to dissolve, and fixing the volume to 10mL to obtain a negative sample solution; in addition, ammonium glycyrrhizate is taken as an ammonium glycyrrhizate reference substance, and 70% methanol is added to prepare a reference substance solution containing 1mg of glycyrrhizic acid per 1 mL; according to the high performance liquid chromatography of the four-part rule 0512 test of the pharmacopoeia of the people's republic of China in 2020 edition, octadecylsilane chemically bonded silica is used as a filler, methanol-0.1% phosphoric acid is used as a mobile phase, wherein the weight ratio of the methanol to the 0.1% phosphoric acid is 65:3, the flow rate is 1.0mL/min, the detection wavelength is 252nm, the sample injection amount is 10 mu L, and the chromatographic peak is observed, if the retention time of the chromatographic peak of the glycyrrhizic acid to be detected solution is the same as that of the chromatographic peak of the ammonium glycyrrhizinate reference substance solution, and the negative is free from interference, the capsule to be detected contains liquorice.

5. The quality detection method of the Shangxiaoting capsule according to claim 1, which is characterized in that: the quality detection method of the Shangxiaoting capsule also comprises the content determination of ephedrine hydrochloride and pseudoephedrine hydrochloride, and comprises the following steps:

preparation of a mixed control solution: respectively weighing ephedrine hydrochloride reference substance 10.68mg and pseudoephedrine hydrochloride reference substance 9.91mg, placing into a 50mL volumetric flask, adding water to dissolve, fixing volume to scale, and shaking to obtain mixed reference substance stock solution; measuring 1mL, 2mL, 4mL, 6mL, 8mL and 10mL of mixed reference stock solution respectively, adding water to the scales in volumetric flasks with 10mL to 10mL, and obtaining mixed reference solution with 6 series of concentrations;

6. The quality detection method of the Shangxiaoting capsule according to claim 5, which is characterized in that: the quality detection method of the Shangxiao capsule also comprises the content measurement of imperatorin, which comprises the following steps:

preparation of test solution: taking the content of the Shangguang capsule, grinding, weighing 1g of powder, placing in an conical flask, precisely adding 25mL of methanol, weighing, performing ultrasonic treatment, cooling, weighing again, supplementing the reduced weight with methanol, shaking uniformly, filtering, and filtering the filtrate with a 0.45 μm filter membrane to obtain a sample solution;