CN114965726A - Chewable tablet fingerprint detection method and fingerprint thereof - Google Patents
Chewable tablet fingerprint detection method and fingerprint thereof Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/065—Preparation using different phases to separate parts of sample
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Abstract
The application relates to the technical field of medicine detection, in particular to a fingerprint detection method and a fingerprint of a chewable tablet; the method comprises the following steps: respectively obtaining a first group of standard solutions and a second group of standard solutions of the components of the chewable tablet; mixing the first group of standard solutions and the second group of standard solutions to obtain standard mixed solution; respectively carrying out high performance liquid chromatography on the first group of standard solutions, the second group of standard solutions and the standard mixed solution to respectively obtain a standard fingerprint spectrum group of the chewable tablet; crushing and superfine grinding the chewable tablets to be detected, and adding a solvent for ultrasonic treatment to obtain a sample solution to be detected; performing high performance liquid chromatography on the sample solution to be detected to obtain a fingerprint of the chewable tablet to be detected; judging whether the fingerprint is qualified or not according to the standard fingerprint group of the chewable tablet and the fingerprint of the chewable tablet to be detected; if yes, outputting a fingerprint; the fingerprint comprises 20 common peaks; by the method, the detection accuracy can be improved.
Description
Technical Field
The application relates to the technical field of medicine detection, in particular to a fingerprint detection method of chewable tablets and a fingerprint thereof.
Background
The chewable tablet is a tablet which is chewed in the oral cavity and then swallowed, and is always the first choice medicament product for children and old people because of the characteristics of strong dissolving capacity, convenient carrying, convenient swallowing and the like. The children wheat-jujube chewable tablet has the functions of strengthening the spleen and stomach, is mainly used for treating weakness of the spleen and the stomach, indigestion and inappetence of children, and is suitable for infant patients.
Currently, the detection of a medicament generally adopts a fingerprint, which refers to a chromatogram or a spectrogram which can mark the chemical characteristics of certain complex substances (such as traditional Chinese medicines), DNA (deoxyribonucleic acid) and protein of certain organisms or certain tissues or cells after being properly processed and obtained by adopting a certain analysis means. Therefore, the types and the quantities of the chemical components contained in the traditional Chinese medicine and the preparation thereof can be comprehensively reflected, and the quality of the medicine can be integrally described and evaluated.
At present, the fingerprint detection of chewable tablets is carried out, and most of chewable tablets are compared with main components due to more medicine content, so that more accurate fingerprint data are obtained, but the specific components are not compared one by one, so that the obtained fingerprint accuracy is low, and therefore, how to provide a high-accuracy fingerprint detection method for the children wheat and jujube chewable tablets is a technical problem which needs to be solved urgently at present.
Disclosure of Invention
The application provides a fingerprint detection method of chewable tablets and a fingerprint thereof, which aim to solve the technical problem of low accuracy of the fingerprint in the prior art.
In a first aspect, the present application provides a fingerprint detection method for chewable tablets, comprising:
respectively obtaining a first group of standard solutions and a second group of standard solutions of the components of the chewable tablet;
mixing the first group of standard solutions and the second group of standard solutions to obtain standard mixed solution;
respectively carrying out high performance liquid chromatography on the first group of standard solutions, the second group of standard solutions and the standard mixed solution to respectively obtain a standard fingerprint group of the chewable tablet;
crushing and superfine grinding the chewable tablets to be detected, and adding a solvent for ultrasonic treatment to obtain a sample solution to be detected;
performing high performance liquid chromatography on the sample solution to be detected to obtain a fingerprint to be detected of the chewable tablet to be detected;
judging whether the fingerprint to be detected is qualified or not according to the standard fingerprint group of the chewable tablet and the fingerprint to be detected of the chewable tablet to be detected;
if yes, outputting the fingerprint to be detected;
the first group of standard solutions are standard solutions containing chemical medicament components of chewable tablets, and the second group of standard solutions are standard solutions containing traditional Chinese medicine medicament components of chewable tablets.
Optionally, the mobile phase of the high performance liquid chromatography comprises: and (B) pump A: 0.1% phosphoric acid aqueous solution by mass fraction, pump B: and (3) acetonitrile.
Optionally, the gradient elution procedure of the high performance liquid chromatography is as follows: 0 min-5 min, pump A: 100%, B pump: 0 percent; 5 min-9 min, pump A: 100% → 93%, B pump: 0% → 7%; 9-15 min, pump A: 93% → 90%, B pump: 7% → 10%; 15 min-30 min, pump A: 90% → 75%, B pump: 10% → 25%; 30-35 min, pump A: 75% → 100%, B pump: 25% → 0%.
Optionally, the detection wavelength of the high performance liquid chromatography is 215nm to 225nm, the sample injection flow rate of the high performance liquid chromatography is 0.5mL/min to 1.5mL/min, and the high performance liquid chromatography is performedThe chromatographic column of the spectrum is BDS type C 18 。
Optionally, the preparation method of the first group of standard solutions specifically includes:
obtaining a first component of a chewable tablet sample, wherein the first component comprises allantoin, guanosine, rutin, chlorogenic acid, epicatechin, 5-hydroxymethylfurfural, hordenine, and adenosine cyclophosphate, and mixtures thereof;
dissolving the first component, and fixing the volume to obtain a first group of standard solutions of the components of the chewable tablet, wherein the solvent for dissolving the first component comprises methanol, water or a phosphoric acid aqueous solution.
Optionally, the judgment of whether the fingerprint to be detected is qualified or not is performed according to the standard fingerprint group of the chewable tablet and the fingerprint to be detected of the chewable tablet, and specifically includes:
obtaining standard similarity;
judging whether the fingerprint to be detected is qualified or not according to the actual similarity of the standard fingerprint group and the fingerprint to be detected;
if the standard similarity is smaller than-0.05 and the actual similarity is smaller than the standard similarity plus 0.05, judging that the fingerprint to be detected is qualified, and outputting the fingerprint to be detected;
if the actual similarity is less than the standard similarity to 0.05 or the actual similarity is more than the standard similarity to 0.05, determining that the fingerprint to be detected is unqualified, and preparing the solution to be detected again.
Optionally, the preparation method of the second group of standard solutions specifically includes:
obtaining a second component of the chewable tablet sample, wherein the second component comprises fructus Jujubae, fructus crataegi, bran-parched rhizoma Dioscoreae fine powder, bran-parched fructus Hordei Germinatus fine powder and extract;
and dissolving the second component, and then performing ultrasonic treatment and filtration to respectively obtain a second group of standard solutions of the components of the chewable tablet.
Optionally, the solvent used to dissolve the second component comprises methanol or water.
Optionally, the ultrasonic time is 25min to 45 min.
In a second aspect, the present application provides a fingerprint of a chewable tablet, the fingerprint comprising 20 common peaks, wherein the retention time of each common peak is: first common peak: 3.0min, second consensus peak: 3.2min, third consensus peak: 3.3min, fourth consensus peak: 4.0min, fifth consensus peak: 7.5min, sixth consensus peak: 10.8min, seventh consensus peak: 11.0min, eighth common peak, 11.2min, ninth common peak: 12.0min, tenth consensus peak: 12.5min, eleventh consensus peak: 13.1min, twelfth consensus peak: 13.3min, thirteenth consensus peak: 14.1min, fourteenth common peak: 14.6min, fifteenth common peak: 15.5min, sixteenth consensus peak: 16.3min, seventeenth common peak: 20.2min, eighteenth consensus peak: 21.6min, nineteenth consensus peak: 23.1min, twentieth consensus peak: 32.0 min.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
the embodiment of the application provides a fingerprint detection method of chewable tablet, through carrying out the preparation of standard solution respectively to the chemical agent composition and the traditional chinese medicine medicament composition of chewable tablet, mix the two again as standard mixed liquid, through carrying out high performance liquid chromatography to three kinds of different standard solutions to obtain accurate standard fingerprint group, and then can conveniently improve the rate of accuracy that detects to the accurate survey of chewable tablet sample that awaits measuring.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
Fig. 1 is a schematic flow chart of a method provided in an embodiment of the present application;
FIG. 2 is a schematic flow chart illustrating a method according to an embodiment of the present disclosure;
FIG. 3 is a high performance liquid chromatogram of a first set of standard solutions provided in the examples herein, wherein the appearance of peaks is allantoin, adenosine cyclophosphate, hordenine, 5-hydroxymethylfurfural, chlorogenic acid, epicatechin, and rutin, in order from left to right;
FIG. 4 is a high performance liquid chromatogram of fructus Jujubae in a second set of standard solutions provided in the examples of the present application;
FIG. 5 is a high performance liquid chromatogram of Hawthorn fruit in a second set of standard solutions provided in the examples herein;
FIG. 6 is a diagram of the peak position of the HPLC of the extract in the second set of standard solutions provided in the examples of the present application, wherein the reference peak is chlorogenic acid;
FIG. 7 is a high performance liquid chromatogram of bran-parched malt fines in a second set of standard solutions provided in the examples herein;
FIG. 8 is a high performance liquid chromatogram of fine bran-fried yam powder in a second set of standard solutions provided in the examples herein;
fig. 9 is a high performance liquid chromatogram of the pediatric fructus corni chewable tablet provided by the embodiment of the application;
fig. 10 is a diagram of an attribution of a middle peak position of a high performance liquid chromatography of the children's fructus ziziphi spinosae chewable tablet provided in the embodiment of the present application, wherein a reference peak is chlorogenic acid;
FIG. 11 is a middle peak position attribution graph of a high performance liquid chromatogram of Jiangzhong Jianwei Xiaoshi tablets in accordance with the comparative example of the application, wherein the reference peak is chlorogenic acid;
fig. 12 is a standard fingerprint without retention time of the pediatric fructus ziziphi spinosae chewable tablet provided by the embodiment of the application, wherein a reference peak is chlorogenic acid;
fig. 13 is a high performance liquid chromatogram without retention time of a Jiangzhong Jianwei Xiaoshi tablet provided in an embodiment of the present application, wherein a reference peak is chlorogenic acid.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In one embodiment of the present application, as shown in fig. 1, there is provided a fingerprint detection method for a chewable tablet, the method comprising:
s1, respectively obtaining a first group of standard solutions and a second group of standard solutions of the components of the chewable tablet;
s2, mixing the first group of standard solutions and the second group of standard solutions to obtain standard mixed solution;
s3, respectively carrying out high performance liquid chromatography on the first group of standard solutions, the second group of standard solutions and the standard mixed solution to respectively obtain standard fingerprint groups of the chewable tablets;
s4, crushing and superfine grinding the chewable tablets to be detected, and adding a solvent for ultrasonic treatment to obtain a sample solution to be detected;
s5, performing high performance liquid chromatography on the sample solution to be detected to obtain a fingerprint to be detected of the chewable tablet to be detected;
s6, judging whether the fingerprint to be detected is qualified or not according to the standard fingerprint group of the chewable tablet and the fingerprint to be detected of the chewable tablet;
if yes, outputting the fingerprint to be detected;
if not, preparing the sample solution to be detected again;
the first group of standard solutions are standard solutions containing chemical medicament components of chewable tablets, and the second group of standard solutions are standard solutions containing traditional Chinese medicine medicament components of chewable tablets.
In some embodiments, the mobile phase of the high performance liquid chromatography comprises: and (B) pump A: 0.1% phosphoric acid aqueous solution by mass fraction, pump B: and (3) acetonitrile.
In this application, through the mobile phase of injecing high performance liquid chromatography, make things convenient for the effectual infiltration of composition of chewable tablet to go out to be detected, can improve the rate of accuracy that detects.
In some embodiments, the gradient elution procedure of high performance liquid chromatography is: 0 min-5 min, pump A: 100%, B pump: 0 percent; 5-9 min, pump A: 100% → 93%, B pump: 0% → 7%; 9-15 min, pump A: 93% → 90%, B pump: 7% → 10%; 15 min-30 min, pump A: 90% → 75%, B pump: 10% → 25%; 30-35 min, pump A: 75% → 100%, B pump: 25% → 0%.
In this application, through the elution procedure of injecing high performance liquid chromatography, utilize stable elution procedure to elute the determinand to abundant with the chromatographic column elution, improve the accuracy that the chromatographic column detected.
In some embodiments, the detection wavelength of the high performance liquid chromatography is 215nm to 225nm, the flow rate of the sample injection of the high performance liquid chromatography is 0.5mL/min to 1.5mL/min, and the chromatographic column of the high performance liquid chromatography is BDS type C 18 。
In the application, the positive effect that the detection wavelength of the high performance liquid chromatography is 215 nm-225 nm is that the chromatograph can accurately measure the components of the solution within the wavelength condition range; when the value of the detection wavelength is larger than the maximum value of the end point of the range, the adverse effect is that the overlong wavelength range leads to the fact that the components in the detection stage part cannot be detected, so that the detection accuracy of the high performance liquid chromatography is reduced, and when the value of the detection wavelength is smaller than the minimum value of the end point of the range, the adverse effect is that the overlong wavelength leads to the fact that the components in the detection stage part cannot be detected, so that the detection accuracy of the high performance liquid chromatography is reduced.
The positive effect of the high performance liquid chromatography that the sample introduction flow rate is 0.5 mL/min-1.5 mL/min is that in the flow rate range, a proper amount of sample solution can be introduced into a chromatograph for detection, thereby improving the detection accuracy; when the value of the sampling flow rate is greater than the maximum value of the end point of the range, the adverse effect is that the excessively fast flow rate causes the excessively fast flow rate of the sample, the retention time of the sample in the chromatographic column is excessively short, and the detection accuracy of the chromatograph is influenced
In some embodiments, the method for preparing the first set of standard solutions specifically comprises:
obtaining a first composition of a chewable tablet sample, wherein the first composition comprises allantoin, guanosine, rutin, chlorogenic acid, epicatechin, 5-hydroxymethylfurfural, barley malt base, and adenosine cyclophosphate, and mixtures thereof;
dissolving the first component, and fixing the volume to obtain a first group of standard solutions of the components of the chewable tablet; the method comprises the following specific steps:
weighing 7.42mg of allantoin (batch number: 111501-;
weighing 0.42mg of guanosine (batch No. 111977-201501, China institute for food and drug testing) and placing the guanosine into a 5mL measuring flask, simultaneously adding 70% of methanol solution for dissolving, diluting the guanosine to a scale by using 70% of methanol solution, shaking up, and sealing to obtain a standard guanosine solution;
weighing rutin (batch number: 10080-;
weighing 1.41mg of chlorogenic acid (batch number: 110753-202018, China institute for food and drug testing) and placing the chlorogenic acid into a 5mL measuring flask, simultaneously adding a methanol solution with the mass fraction of 70% for dissolving, diluting the chlorogenic acid to a scale by adopting the methanol solution with the mass fraction of 70%, shaking up and sealing to obtain a standard solution of the chlorogenic acid;
weighing 1.93mg of epicatechin (batch number: 110828-201703, China institute for food and drug testing) and placing the epicatechin in a 5mL measuring flask, simultaneously adding a methanol solution with the mass fraction of 70% for dissolution, adopting the methanol solution with the mass fraction of 70% for dilution to a scale, shaking up, and sealing to obtain a standard solution of the epicatechin;
weighing 10.02mg of 5-hydroxymethylfurfural (batch number: 111626-;
weighing 2.85mg of hordenine, placing the weighed hordenine in a 5mL measuring flask, simultaneously adding a phosphoric acid aqueous solution with the mass fraction of 0.1% for dissolving, diluting the solution to a scale by adopting the phosphoric acid aqueous solution with the mass fraction of 0.1%, shaking up, and sealing to obtain a standard solution of the hordenine;
weighing 1.22mg of adenosine cyclophosphate (batch number: 110828-201703, China institute for food and drug testing) and placing the adenosine cyclophosphate in a 5mL measuring flask, simultaneously adding a methanol solution with the mass fraction of 70% for dissolving, adopting the methanol solution with the mass fraction of 70% for diluting to a scale, shaking up, sealing to obtain a standard solution of the adenosine cyclophosphate.
Respectively weighing 0.1mL of standard solutions of the allantoin, the guanosine, the rutin, the chlorogenic acid, the epicatechin, the 5-hydroxymethylfurfural, the hordenine and the adenosine cyclophosphate, placing the standard solutions into a sample feeding bottle, and shaking up to obtain a standard solution of a mixture.
The solvent used for dissolving the first component comprises methanol, water or phosphoric acid aqueous solution.
In the application, the preparation of the standard solution is carried out on allantoin, guanosine, rutin, chlorogenic acid, epicatechin, 5-hydroxymethylfurfural, hordenine and adenosine cyclophosphate in the chewable tablets, so that most chemical medicament components of the chewable tablets can be included, the standard solution of the chemical medicament components of the chewable tablets can be completely constructed, and the accuracy of the contrast detection of a sample to be detected is improved.
In some embodiments, the determining whether the fingerprint spectrum is qualified according to the standard fingerprint spectrum group of the chewable tablet and the fingerprint spectrum to be detected of the chewable tablet specifically includes:
s61, obtaining standard similarity;
s62, judging whether the fingerprint to be detected is qualified or not according to the actual similarity of the standard fingerprint group and the fingerprint to be detected;
if the standard similarity is more than-0.05 and the actual similarity is less than the standard similarity plus 0.05, judging that the fingerprint to be detected is qualified, and outputting the fingerprint to be detected;
and if the actual similarity is less than the standard similarity of-0.05 or the actual similarity is more than the standard similarity of +0.05, judging that the fingerprint to be detected is unqualified, and preparing the sample solution to be detected again.
In some embodiments, the method for preparing the second set of standard solutions specifically comprises:
obtaining a second component of the chewable tablet sample, wherein the second component comprises fructus Jujubae, fructus crataegi, bran-parched rhizoma Dioscoreae fine powder, bran-parched fructus Hordei Germinatus fine powder and extract;
dissolving the second component, and then performing ultrasonic treatment and filtration to respectively obtain a second group of standard solutions of the components of the chewable tablet, wherein the specific steps comprise:
cutting fructus Jujubae, weighing 4.018g, adding 25mL of solvent, performing ultrasonic treatment for 30min, and filtering to obtain filtrate to obtain standard solution of fructus Jujubae.
Cutting fructus crataegi into pieces, weighing 2.939g, adding 25mL of solvent, performing ultrasonic treatment for 30min, and filtering to obtain filtrate to obtain standard solution of fructus crataegi.
Weighing 0.998g of bran-fried yam fine powder, adding 25mL of solvent, carrying out ultrasonic treatment for 30min, and filtering to obtain a subsequent filtrate to obtain a standard solution of the bran-fried yam fine powder.
Weighing 1.002g of bran-parched malt fine powder, adding 25mL of solvent, performing ultrasonic treatment for 30min, and filtering to obtain a filtrate to obtain a standard solution of bran-parched malt fine powder.
2.282g of extract (batch number: 2021017) is weighed, 25mL of solvent is added, ultrasonic treatment is carried out for 30min, and then filtration is carried out, so as to obtain the standard solution of the extract.
In the application, standard solution preparation is carried out on Chinese date, hawthorn, bran-fried Chinese yam fine powder, bran-fried malt fine powder and extract of the traditional Chinese medicine preparation of the chewable tablet, so that most of traditional Chinese medicine preparation components of the chewable tablet can be included, the standard solution of the traditional Chinese medicine preparation components of the chewable tablet can be completely constructed, and the accuracy of comparison detection on a sample to be detected is improved.
In some embodiments, the solvent in which the second component is dissolved comprises methanol or water.
In some embodiments, the time of the sonication is between 25min and 45 min.
In the application, the positive effect that the ultrasonic time is 25-45 min is to limit the ultrasonic time, so that the sample to be detected can be conveniently and fully dissolved, and meanwhile, the ultrasonic treatment is carried out in the preparation of the standard solution, so that the separation speed and the separation amount of the medicament components can be improved, the accuracy of the constructed standard solution is further improved, and the accuracy of the detection of the sample to be detected is further improved; when the value of the time is greater than the maximum value of the end point of the range, the adverse effect is that the overlong ultrasonic time causes the component separation of the sample to be detected, the construction of the fingerprint of the sample to be detected is not facilitated, and when the value of the time is greater than the minimum value of the end point of the range, the adverse effect is that the overlong ultrasonic time causes the component of the sample to be detected to be fully dissolved out, and meanwhile, in the preparation stage of the standard solution, the component of the traditional Chinese medicine cannot be fully separated out, and the accuracy of the detection result is affected.
In one embodiment of the present application, a fingerprint of a chewable tablet is provided, the fingerprint includes 20 common peaks, wherein the retention time of each common peak is: first common peak: 3.0min, second consensus peak: 3.2min, third consensus peak: 3.3min, fourth consensus peak: 4.0min, fifth consensus peak: 7.5min, sixth consensus peak: 10.8min, seventh consensus peak: 11.0min, eighth common peak, 11.2min, ninth common peak: 12.0min, tenth consensus peak: 12.5min, eleventh consensus peak: 13.1min, twelfth consensus peak: 13.3min, thirteenth consensus peak: 14.1min, fourteenth common peak: 14.6min, fifteenth common peak: 15.5min, sixteenth consensus peak: 16.3min, seventeenth common peak: 20.2min, eighteenth consensus peak: 21.6min, nineteenth consensus peak: 23.1min, twentieth common peak: 32.0 min.
In the application, the constructed standard fingerprint is subjected to multiple times of measurement and screening, so that the peak values of the high performance liquid chromatography of all components in the chewable tablet can be accurately obtained, the follow-up comparison and detection of the to-be-measured fingerprint of a to-be-measured sample are facilitated, and the detection accuracy is improved.
Example 1
As shown in fig. 1, a method for detecting fingerprint of a chewable tablet comprises:
s1, respectively obtaining a first group of standard solutions and a second group of standard solutions of the components of the chewable tablet;
s2, mixing the first group of standard solutions and the second group of standard solutions to obtain standard mixed liquor;
s3, respectively carrying out high performance liquid chromatography on the first group of standard solutions, the second group of standard solutions and the standard mixed solution to respectively obtain a standard fingerprint group of the chewable tablet;
s4, crushing and superfine grinding the chewable tablets to be detected, and adding a solvent for ultrasonic treatment to obtain a sample solution to be detected;
s5, performing high performance liquid chromatography on the sample solution to be detected to obtain a fingerprint to be detected of the chewable tablet to be detected;
s61, obtaining standard similarity, wherein the standard similarity is 0.95;
s62, judging whether the fingerprint to be detected is qualified or not according to the actual similarity of the standard fingerprint group and the fingerprint to be detected;
if the standard similarity is-0.05 and the actual similarity is less than the standard similarity and 0.05, judging that the fingerprint is qualified, and outputting the fingerprint to be detected;
if the actual similarity is less than the standard similarity of-0.05 or the actual similarity is more than the standard similarity of +0.05, determining that the fingerprint to be detected is unqualified, and preparing the sample solution to be detected again.
The first group of standard solutions are standard solutions containing chemical medicament components of chewable tablets, the second group of standard solutions are standard solutions containing traditional Chinese medicine medicament components of chewable tablets, and the standard similarity is 1.
The mobile phase of the high performance liquid chromatography comprises: and (B) pump A: 0.1% phosphoric acid aqueous solution by mass fraction, pump B: and (3) acetonitrile.
The gradient elution procedure of the high performance liquid chromatography is as follows: 0 min-5 min, pump A: 100%, B pump: 0 percent; 5 min-9 min, pump A: 100% → 93%, B pump: 0% → 7%; 9-15 min, pump A: 93% → 90%, B pump: 7% → 10%; 15 min-30 min, pump A: 90% → 75%, B pump: 10% → 25%; 30-35 min, pump A: 75% → 100%, B pump: 25% → 0%.
The detection wavelength of the high performance liquid chromatography is 220nm, the sample injection flow rate of the high performance liquid chromatography is 1.0mL/min, and the chromatographic column of the high performance liquid chromatography is BDS type C 18 。
The preparation method of the first group of standard solutions specifically comprises the following steps:
obtaining a first component of the chewable tablet sample, wherein the first component comprises allantoin, guanosine, rutin, chlorogenic acid, epicatechin, 5-hydroxymethylfurfural, hordenine, adenosine cyclophosphate, and mixtures thereof;
dissolving the first component, and fixing the volume to obtain a first group of standard solutions of the components of the chewable tablet; the method comprises the following specific steps:
weighing 7.42mg of allantoin (batch number: 111501-;
weighing 0.42mg of guanosine (batch No. 111977-;
weighing rutin (batch number: 10080-;
weighing 1.41mg of chlorogenic acid (batch number: 110753-202018, China institute for food and drug testing) and placing the chlorogenic acid into a 5mL measuring flask, simultaneously adding a methanol solution with the mass fraction of 70% for dissolving, diluting the chlorogenic acid to a scale by adopting the methanol solution with the mass fraction of 70%, shaking up and sealing to obtain a standard solution of the chlorogenic acid;
weighing 1.93mg of epicatechin (batch number: 110828-201703, China institute for food and drug testing) and placing the epicatechin in a 5mL measuring flask, simultaneously adding a methanol solution with the mass fraction of 70% for dissolution, adopting the methanol solution with the mass fraction of 70% for dilution to a scale, shaking up, and sealing to obtain a standard solution of the epicatechin;
weighing 10.02mg of 5-hydroxymethylfurfural (batch number: 111626-;
weighing 2.85mg of hordenine, placing the weighed hordenine in a 5mL measuring flask, simultaneously adding a phosphoric acid aqueous solution with the mass fraction of 0.1% for dissolving, diluting the solution to a scale by adopting the phosphoric acid aqueous solution with the mass fraction of 0.1%, shaking up, and sealing to obtain a standard solution of the hordenine;
weighing 1.22mg of adenosine cyclophosphate (batch number: 110828-201703, China institute for food and drug testing) and placing the adenosine cyclophosphate in a 5mL measuring flask, simultaneously adding a methanol solution with the mass fraction of 70% for dissolving, adopting the methanol solution with the mass fraction of 70% for diluting to a scale, shaking up, sealing to obtain a standard solution of the adenosine cyclophosphate.
Respectively weighing 0.1mL of standard solutions of allantoin, guanosine, rutin, chlorogenic acid, epicatechin, 5-hydroxymethylfurfural, hordenine and adenosine cyclophosphate, placing the standard solutions into a sample feeding bottle, and shaking up to obtain the standard solution of the mixture.
The solvent used for dissolving the first component comprises methanol, water or phosphoric acid aqueous solution.
The preparation method of the second group of standard solutions specifically comprises the following steps:
obtaining a second component of the chewable tablet sample, wherein the second component comprises fructus Jujubae, fructus crataegi, bran-parched rhizoma Dioscoreae fine powder, bran-parched fructus Hordei Germinatus fine powder and extract;
dissolving the second component, and then performing ultrasonic treatment and filtration to respectively obtain a second group of standard solutions of the components of the chewable tablet, wherein the specific steps comprise:
cutting fructus Jujubae, weighing 4.018g, adding 25mL of solvent, performing ultrasonic treatment for 30min, and filtering to obtain filtrate to obtain standard solution of fructus Jujubae.
Cutting fructus crataegi into pieces, weighing 2.939g, adding 25mL of solvent, performing ultrasonic treatment for 30min, and filtering to obtain filtrate to obtain standard solution of fructus crataegi.
Weighing 0.998g of bran-fried yam fine powder, adding 25mL of solvent, carrying out ultrasonic treatment for 30min, and filtering to obtain a subsequent filtrate to obtain a standard solution of the bran-fried yam fine powder.
Weighing 1.002g of bran-parched malt fine powder, adding 25mL of solvent, performing ultrasonic treatment for 30min, and filtering to obtain a filtrate to obtain a standard solution of bran-parched malt fine powder.
2.282g of extract (batch number: 2021017) is weighed, 25mL of solvent is added, ultrasonic treatment is carried out for 30min, and then filtration is carried out, so as to obtain the standard solution of the extract.
The solvent for dissolving the second component comprises methanol or water.
The time of ultrasonication was 30 min.
The sample to be tested is the children wheat and jujube chewable tablet, and the preparation method of the sample solution to be tested comprises the following steps: weighing 14.876g of the 3004 th batch of tablet fine powder, adding 25ml of water, carrying out ultrasonic treatment for 30min, and filtering to obtain a subsequent filtrate; weighing 14.869g of 5001 batches of tablet fine powder, adding 25ml of water, carrying out ultrasonic treatment for 30min, filtering, taking subsequent filtrate, and mixing the two subsequent filtrates according to the volume ratio of 1: 1 to obtain the aqueous solution of the sample to be detected.
A chewable tablet fingerprint comprises 20 common peaks, wherein the retention time of each common peak is as follows: first common peak: 3.0min, second consensus peak: 3.2min, third consensus peak: 3.3min, fourth consensus peak: 4.0min, fifth consensus peak: 7.5min, sixth consensus peak: 10.8min, seventh consensus peak: 11.0min, eighth common peak, 11.2min, ninth common peak: 12.0min, tenth consensus peak: 12.5min, eleventh consensus peak: 13.1min, twelfth consensus peak: 13.3min, thirteenth consensus peak: 14.1min, fourteenth common peak: 14.6min, fifteenth common peak: 15.5min, sixteenth consensus peak: 16.3min, seventeenth common peak: 20.2min, eighteenth consensus peak: 21.6min, nineteenth consensus peak: 23.1min, twentieth consensus peak: 32.0 min.
Example 2
Comparing example 2 with comparative example 1, example 2 differs from example 1 in that:
the time of ultrasonication was 25 min.
The detection wavelength of the high performance liquid chromatography is 215nm, and the sample injection flow rate of the high performance liquid chromatography is 0.5 mL/min.
Example 3
Comparing example 3 with comparative example 1, example 3 differs from example 1 in that:
the time of sonication was 45 min.
The detection wavelength of the high performance liquid chromatography is 215 nm-225 nm, and the sample injection flow rate of the high performance liquid chromatography is 1.5mL/min
Comparative example 1
Comparative example 1 and example 1 were compared, and comparative example 1 and example 1 were distinguished in that:
the chewable tablet to be detected is replaced by Jiangzhong Jianwei Xiaoshi tablet, and the specific preparation steps are as follows: 14.72g of fine powder of Jianzhong Jianwei Xiaoshi tablets is weighed, and 25mL of water is added. And (4) after ultrasonic treatment for 30min, filtering, and taking a subsequent filtrate to obtain a sample solution to be detected.
Comparative example 2
Comparative example 2 is compared with example 1, and comparative example 2 differs from example 1 in that:
the time of ultrasonication was 20 min.
The detection wavelength of the high performance liquid chromatography is 205nm, and the sample injection flow rate of the high performance liquid chromatography is 0.3 mL/min.
Comparative example 3
Comparative example 3 is compared with example 1, and comparative example 3 differs from example 1 in that:
the time of ultrasonication was 50 min.
The detection wavelength of the high performance liquid chromatography is 245nm, and the sample injection flow rate of the high performance liquid chromatography is 2.0 mL/min.
Related experiments:
the methods of examples 1 to 3 and comparative examples 1 to 3 were repeated ten times, respectively, and the average similarity of the fingerprint spectra of examples 1 to 3 and comparative examples 1 to 3 was collected, and the statistical results are shown in table 1.
Test methods of the related experiments:
similarity of fingerprint spectra: the data of each example and comparative example measured by Agilent 1260 high performance liquid chromatograph were analyzed by clustering analysis (HCA), Principal Component Analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA) multivariate statistical analysis.
TABLE 1
| Categories | Similarity of fingerprint |
| Example 1 | 0.998 |
| Example 2 | 0.996 |
| Example 3 | 0.995 |
| Comparative example 1 | 0.595 |
| Comparative example 2 | 0.798 |
| Comparative example 3 | 0.854 |
Table 1 specific analysis:
the similarity of the fingerprint refers to the similarity between the fingerprint of the sample to be detected and the standard fingerprint after multiple detections, and the closer the similarity is to 1, the more accurate the measured fingerprint is.
As can be seen from the data of examples 1-3,
when different ultrasonic and high performance liquid chromatography conditions are adopted, the influence on the similarity of the fingerprint is less.
As can be seen from the data of comparative examples 1-3,
if the sample to be detected is not a product of the children wheat-jujube chewable tablet, the detection accuracy is reduced, which shows that the fingerprint provided by the application can effectively detect the children wheat-jujube chewable tablet, and meanwhile, if the process parameter conditions provided by the application are not adopted, the similarity of the fingerprint is reduced, and the accuracy of the detection result is influenced.
One or more technical solutions in the embodiments of the present application at least have the following technical effects or advantages:
(1) according to the method provided by the embodiment of the application, the standard solutions are respectively prepared for the chemical components and the traditional Chinese medicine components of the chewable tablet, and the standard mixed solution formed by mixing the chemical components and the traditional Chinese medicine components and the mixture of the traditional Chinese medicine components are prepared, so that abundant standard fingerprint spectrums can be obtained, whether the fingerprint spectrums are qualified or not can be accurately judged, and the accuracy of the fingerprint spectrums is improved.
(2) The fingerprint provided by the embodiment of the application has 20 clear common peaks, and can cover most of components of the children's wheat and jujube chewable tablets, so that the accuracy of the whole detection method can be improved.
(3) The method provided by the embodiment of the application can be used for detecting the traditional Chinese medicine chewable tablets, and particularly can be used for detecting the children's wheat and jujube chewable tablets most accurately.
Description of the drawings:
FIG. 3 is a high performance liquid chromatogram of a first set of standard solutions provided in the examples herein, wherein the appearance of peaks is allantoin, adenosine cyclophosphate, hordenine, 5-hydroxymethylfurfural, chlorogenic acid, epicatechin, and rutin, in order from left to right;
FIG. 4 is a high performance liquid chromatogram of fructus Jujubae in a second set of standard solutions provided in the examples of the present application;
FIG. 5 is a high performance liquid chromatogram of Hawthorn fruit in a second set of standard solutions provided in the examples herein;
FIG. 6 is a diagram of the peak position of the HPLC of the extract in the second set of standard solutions provided in the examples of the present application, wherein the reference peak is chlorogenic acid;
FIG. 7 is a high performance liquid chromatogram of bran-parched malt fines in a second set of standard solutions provided in the examples of the present application;
FIG. 8 is a high performance liquid chromatogram of fine bran-fried yam powder in a second set of standard solutions provided in the examples herein;
fig. 9 is a high performance liquid chromatogram of the pediatric fructus corni chewable tablet provided by the embodiment of the application;
fig. 10 is a diagram of a peak position assignment in high performance liquid chromatography of a pediatric wheat-jujube chewable tablet provided in an embodiment of the present application, where a reference peak is chlorogenic acid;
as can be seen from fig. 3 to 10, the first group of standard solutions and the second group of standard easy fingerprints provided by the present application can be used as a standard fingerprint group, and the detection accuracy of the children's fructus corni chewable tablets is high.
FIG. 11 is a middle peak position attribution diagram of a high performance liquid chromatogram of Jiangzhong Jianwei Xiaoshi tablets in comparison example provided by the application, wherein a reference peak is chlorogenic acid;
fig. 12 is a standard fingerprint without retention time of the pediatric fructus ziziphi spinosae chewable tablet provided by the embodiment of the application, wherein a reference peak is chlorogenic acid;
fig. 13 is a high performance liquid chromatogram without retention time of a Jiangzhong Jianwei Xiaoshi tablet provided in an embodiment of the present application, wherein a reference peak is chlorogenic acid.
As can be seen from fig. 11 to 13, the smaller components contained in the stomach-invigorating and digestion-promoting tablets in the river cause more components in the fructus ziziphi spinosae chewable tablets, so that the smaller number of peaks of the high performance liquid chromatography of the stomach-invigorating and digestion-promoting tablets in the river cause more peaks of the high performance liquid chromatography of the fructus ziziphi spinosae chewable tablets, and the smaller number of peaks of the high performance liquid chromatography of the stomach-invigorating and digestion-promoting tablets in the river cause less similarity of fingerprint spectra, thereby indirectly explaining that the method provided by the application can effectively improve the accuracy.
It is noted that, in this document, relational terms such as "first" and "second," and the like, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A fingerprint detection method of a chewable tablet is characterized by comprising the following steps:
respectively obtaining a first group of standard solutions and a second group of standard solutions of the components of the chewable tablet;
mixing the first group of standard solutions and the second group of standard solutions to obtain standard mixed solution;
respectively carrying out high performance liquid chromatography on the first group of standard solutions, the second group of standard solutions and the standard mixed solution to respectively obtain a standard fingerprint group of the chewable tablet;
crushing and superfine grinding the chewable tablets to be detected, and adding a solvent for ultrasonic treatment to obtain a sample solution to be detected;
performing high performance liquid chromatography on the sample solution to be detected to obtain a fingerprint to be detected of the chewable tablet to be detected;
judging whether the fingerprint to be detected is qualified or not according to the standard fingerprint group of the chewable tablet and the fingerprint to be detected of the chewable tablet to be detected;
if yes, outputting the fingerprint to be detected;
the first group of standard solutions are standard solutions containing chemical medicament components of chewable tablets, and the second group of standard solutions are standard solutions containing traditional Chinese medicine medicament components of chewable tablets.
2. The method of claim 1, wherein the mobile phase of high performance liquid chromatography comprises: and (B) pump A: 0.1% phosphoric acid aqueous solution by mass fraction, pump B: and (3) acetonitrile.
3. The method according to claim 1 or 2, characterized in that the gradient elution procedure of the high performance liquid chromatography is: 0 min-5 min, pump A: 100%, B pump: 0%; 5 min-9 min, pump A: 100% → 93%, B pump: 0% → 7%; 9-15 min, pump A: 93% → 90%, B pump: 7% → 10%; 15 min-30 min, pump A: 90% → 75%, B pump: 10% → 25%; 30-35 min, pump A: 75% → 100%, B pump: 25% → 0%.
4. The method of claim 1 or 2The method is characterized in that the detection wavelength of the high performance liquid chromatography is 215nm to 225nm, the sample injection flow rate of the high performance liquid chromatography is 0.5mL/min to 1.5mL/min, and a chromatographic column of the high performance liquid chromatography is BDS type C 18 。
5. The method according to claim 1, wherein the preparation method of the first group of standard solutions specifically comprises:
obtaining a first component of a chewable tablet sample, wherein the first component comprises allantoin, guanosine, rutin, chlorogenic acid, epicatechin, 5-hydroxymethylfurfural, hordenine, and adenosine cyclophosphate, and mixtures thereof;
dissolving the first component, and fixing the volume to obtain a first group of standard solutions of the components of the chewable tablet,
wherein the solvent used for dissolving the first component comprises methanol, water or phosphoric acid aqueous solution.
6. The method according to claim 5, wherein the determining whether the fingerprint spectrum to be tested is qualified according to the standard fingerprint spectrum group of the chewable tablet and the fingerprint spectrum to be tested of the chewable tablet specifically comprises:
obtaining standard similarity;
judging whether the fingerprint to be detected is qualified or not according to the actual similarity of the standard fingerprint group and the fingerprint to be detected;
if the standard similarity is more than-0.05 and the actual similarity is less than the standard similarity plus 0.05, judging that the fingerprint is qualified, and outputting the fingerprint;
if the actual similarity is less than the standard similarity of-0.05 or the actual similarity is more than the standard similarity of +0.05, determining that the fingerprint is unqualified, and preparing the sample solution to be detected again.
7. The method according to claim 1, wherein the preparation method of the second set of standard solutions specifically comprises:
obtaining a second component of the chewable tablet sample, wherein the second component comprises fructus Jujubae, fructus crataegi, bran-parched rhizoma Dioscoreae fine powder, bran-parched fructus Hordei Germinatus fine powder and extract;
and dissolving the second component, and then performing ultrasonic treatment and filtration to respectively obtain a second group of standard solutions of the components of the chewable tablet.
8. The method of claim 7, wherein the solvent in which the second component is dissolved comprises methanol or water.
9. The method of claim 1, wherein the ultrasound is timed to
25min～45min。
10. A fingerprint of a chewable tablet, wherein the fingerprint comprises 20 common peaks, wherein the retention time of each common peak is: first common peak: 3.0min, second consensus peak: 3.2min, third consensus peak: 3.3min, fourth consensus peak: 4min, fifth common peak: 7.5min, sixth consensus peak: 10.8min, seventh consensus peak: 11.0min, eighth common peak, 11.2min, ninth common peak: 12.0min, tenth consensus peak: 12.5min, eleventh consensus peak: 13.1min, twelfth consensus peak: 13.3min, thirteenth consensus peak: 14.1min, fourteenth common peak: 14.6min, fifteenth common peak: 15.5min, sixteenth consensus peak: 16.3min, seventeenth common peak: 20.2min, eighteenth consensus peak: 21.6min, nineteenth consensus peak: 23.1min, twentieth consensus peak: 32.0 min.
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