CN113063888A - Detection method and consistency evaluation method for azithromycin tablet impurities - Google Patents
Detection method and consistency evaluation method for azithromycin tablet impurities Download PDFInfo
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- CN113063888A CN113063888A CN202110330954.9A CN202110330954A CN113063888A CN 113063888 A CN113063888 A CN 113063888A CN 202110330954 A CN202110330954 A CN 202110330954A CN 113063888 A CN113063888 A CN 113063888A
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8872—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample impurities
Abstract
The invention discloses a detection method and a consistency evaluation method for azithromycin tablet impurities, which are characterized in that 0.05mol/L ammonium dihydrogen phosphate buffer solution and pyrrolidine-formic acid-acetonitrile mixed solution are selected as mobile phases for gradient elution, so that the accuracy of the detection method is improved, the detection time is reduced, the working efficiency in the production process is improved, and the types and the contents of the impurities in the azithromycin tablet can be comprehensively detected. The invention also provides a consistency evaluation method, when the types and the contents of the impurities in the reference preparation and the azithromycin tablet are consistent, the consistency of the product structures and the quality of the reference preparation and the azithromycin tablet can be judged. The invention provides a detection method and a consistency evaluation method for azithromycin tablet impurities, which are used for solving the technical problems of low accuracy, long detection time and few detected impurity types of the existing detection method.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a detection method and a consistency evaluation method for azithromycin tablets.
Background
Azithromycin is an antibiotic belonging to macrolide, is an antibiotic which is very commonly used clinically and is commonly used for acute pharyngitis and acute tonsillitis caused by streptococcus pyogenes; sinusitis, otitis media, acute bronchitis and acute attack of chronic bronchitis caused by sensitive bacteria; pneumonia caused by streptococcus pneumoniae, haemophilus influenzae, and mycoplasma pneumoniae; urethritis and cervicitis caused by chlamydia trachomatis and non-multiple drug-resistant neisseria gonorrhoeae; infection of skin soft tissue by sensitive bacteria. Compared with erythromycin, the azithromycin tablet has the advantages of acid stability, no gastric acid damage during oral administration, long half-life, high concentration of infected parts and cells, enhanced action on gram-negative bacteria, particularly enhanced action on influenza bacillus, wider antibacterial spectrum and stronger antibacterial action.
As the azithromycin tablets are semi-synthetic products, more impurities are easily generated in the starting materials and the synthetic process, and the azithromycin tablets are sensitive to factors such as acid, alkali, heat, oxidation and the like, the impurity control and detection of the azithromycin tablets are more troublesome than other antibiotic varieties. At present, the methods of HPLC (high performance liquid chromatography) adopted for measuring azithromycin tablets and impurities thereof are reported by domestic pharmacopoeia and documents, the detection accuracy is lower, the detection time is long, and the types of the detected impurities are less. Therefore, there is a need for improvements to existing detection methods.
Disclosure of Invention
The invention provides a detection method and a consistency evaluation method for azithromycin tablets, which are used for solving the technical problems of low accuracy, long detection time and few detected impurities in the existing detection method.
In view of the above, the invention provides a method for detecting azithromycin tablet impurities, which comprises the steps of dissolving an azithromycin tablet sample by using a dissolving agent, and detecting by using a high performance liquid chromatography, wherein the chromatographic conditions are as follows: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column, and an ultraviolet detector is adopted to carry out gradient elution by taking 0.05mol/L ammonium dihydrogen phosphate buffer solution as a mobile phase A and taking a pyrrolidine-formic acid-acetonitrile mixed solution as a mobile phase B; the dissolving agent is formic acid aqueous solution, and ammonium dihydrogen phosphate buffer solution is adjusted to pH value of 6.5 by triethylamine solution.
Optionally, the chromatography column is: waters XterraTM RP18 liquid chromatography column.
Optionally, the volume ratio of the pyrrolidine-formic acid-acetonitrile mixture is 5: 10: 85.
optionally, the gradient elution comprises:
the volume ratio of the mobile phase A to the mobile phase B is 70: 30, carrying out the first elution for 0-30 minutes; the volume ratio of mobile phase a to mobile phase B was 90: 10, carrying out second elution for 30-50 minutes; the volume ratio of mobile phase a to mobile phase B was 95: 5, carrying out third elution for 50-65 minutes; the volume ratio of mobile phase a to mobile phase B was 70: and 30, carrying out fourth elution for 65-72 minutes.
Optionally, the chromatographic conditions further comprise: the column temperature was 38 ℃, the sample injection amount was 25. mu.l, the flow rate was 1.5ml/min, and the detection wavelength was 210 nm.
Optionally, the dissolution agent is 90% aqueous formic acid.
Optionally, the dissolution agent dissolves the azithromycin tablet sample under ultrasonic dissolution conditions.
The invention also provides a consistency evaluation method based on the detection method of the azithromycin tablets impurities, which comprises the steps of comparing the azithromycin tablets with reference preparations for impurities;
the impurity comparison comprises detecting impurities in the azithromycin tablets and the reference preparation by adopting a high performance liquid chromatography, and comparing whether the types and the contents of the impurities in the two medicines are consistent; the reference formulation is zthromax;
and when the types and the contents of the impurities in the azithromycin tablet and the reference preparation are the same, judging that the structures of the azithromycin tablet and the reference preparation have consistency.
Optionally, the method also comprises crystal form comparison, wherein an X-ray diffraction method is adopted to detect the crystal forms of the azithromycin tablets and the reference preparation, and the diffraction angles of the crystal forms are compared.
Optionally, the method further comprises a dissolution curve comparison, wherein water, a phosphate buffer solution with pH6.8, a phosphate buffer solution with pH6.0, a phosphate buffer solution with pH5.0 and a hydrochloric acid solution with 0.1mol/L are used as dissolution media, dissolution rates at different sampling times are respectively measured, and a dissolution curve is obtained by drawing, so that a dissolution curve F2 value is obtained.
According to the technical scheme, the embodiment of the invention has the following advantages:
the invention provides a method for detecting azithromycin tablet impurities, which is characterized in that 0.05mol/L ammonium dihydrogen phosphate buffer solution and pyrrolidine-formic acid-acetonitrile mixed solution are selected as mobile phases for gradient elution, so that the accuracy of the detection method is improved, the detection time is reduced, the working efficiency in the production process is improved, and the types and the content of the impurities in the azithromycin tablet can be comprehensively detected. The invention also provides a consistency evaluation method, when the types and the contents of the impurities in the reference preparation and the azithromycin tablet are consistent, the consistency of the product structures and the quality of the reference preparation and the azithromycin tablet can be judged. The invention provides a detection method and a consistency evaluation method for azithromycin tablet impurities, which are used for solving the technical problems of low accuracy, long detection time and few detected impurity types of the existing detection method.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and it is obvious for those skilled in the art to obtain other drawings according to these drawings.
Figure 1 is an impurity comparison spectrum of an azithromycin tablet and a reference preparation provided by the embodiment 4 of the invention;
figure 2 is a schematic illustration of the dissolution profiles of azithromycin tablets provided in example 6 of the invention in different dissolution media;
FIG. 3 is a structural view of impurity A;
FIG. 4 is a structural view of impurity B;
FIG. 5 is a structural view of impurity C;
FIG. 6 is a structural view of impurity E;
FIG. 7 is a structural view of impurity F;
FIG. 8 is a structural view of impurity G;
FIG. 9 is a structural view of impurity H;
FIG. 10 is a structural view of impurity I;
FIG. 11 is a structural view of impurity J;
FIG. 12 is a structural view of impurity K;
FIG. 13 is a structural view of impurity L;
FIG. 14 is a structural view of the impurity M;
FIG. 15 is a structural view of impurity N;
FIG. 16 is a structural view of an impurity Q;
FIG. 17 is a structural view of an impurity R;
fig. 18 is a structural view of the impurity S.
Detailed Description
In order to make those skilled in the art better understand the technical solutions of the present invention, the following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and 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 invention. Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
The embodiment of the detection method of the azithromycin tablet impurity provided by the invention comprises the following steps of dissolving an azithromycin tablet sample (self-made, batch number: 200501) by a dissolving agent, and detecting by adopting a high performance liquid chromatography, wherein the chromatographic conditions are as follows: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column, and an ultraviolet detector is adopted to carry out gradient elution by taking 0.05mol/L ammonium dihydrogen phosphate buffer solution as a mobile phase A and taking a pyrrolidine-formic acid-acetonitrile mixed solution as a mobile phase B; the dissolving agent is formic acid aqueous solution, and ammonium dihydrogen phosphate buffer solution is adjusted to pH value of 6.5 by triethylamine solution.
The azithromycin tablet has higher stability in an acid environment, and the influence of the external environment on the detection result in the detection process can be reduced by adjusting the pH value of the mobile phase to be acidic. By selecting 0.05mol/L ammonium dihydrogen phosphate buffer solution and pyrrolidine-formic acid-acetonitrile mixed solution as mobile phase to carry out gradient elution, the accuracy of the detection method is improved, the detection time is reduced, the working efficiency in the production process is improved, and the types and the content of impurities in the azithromycin tablets are comprehensively detected. The method for detecting the azithromycin tablet impurities, provided by the embodiment of the invention, solves the technical problems of low accuracy, long detection time and few detected impurity types in the existing detection method.
Example 2
As a further improvement to example 1, the HPLC method employs a Waters Xterra RP18 liquid chromatography column, the column temperature is 38 ℃, the sample loading is 25 μ l, the flow rate is 1.5ml/min, the detection wavelength is 210nm, and the volume ratio of the mobile phase B pyrrolidine-formic acid-acetonitrile mixture is 5: 10: 85, gradient elution is carried out according to the following steps:
the volume ratio of the mobile phase A to the mobile phase B is 70: 30, carrying out the first elution for 0-30 minutes; the volume ratio of mobile phase a to mobile phase B was 90: 10, carrying out second elution for 30-50 minutes; the volume ratio of mobile phase a to mobile phase B was 95: 5, carrying out third elution for 50-65 minutes; the volume ratio of mobile phase a to mobile phase B was 70: and 30, carrying out fourth elution for 65-72 minutes.
Example 3
As a further improvement to example 2, a 90% aqueous formic acid solution was selected as the dissolving agent, and the azithromycin tablet samples were dissolved under ultrasonic dissolution conditions, wherein the power density at which ultrasonic dissolution was set at 0.65W/cm2～0.70W/cm2The sample dissolution is accelerated and the degassing treatment is carried out at the same time, so that the influence of air in the solution on the detection result is reduced; the dissolving temperature is set to 37 ℃, and the temperature is not suitable to be set too high, otherwise, the sample can be degraded, and the accuracy of the detection result is influenced.
Comparative example 1
As a comparative example of the invention, a method for detecting azithromycin tablet impurities is provided, which adopts high performance liquid chromatography to detect, wherein a mobile phase A is a mixed solution of 0.05 mol/dipotassium hydrogen phosphate solution and acetonitrile, and the volume ratio of the dipotassium hydrogen phosphate solution to the acetonitrile is 45: 55, wherein the dipotassium hydrogen phosphate solution is adjusted to the pH value of 8.2 by using a 20% phosphoric acid solution; the mobile phase B is methanol, and gradient elution is carried out according to the following steps:
the volume ratio of the mobile phase A to the mobile phase B is 75: 25, carrying out first elution for 0-35 minutes; the volume ratio of mobile phase a to mobile phase B was 95: 5, carrying out secondary elution for 35-64 minutes; the volume ratio of mobile phase a to mobile phase B was 95: 5, carrying out third elution for 64-65 minutes; the volume ratio of mobile phase a to mobile phase B was 75: and 25, carrying out fourth elution for 65-71 minutes.
In order to illustrate the advantages of the invention, the recovery test and the impurity content detection test are carried out on the azithromycin tablets according to the detection methods of the examples 2-3 and the comparative example 1, and the specific steps are as follows:
1. recovery test
Adopting a standard addition recovery test, precisely weighing 3 parts of azithromycin tablet samples containing 25mg of azithromycin, placing the azithromycin tablet samples into 50ml volumetric flasks, and adding 20ml of 0.05mol/L ammonium dihydrogen phosphate buffer solution for dissolving; after dissolving, respectively adding 15 mg, 25mg and 35mg of azithromycin reference substances (the purity is 94.3% by China institute for food and drug inspection), adding 0.05mol/L ammonium dihydrogen phosphate buffer solution for constant volume to obtain 3 solutions to be detected with different concentrations, respectively detecting the solutions to be detected according to the detection methods in the embodiments 2-3 and the comparative example 1, and calculating to obtain the average recovery rate. Wherein, any one of the 3 solutions to be detected with different concentrations is repeatedly subjected to sample injection detection for 6 times according to the detection methods in the embodiments 2-3 and the comparative example 1 to obtain the relative standard deviation RSD, and the result is as follows:
as can be seen from the above table, the recovery rate and the relative standard deviation of comparative example 1 are relatively low compared with those of examples 2 to 3, and the accuracy and precision are relatively low; and in the embodiment 3, 90% formic acid aqueous solution is selected as a dissolving agent, and the dissolution and the degassing treatment are carried out by selecting proper ultrasonic dissolution conditions, so that better accuracy and precision are obtained.
2. Test for detecting impurity content
Preparation of mixed control solution: and taking an appropriate amount of impurity A, B, C, E, F, G, H, I, J, K, L, M, N, Q, R, S and azithromycin, adding a diluent, dissolving and diluting to prepare a solution containing 0.05mg of each impurity and 10mg of azithromycin in every 1mL, and taking the solution as a mixed control solution. The volume ratio of the diluent is 7: 7: 6, the mixture of the ammonium dihydrogen phosphate solution, the methanol and the acetonitrile, wherein the preparation steps of the ammonium dihydrogen phosphate solution are as follows: weighing 1.73g of ammonium dihydrogen phosphate, adding water to dissolve and dilute the ammonium dihydrogen phosphate to 1000mL, and adjusting the pH value to 10.0 +/-0.1 by using an ammonia test solution, wherein the structure of the impurity A, B, C, E, F, G, H, I, J, K, L, M, N, Q, R, S is shown in a figure 3-18.
Preparing a test solution: precisely weighing 250mg of azithromycin tablets, putting the azithromycin tablets into a 25mL measuring flask, adding a proper amount of diluent, carrying out ultrasonic treatment for 10 minutes to dissolve the azithromycin tablets, cooling the azithromycin tablets, adding the diluent to be diluted to a scale, shaking the azithromycin tablets evenly, filtering the solution containing 10mg of azithromycin tablets in every 1mL of diluent, and taking filtrate to obtain the azithromycin tablets.
Control solution: precisely measuring 1mL of the test solution, placing into a 100mL measuring flask, adding the diluent to dilute to scale, and shaking up to obtain the final product.
The content of each impurity is detected according to the detection methods of the examples 2-3 and the comparative example 1, and the result is as follows:
as can be seen from the above table, the impurity types detected in comparative example 1 are less, the content of the unknown impurities which cannot be detected is more, and the detection effect is not good; the detection method of the embodiment 3 has less unknown impurity content than that of the embodiment 2, and the content of each impurity is more than that of the embodiment 2 on the whole, which shows that the detection method of the embodiment 3 is more precise, and the error in the detection method of the embodiment 2 is reduced.
Example 4
The invention also provides a consistency evaluation method based on the detection method of the azithromycin tablets impurities, which comprises the steps of comparing the azithromycin tablets with reference preparations for impurities;
the impurity comparison comprises detecting impurities in the azithromycin tablets and the reference preparation by adopting a high performance liquid chromatography, and comparing whether the types and the contents of the impurities in the two medicines are consistent; the reference formulation is zthromax.
And when the types and the contents of the impurities in the azithromycin tablet and the reference preparation are the same, judging that the structures of the azithromycin tablet and the reference preparation have consistency.
It should be noted that the detection method in embodiments 1 to 3 can be adopted for detection in this embodiment, and preferably the detection method in embodiment 3 is adopted for determination, and an impurity comparison spectrogram of the azithromycin tablet and the reference preparation is shown in fig. 1, so that the spectrogram comparison is basically consistent, and the types and contents of impurities in the reference preparation and the azithromycin tablet are consistent, so that the consistency of the product structures and the quality of the reference preparation and the azithromycin tablet can be determined.
Example 5
As a further improvement to example 4, this example also includes crystal form comparison; the crystal forms of the azithromycin tablets and the reference preparation are detected by adopting an X-ray diffraction method, and the diffraction angles of the crystal forms are compared, so that the results are as follows:
as can be seen from the above table, the crystal forms of the azithromycin tablets and the reference preparation have consistency, thus demonstrating that the solubility and bioavailability of the azithromycin tablets and the reference preparation also have consistency.
Example 6
As a further improvement to example 4, this example further includes a dissolution curve comparison, in which water, ph6.8 phosphate buffer solution, ph6.0 phosphate buffer solution, ph5.0 phosphate buffer solution and 0.1mol/L hydrochloric acid solution are used as dissolution media, an azithromycin tablet and a reference preparation are respectively dissolved in the dissolution media, the dissolution media are placed in a dissolution device, the rotation speed of the dissolution device is set to 50 revolutions per minute, dissolution rates at different times are measured by sampling at 5min, 10min, 15min, 20min and 30min, dissolution curves of the azithromycin tablet in different dissolution media are plotted to obtain a dissolution curve F2 value of the azithromycin tablet and the reference preparation, and the dissolution curves of the azithromycin tablet in different dissolution media are shown in fig. 2. The F2 values of the azithromycin tablet and the reference preparation measured in the embodiment reach more than 85 percent, which shows that the dissolution curves of the azithromycin tablet and the reference preparation have consistency, the drug release mechanism in human bodies is basically consistent, and the drug effect is consistent.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for detecting azithromycin tablet impurities is characterized by comprising the steps of dissolving an azithromycin tablet sample by using a dissolving agent, and detecting by adopting a high performance liquid chromatography, wherein the chromatographic conditions are as follows: the chromatographic column is an octadecylsilane chemically bonded silica chromatographic column, and an ultraviolet detector is adopted to carry out gradient elution by taking 0.05mol/L ammonium dihydrogen phosphate buffer solution as a mobile phase A and taking a pyrrolidine-formic acid-acetonitrile mixed solution as a mobile phase B; the dissolving agent is formic acid aqueous solution, and the pH value of the ammonium dihydrogen phosphate buffer solution is adjusted to 6.5 by triethylamine solution.
2. The method for detecting azithromycin tablet impurities of claim 1, wherein the chromatographic column is: waters XterraTM RP18 liquid chromatography column.
3. The method for detecting the azithromycin tablet impurity of claim 1, wherein the volume ratio of the pyrrolidine-formic acid-acetonitrile mixture is 5: 10: 85.
4. the method for detecting azithromycin tablet impurities of claim 1, wherein the gradient elution comprises:
adopting the volume ratio of the mobile phase A to the mobile phase B as 70: 30, carrying out the first elution for 0-30 minutes; the volume ratio of the mobile phase A to the mobile phase B is 90: 10, carrying out second elution for 30-50 minutes; the volume ratio of the mobile phase A to the mobile phase B is 95: 5, carrying out third elution for 50-65 minutes; the volume ratio of the mobile phase A to the mobile phase B is 70: and 30, carrying out fourth elution for 65-72 minutes.
5. The method for detecting azithromycin tablet impurity of claim 1, wherein the chromatographic conditions further comprise: the column temperature was 38 ℃, the sample injection amount was 25. mu.l, the flow rate was 1.5ml/min, and the detection wavelength was 210 nm.
6. The method for detecting azithromycin tablet impurity of claim 1, wherein the dissolving agent is 90% formic acid aqueous solution.
7. The method for detecting azithromycin tablet impurity of claim 1 wherein the dissolution agent dissolves the azithromycin tablet sample under ultrasonic dissolution conditions.
8. A consistency evaluation method based on the detection method of azithromycin tablets impurities as claimed in any of claims 1 to 7 is characterized by comprising the following steps of comparing the azithromycin tablets with a reference preparation for impurities;
the impurity comparison comprises detecting impurities in the azithromycin tablets and the reference preparation by adopting the high performance liquid chromatography, and comparing whether the types and the contents of the impurities in the two medicines are consistent; the reference formulation is zthromax;
and when the types and the contents of the impurities in the azithromycin tablet and the reference preparation are the same, judging that the structures of the azithromycin tablet and the reference preparation have consistency.
9. The consistency evaluation method according to claim 8, further comprising crystal form comparison, wherein the crystal forms of the azithromycin tablet and the reference preparation are detected by an X-ray diffraction method, and diffraction angles of the crystal forms are compared.
10. The method for evaluating the consistency according to claim 8, further comprising a dissolution curve comparison, wherein dissolution rates at different sampling times are respectively measured by using water, a phosphate buffer solution with pH6.8, a phosphate buffer solution with pH6.0, a phosphate buffer solution with pH5.0 and a hydrochloric acid solution with 0.1mol/L as dissolution media, and a dissolution curve is obtained by drawing, so as to obtain a value of the dissolution curve F2.
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