CN113624859A - Method for detecting related substances in pazufloxacin mesylate raw material medicine by adopting HPLC - Google Patents
Method for detecting related substances in pazufloxacin mesylate raw material medicine by adopting HPLC Download PDFInfo
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- CN113624859A CN113624859A CN202110738079.8A CN202110738079A CN113624859A CN 113624859 A CN113624859 A CN 113624859A CN 202110738079 A CN202110738079 A CN 202110738079A CN 113624859 A CN113624859 A CN 113624859A
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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
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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
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- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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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
- G01N30/62—Detectors specially adapted therefor
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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
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- G01N30/8624—Detection of slopes or peaks; baseline correction
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Abstract
The invention discloses a method for detecting related substances in pazufloxacin mesilate by adopting HPLC (high performance liquid chromatography), which comprises the following steps of: preparing a test solution of pazufloxacin mesilate bulk drug, and taking the test solution to dilute to obtain a control solution; acetonitrile-10% triethylamine methanesulfonate solution-1.0 mol/L dipotassium hydrogen phosphate-water in a volume ratio of 30:10:7:170 are respectively used as a first mobile phase, and acetonitrile-10% triethylamine methanesulfonate solution-1.0 mol/L dipotassium hydrogen phosphate-water in a volume ratio of 45:10:7:138 are used as a second mobile phase to detect pazufloxacin methanesulfonate bulk drug. Therefore, the first mobile phase and the second mobile phase are combined for use, so that the related substances of the pazufloxacin mesylate raw material medicine can be detected more accurately and scientifically.
Description
Technical Field
The invention relates to the field of quality control of pazufloxacin mesilate, in particular to a method for detecting related substances in pazufloxacin mesilate bulk drugs by adopting HPLC (high performance liquid chromatography).
Background
The pazufloxacin mesylate is a novel fluoroquinolone antibacterial drug developed by Japanese research, is a mesylate of pazufloxacin, and has the characteristics of wide antibacterial spectrum, high antibacterial activity, small side effect, good tolerance and the like. It can be used for treating gram-positive and gram-negative bacterial infections, such as bronchial and pulmonary infection, bacillary dysentery, urinary system infection, skin infection, and soft tissue infection.
During the synthesis process and the subsequent storage, transportation and use processes of pazufloxacin mesilate, some related substances (related substances) with similar structures to the pazufloxacin mesilate may be generated, and the related substances may influence the curative effect and the safety of the medicine, so that the detection of the related substances is essential to the quality control of the medicine.
High Performance Liquid Chromatography (HPLC) can be used for detecting related substances in pazufloxacin mesylate. In a known method for detecting related substances in pazufloxacin mesylate by HPLC, acetonitrile-10% triethylamine mesylate-1M dipotassium hydrogen phosphate-water (30:10:7:153) is used as a mobile phase. The inventors of the present application have found that when the mobile phase is used for detection, separation of the relevant substance from the main drug (pazufloxacin mesylate) is not preferable. Furthermore, the inventors have further found that when a substance of interest is detected using the mobile phase, a substance of interest having a relatively small polarity and a retention time after the main drug cannot be detected efficiently.
Therefore, there is a need to further improve the mobile phase of HPLC to detect relevant substances in pazufloxacin mesylate bulk drug more comprehensively and accurately.
Disclosure of Invention
The invention provides a method for detecting related substances in pazufloxacin mesilate bulk drugs by adopting HPLC (high performance liquid chromatography), so as to more comprehensively and accurately detect the related substances in the pazufloxacin mesilate bulk drugs.
The technical scheme is as follows:
a method for detecting related substances in pazufloxacin mesylate raw material medicines by adopting HPLC comprises the following steps:
(1) preparing a test solution of pazufloxacin mesilate bulk drug, and taking the test solution to dilute to obtain a control solution;
(2) taking acetonitrile-10% triethylamine methanesulfonate solution-1.0 mol/L dipotassium hydrogen phosphate-water with the volume ratio of 30:10:7:170 as a first mobile phase, respectively injecting a test solution and a control solution into a high performance liquid chromatograph, and recording the chromatogram until the retention time of characteristic peaks of pazufloxacin methanesulfonate is 2 times;
(3) taking acetonitrile-10% triethylamine methanesulfonate solution-1.0 mol/L dipotassium hydrogen phosphate-water with the volume ratio of 45:10:7:138 as a second mobile phase, respectively injecting the test solution and the control solution into a high performance liquid chromatograph, and recording the chromatogram until the retention time of characteristic peaks of pazufloxacin methanesulfonate is 7 times;
(4) comparing the peak area of the related substances with the retention time less than the characteristic peak of pazufloxacin mesylate in the spectrogram of the test solution obtained in the step 2 with the characteristic peak area of pazufloxacin mesylate in the spectrogram of the control solution obtained in the step 2, and
and (3) comparing the peak area of the related substance with the retention time longer than the characteristic peak of pazufloxacin mesylate in the spectrogram of the test solution obtained in the step (3) with the characteristic peak area of pazufloxacin mesylate in the spectrogram of the control solution obtained in the step (3).
In some embodiments of the present application, the test solution and the control solution are formulated with a first mobile phase as a solvent.
In some embodiments of the present application, the concentration of pazufloxacin mesylate drug substance in the test solution is 100 times greater than the control solution.
In some embodiments of the present application, the concentration of pazufloxacin mesylate drug substance in the test solution is 0.3 mg/ml.
In some embodiments of the present application, the sample size in step 2 and step 3 is 20 μ l.
In some embodiments herein, the chromatographic conditions for HPLC in step 2 and step 3 further comprise:
stationary phase: octadecylsilane chemically bonded silica gel, and a silane,
flow rate: 1.0ml/min of the mixture is added,
detection wavelength: 254 nm.
In some embodiments of the present application, step 4 further comprises:
determining the first content of the related substances according to the comparison result of the two spectrograms obtained in the step 2;
determining a second content of the related substances according to the comparison result of the two spectrograms obtained in the step 3;
and adding the first content of the related substances and the second content of the related substances to finally determine the content of all the related substances in the pazufloxacin mesylate raw material medicine.
Advantageous effects
According to the detection method, the proportion of the mobile phase is adjusted, the first mobile phase is used for HPLC detection, compared with the mobile phase in the prior art, the related substances with retention time smaller than the characteristic peak of pazufloxacin mesylate are well separated from the characteristic peak of pazufloxacin mesylate, and the retention time of the characteristic peak of pazufloxacin mesylate is appropriate. However, the first mobile phase cannot detect the related substances with relatively low polarity, the retention time of which is after pazufloxacin mesylate, which is the main drug.
In view of this, when the ratio of the mobile phase is further adjusted to obtain the second mobile phase and the relevant substance is detected using the second mobile phase, the relevant substance that cannot be detected using the first mobile phase can be effectively detected within 7 times of the retention time of pazufloxacin mesylate.
Therefore, the first mobile phase and the second mobile phase are combined for use, so that the related substances of the pazufloxacin mesylate can be detected more accurately and scientifically.
Drawings
FIG. 1A is an HPLC chromatogram of pazufloxacin mesylate bulk drug detected using a first mobile phase in example 1;
FIG. 1B is an HPLC chromatogram of comparative example 1 for detecting pazufloxacin mesylate bulk drug;
FIG. 2A is an HPLC chromatogram of pazufloxacin mesylate raw drug substance detected by a second mobile phase in example 2;
FIG. 2B is an HPLC chromatogram of comparative example 2 for detecting pazufloxacin mesylate bulk drug;
FIG. 3A is an HPLC chromatogram of a test solution of example 3 using a first mobile phase;
FIG. 3B is an HPLC chromatogram of a control solution of example 3 using a first mobile phase;
FIG. 3C is an HPLC chromatogram of the test solution of example 3 using a second mobile phase;
figure 3D is an HPLC chromatogram of a control solution of example 3 using a second mobile phase.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be clearly and completely described below through specific embodiments.
In the following examples, those not indicated with specific conditions were performed according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1 detection of pazufloxacin mesylate drug substance using first flow phase
The chromatographic conditions were as follows:
stationary phase: octadecylsilane chemically bonded silica gel, and a silane,
a first mobile phase: acetonitrile-10% Methylsulfonic acid Triethylamine-1M dipotassium phosphate-Water (30:10:7:170)
Flow rate: 1.0ml/min of the mixture is added,
detection wavelength: the wavelength of the light beam is 254nm,
sample introduction amount: 20 μ l.
The detection steps are as follows:
(1) taking 30mg of pazufloxacin mesilate as a raw material, precisely weighing, placing in a 100ml measuring flask, adding the first mobile phase for dissolving, diluting to a scale, and shaking uniformly to serve as a test solution.
(2) Under the condition of the first mobile phase, 20 mul of the test solution is injected into a liquid chromatograph, and the chromatogram is recorded until the retention time of the characteristic peak of pazufloxacin mesylate is 2 times, and the HPLC chromatogram is shown in figure 1A.
Wherein, the 10% triethylamine methanesulfonate solution is prepared as follows:
under the condition of ice bath, 30ml of methanesulfonic acid and 30ml of triethylamine are slowly added into 200ml of water, and after complete dissolution, water is added to 300 ml.
As can be seen from fig. 1A, the impurity peak of the relevant substance is well separated from the characteristic peak of pazufloxacin sulfonate, which is the main drug.
Comparative example 1 detection of Pazufloxacin mesylate drug substance (non-first mobile phase)
HPLC detection was performed on pazufloxacin mesylate as a crude drug under the condition of acetonitrile-10% triethylamine methanesulfonate-1M dipotassium hydrogen phosphate-water (30:10:7:153) as a mobile phase, and the chromatographic conditions and detection procedures except for the mobile phase were the same as those in example 1. The chromatogram obtained is shown in FIG. 1B.
As can be seen from fig. 1B, the impurity peak of the relevant substance is not perfectly separated from pazufloxacin sulfonate, which is the main drug.
As can be seen from the comparison between example 1 and comparative example 1, the separation degree of the related substances and the main drug can be improved by adjusting the first mobile phase obtained by different ratios of the buffer solution and the organic solvent.
Example 2 detection of pazufloxacin mesylate drug substance with a second flow
The chromatographic conditions were as follows:
stationary phase: octadecylsilane chemically bonded silica gel, and a silane,
a second mobile phase: acetonitrile-10% Methylsulfonic acid Triethylamine-1M dipotassium phosphate-Water (45:10:7:138)
Flow rate: 1.0ml/min of the mixture is added,
detection wavelength: the wavelength of the light beam is 254nm,
sample introduction amount: 20 μ l.
The detection steps are as follows:
(1) a test solution was prepared in the same manner as in the step (1) of example 1.
(2) Under the condition of the second mobile phase, 20 mul of the test solution is injected into a liquid chromatograph, and the chromatogram is recorded until the retention time of the characteristic peak of pazufloxacin mesilate is 7 times, and the HPLC chromatogram is shown in figure 2A.
As can be seen from fig. 2A, the second mobile phase can effectively detect some related substances with lower polarity and peaks after the retention time of the main drug, and the impurity peaks of the related substances are well separated from the main drug pazufloxacin sulfonate.
The substances with relatively low polarity are generally derived from some degradation products generated by the pazufloxacin mesylate through illumination, oxidation, high temperature and the action of acid and alkali during storage, transportation and use. Therefore, the quality of the pazufloxacin mesylate raw material medicine after storage and transportation can be better controlled by adopting the second mobile phase for HPLC detection.
Comparative example 2 HPLC detection of photodegraded Pazufloxacin mesylate (non-second mobile phase)
The pazufloxacin mesylate was subjected to HPLC detection under the condition of acetonitrile-10% triethylamine methanesulfonate-1M dipotassium hydrogenphosphate-water (70:10:7:113) as a mobile phase, and the chromatographic conditions and detection procedure except for the mobile phase were the same as in example 2. The chromatogram obtained is shown in FIG. 2B.
As can be seen from fig. 2B, the detection effect of the impurity peak of the relevant substance after the retention time of pazufloxacin sulfonate as the main drug is significantly worse than the detection result using the second mobile phase.
It can be seen from the comparison between example 2 and comparative example 2 that, according to the second mobile phase obtained by adjusting different ratios of the buffer solution to the organic solvent, the related substances with lower polarity after the retention time of pazufloxacin sulfonate can be effectively detected within 7 times of the retention time of the main drug, and the second mobile phase has good separation degree with the main drug. The mobile phase used in comparative example 2 was not satisfactory.
Example 3 detection Using a combination of a first mobile phase and a second mobile phase vs Pazufloxacin mesylate
Pazufloxacin mesylate raw material medicine (internal batch number 0125) synthesized inside a company is subjected to detection of related substances.
The detection steps are as follows:
(1) taking 30mg of pazufloxacin mesilate raw material medicine, precisely weighing, placing in a 100ml measuring flask, adding the first mobile phase for dissolving, diluting to a scale, and shaking uniformly to serve as a test solution; precisely measuring 1ml of the test solution, placing the test solution into a 100ml measuring flask, diluting the test solution to a scale with the first mobile phase, and shaking up to obtain a control solution.
(2) Under the condition of a first mobile phase, respectively taking a test solution and a control solution, injecting the test solution and the control solution into a high performance liquid chromatograph, and recording the retention time of a characteristic peak of pazufloxacin mesylate when the chromatogram is 2 times that of the chromatogram, wherein the chromatograms of the test solution and the control solution are respectively shown in a figure 3A and a figure 3B;
(3) under the condition of a second mobile phase, respectively injecting a test solution and a control solution into a high performance liquid chromatograph, and recording the retention time of characteristic peaks of pazufloxacin mesylate of which the chromatogram is 7 times that of the chromatogram, wherein the chromatograms of the test solution and the control solution are respectively shown in a figure 3C and a figure 3D;
(4) comparing the peak area of the related substance with retention time less than that of pazufloxacin mesylate in figure 3A with the characteristic peak area of pazufloxacin mesylate in figure 3B, thereby determining the first content of the related substance,
comparing the peak area of the related substance with the retention time of the pazufloxacin mesylate characteristic peak in the graph 3C with the characteristic peak area of the pazufloxacin mesylate in the graph 3D, thereby determining the second content of the related substance.
And adding the contents of the two related substances to obtain the total content of the related substances in the pazufloxacin mesilate bulk drug.
Other chromatographic conditions were as follows:
a chromatographic column: octadecylsilane chemically bonded silica;
flow rate: 1.0ml/min of the mixture is added,
detection wavelength: 254 nm.
As can be seen from FIGS. 3A-D, pazufloxacin mesylate bulk drug substance of batch 0125, had little or no related substances of small polarity, probably because the batch of pazufloxacin mesylate had substantially no degradation.
And (3) respectively detecting two batches of pazufloxacin mesylate raw material medicines with the batch numbers of 0224 and 0324 according to the detection method.
The detection results of three batches of pazufloxacin mesylate bulk drugs are shown in the following table:
the above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (7)
1. A method for detecting related substances in pazufloxacin mesylate raw material medicines by adopting HPLC is characterized by comprising the following steps:
(1) preparing a test solution of pazufloxacin mesilate bulk drug, and taking the test solution to dilute to obtain a control solution;
(2) taking acetonitrile-10% triethylamine methanesulfonate solution-1.0 mol/L dipotassium hydrogen phosphate-water with the volume ratio of 30:10:7:170 as a first mobile phase, respectively injecting a test solution and a control solution into a high performance liquid chromatograph, and recording the chromatogram until the retention time of characteristic peaks of pazufloxacin methanesulfonate is 2 times;
(3) taking acetonitrile-10% triethylamine methanesulfonate solution-1.0 mol/L dipotassium hydrogen phosphate-water with the volume ratio of 45:10:7:138 as a second mobile phase, respectively injecting the test solution and the control solution into a high performance liquid chromatograph, and recording the chromatogram until the retention time of characteristic peaks of pazufloxacin methanesulfonate is 7 times;
(4) comparing the peak area of the related substances with the retention time less than the characteristic peak of pazufloxacin mesylate in the spectrogram of the test solution obtained in the step 2 with the characteristic peak area of pazufloxacin mesylate in the spectrogram of the control solution obtained in the step 2, and
and (3) comparing the peak area of the related substance with the retention time longer than the characteristic peak of pazufloxacin mesylate in the spectrogram of the test solution obtained in the step (3) with the characteristic peak area of pazufloxacin mesylate in the spectrogram of the control solution obtained in the step (3).
2. The method of claim 1, wherein the test solution and the control solution are formulated with a first mobile phase as a solvent.
3. The method of claim 2, wherein the concentration of pazufloxacin mesylate drug substance in the test solution is 100 times greater than the control solution.
4. The method of claim 3, wherein the concentration of pazufloxacin mesylate drug substance in the test solution is 0.3 mg/ml.
5. The method of claim 1, wherein the sample size in step 2 and step 3 is 20 μ l.
6. The method of any one of claims 1 to 5, wherein the chromatographic conditions of the HPLC in step 2 and step 3 further comprise:
stationary phase: octadecylsilane chemically bonded silica gel, and a silane,
flow rate: 1.0ml/min of the mixture is added,
detection wavelength: 254 nm.
7. The method of any one of claims 1-5, wherein step 4 further comprises:
determining the first content of the related substances according to the comparison result of the two spectrograms obtained in the step 2;
determining a second content of the related substances according to the comparison result of the two spectrograms obtained in the step 3;
and adding the first content of the related substances and the second content of the related substances to finally determine the content of all the related substances in the pazufloxacin mesylate raw material medicine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114354794A (en) * | 2021-12-29 | 2022-04-15 | 四川美大康佳乐药业有限公司 | Quality control method of pazufloxacin mesilate injection |
| WO2023272962A1 (en) * | 2021-06-30 | 2023-01-05 | 海南海神同洲制药有限公司 | Method for detecting small polar impurities in pazufloxacin mesylate bulk drug |
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Cited By (2)
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| WO2023272962A1 (en) * | 2021-06-30 | 2023-01-05 | 海南海神同洲制药有限公司 | Method for detecting small polar impurities in pazufloxacin mesylate bulk drug |
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Application publication date: 20211109 |