CN113702517A - Method for detecting small-polarity impurities in pazufloxacin mesylate raw material medicine - Google Patents
Method for detecting small-polarity impurities in pazufloxacin mesylate raw material medicine Download PDFInfo
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Abstract
The application discloses a method for detecting small-polarity impurities in pazufloxacin mesylate raw material medicines, which adopts a high performance liquid chromatography for detection, wherein a mobile phase is acetonitrile-10% triethylamine methanesulfonate solution-1.0 mol/L dipotassium hydrogen phosphate-water in a volume ratio of 45:10:7: 138; the method comprises the following steps: and respectively injecting the test solution and the control solution into a high performance liquid chromatograph, and recording the retention time of the characteristic peak of pazufloxacin mesylate, which is 7 times of the chromatogram. The method adopts HPLC to detect pazufloxacin mesilate bulk drug, and can effectively detect the small-polarity impurities with retention time larger than the characteristic peak of pazufloxacin mesilate within 7 times of the retention time of the pazufloxacin mesilate through the mobile phase with specific proportion. Therefore, the quality control of the pazufloxacin mesilate bulk drug can be realized more accurately and scientifically.
Description
Technical Field
The application relates to the field of quality control of pazufloxacin mesilate bulk drugs, in particular to a method for detecting small-polarity impurities in the pazufloxacin mesilate bulk drugs.
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 storage, transportation and use of pazufloxacin mesilate bulk drugs, degradation products may be generated through the action of light, oxidation, high temperature and acid and alkali, and the degradation products may affect the curative effect and even the safety of the drugs, so that the degradation products need to be detected.
In the prior art, High Performance Liquid Chromatography (HPLC) is generally adopted to detect related substances in pazufloxacin sulfonate bulk drugs. After the inventor researches a large number of HPLC detection methods, the flow adopted by the HPLC detection methods is relatively low-polarity impurities, particularly the impurities with the retention time longer than the characteristic peak of pazufloxacin mesylate serving as a main medicine, and the detection cannot be effectively carried out. The impurities with small polarity may be derived from degradation products generated by the action of light, oxidation, high temperature and acid and alkali during the storage, transportation and use of pazufloxacin mesylate bulk drug, and the degradation products may affect the curative effect and even the safety of the drug, so the comprehensive and accurate detection of the impurities with small polarity is very necessary for the quality control of the drug.
Disclosure of Invention
The invention provides a method for detecting small-polarity impurities in pazufloxacin mesilate bulk drugs, which is used for more comprehensively and accurately controlling the quality of the pazufloxacin mesilate bulk drugs.
The technical scheme is as follows:
a method for detecting small polar impurities in pazufloxacin mesilate bulk drugs adopts high performance liquid chromatography for detection, and a mobile phase is acetonitrile-10% triethylamine mesilate solution-1.0 mol/L dipotassium hydrogen phosphate-water with the volume ratio of 45:10:7: 138;
the method comprises the following steps:
preparing a test solution of pazufloxacin mesylate raw material medicine by taking a mobile phase as a solvent;
diluting the test solution with a mobile phase to obtain a control solution;
respectively injecting the test solution and the control solution into a high performance liquid chromatograph, and recording the retention time of the characteristic peak of pazufloxacin mesylate, the time of which is 7 times that of the chromatogram;
and comparing the peak area of the impurity with the retention time of the pazufloxacin mesylate characteristic peak in the obtained test solution spectrogram with the characteristic peak area of the pazufloxacin mesylate in the control solution spectrogram, thereby determining the content of the impurity relative to the pazufloxacin mesylate.
In some embodiments of the present application, the control solution is obtained by diluting a test solution 100-fold.
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 of the hplc is 20 μ l.
In some embodiments of the present application, the chromatographic conditions of high performance liquid chromatography 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, the degree of separation by high performance liquid chromatography is 1.6.
In some embodiments of the present application, the theoretical plate number of the high performance liquid chromatography should not be less than 2000 calculated from the characteristic peak of pazufloxacin mesylate.
In some embodiments of the present application, before separately taking the test solution and the control solution to inject into the hplc, the method further comprises:
and (3) injecting 20 mu l of the control solution into a liquid chromatograph, and adjusting the detection sensitivity to ensure that the peak height of the main component chromatographic peak is 10-25% of the full range.
Advantageous effects
According to the detection method, HPLC is adopted to detect pazufloxacin mesilate bulk drug, and by the mobile phase with a specific ratio, small-polarity impurities with retention time larger than the characteristic peak of pazufloxacin mesilate can be effectively detected within 7 times of retention time of pazufloxacin mesilate. Therefore, the quality control of the pazufloxacin mesilate bulk drug can be realized more accurately and scientifically.
Drawings
FIG. 1A is an HPLC chromatogram of pazufloxacin mesylate raw drug substance detected by using a mobile phase 1 in example 1;
FIG. 1B is an HPLC chromatogram of pazufloxacin mesylate raw drug substance detected by using a mobile phase 2 in example 1;
FIG. 1C is an HPLC chromatogram of pazufloxacin mesylate raw drug substance detected using mobile phase 3 in example 1;
FIG. 1D is an HPLC chromatogram of pazufloxacin mesylate raw drug substance detected using mobile phase 4 in example 1;
FIG. 2 is an HPLC chromatogram of pazufloxacin mesylate bulk drug after photodegradation in example 2;
FIG. 3 is an HPLC chromatogram of pazufloxacin mesylate drug substance after acid degradation in example 3;
FIG. 4 is an HPLC chromatogram of pazufloxacin mesylate drug substance after base degradation in example 4.
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 screening of mobile phases for detection of small polar impurities
The flow phase shown in table 1 below was used for detection against pazufloxacin mesylate as the bulk drug, respectively.
TABLE 1
| Mobile phase 1 | Acetonitrile-10% Methylsulfonic acid Triethylamine-1M dipotassium phosphate-Water (30:10:7:170) |
| Mobile phase 2 | Acetonitrile-10% Methylsulfonic acid Triethylamine-1M dipotassium phosphate-Water (30:10:7:153) |
| Mobile phase 3 | Acetonitrile-10% Methylsulfonic acid Triethylamine-1M dipotassium phosphate-Water (45:10:7:138) |
| Mobile phase 4 | Acetonitrile-10% Methylsulfonic acid Triethylamine-1M dipotassium phosphate-Water (70:10:7:113) |
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.
The chromatographic conditions were as follows:
stationary phase: octadecylsilane chemically bonded silica gel, and a silane,
mobile phase: see Table 1
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) preparing a test solution: taking 30mg of pazufloxacin mesilate raw material medicine, precisely weighing, placing in a 100ml measuring flask, adding a mobile phase for dissolving, diluting to a scale, and shaking uniformly to serve as a test solution.
(2) According to the chromatographic conditions, respectively taking 20 μ l of the test solution, injecting into a liquid chromatograph, recording the chromatogram to 2 times of the retention time of the characteristic peak of pazufloxacin mesylate under the conditions of a mobile phase 1 and a mobile phase 2, and recording the chromatogram to 7 times of the retention time of the characteristic peak of pazufloxacin mesylate under the conditions of a mobile phase 3 and a mobile phase 4, wherein HPLC chromatograms corresponding to different flows are respectively shown in figures 1A-1D.
As can be seen from fig. 1A to fig. 1D, when the pazufloxacin mesylate raw material drug is detected by using the mobile phase 1 and the mobile phase 2, impurities with retention time longer than the characteristic peak of pazufloxacin mesylate cannot be detected. For the mobile phase 3, related substances with lower polarity after the retention time of the pazufloxacin mesylate can be effectively detected within 7 times of the retention time of the pazufloxacin mesylate, and the mobile phase has good separation degree with the main drug. The detection effect using mobile phase 4 is not ideal compared to mobile phase 3.
Therefore, the small-polarity impurities can be comprehensively and accurately detected within 7 times of the retention time of the characteristic peak of pazufloxacin mesylate, by adopting the mobile phase of acetonitrile-10% triethylamine methanesulfonate solution-1.0 mol/L dipotassium hydrogen phosphate-water in the volume ratio of 45:10:7: 138.
Example 2 HPLC qualitative detection of photodegraded pazufloxacin mesylate bulk drug
The mobile phase 3 was used and the other chromatographic conditions were the same as in example 1.
The detection steps are as follows:
(1) preparing a photodegradation test sample solution: taking 30mg of the product, placing the product in a 100ml measuring flask, preparing a solution containing 300 mu g of pazufloxacin mesilate per 1ml by using a mobile phase, and placing the solution under ultraviolet light for 7 days to serve as a test solution.
(2) HPLC detection was carried out in the same manner as in example 1. The chromatogram is shown in FIG. 2.
As can be seen from fig. 2, for the bulk drug after photodegradation, the mobile phase provided by the present application can comprehensively and accurately detect the small-polarity impurities generated by the degradation within 7 times of the retention time of the pazufloxacin mesylate characteristic peak.
Example 3 the mobile phase 3 was used for the HPLC qualitative detection of acid-degraded pazufloxacin mesylate bulk drug, and the other chromatographic conditions were the same as in example 1.
The detection steps are as follows:
(1) preparing an acid degradation test solution: 30mg of pazufloxacin mesilate raw material medicine is taken and placed in a 50ml measuring flask, 25ml of 1.0mol/L hydrochloric acid is added and heated in a boiling water bath in a dark place for 12 hours, and 1.0mol/L sodium hydroxide is additionally added to dilute and neutralize to a scale for being used as a test solution.
(2) HPLC detection was carried out in the same manner as in example 1. The chromatogram is shown in FIG. 3. As can be seen from fig. 3, for the crude drug after acid degradation, the mobile phase provided by the present application can comprehensively and accurately detect the small-polarity impurities generated by degradation within 7 times of the retention time of the pazufloxacin mesylate characteristic peak.
Example 4 the mobile phase 3 was used for HPLC qualitative detection of pazufloxacin mesylate bulk drug after base degradation, and other chromatographic conditions were the same as in example 1.
The detection steps are as follows:
(1) preparing an alkali degradation test solution: 30mg of pazufloxacin mesilate raw material medicine is taken and placed in a 50ml measuring flask, 25ml of 1.0mol/L sodium hydroxide is added and heated in a boiling water bath in dark place for 12 hours, and 1.0mol/L hydrochloric acid is added for dilution and neutralization to the scale to be used as a test solution.
(2) HPLC detection was carried out in the same manner as in example 1. The chromatogram is shown in FIG. 4.
As can be seen from fig. 4, for the bulk drug after the base degradation, the mobile phase provided by the present application can comprehensively and accurately detect the small-polarity impurities generated by the degradation within 7 times of the retention time of the pazufloxacin mesylate characteristic peak.
Example 5 HPLC quantitative detection of Pazufloxacin mesylate drug substance
The mobile phase 3 was used and the other chromatographic conditions were the same as in example 1.
The detection steps are as follows:
taking 30mg of pazufloxacin mesilate raw material medicine, precisely weighing, placing in a 100ml measuring flask, adding a 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 in a measuring flask of 100ml, diluting the test solution to a scale with a mobile phase, and shaking up to obtain a control solution.
And (3) injecting 20 mu l of the control solution into a liquid chromatograph, and adjusting the detection sensitivity to ensure that the peak height of the main component chromatographic peak is 10-25% of the full range.
Respectively taking 20 mul of each of the test solution and the control solution, injecting into a liquid chromatograph, and recording the chromatogram until the retention time of the main component peak is 7 times.
Measuring the sum of the peak areas of various impurities with retention time longer than the characteristic peak of pazufloxacin mesylate as the main drug in the chromatogram of the test solution, and comparing the sum with the peak area of pazufloxacin mesylate as the main drug in the chromatogram of the control solution to determine the content of the degradation product.
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 (8)
1. A detection method of small polar impurities in pazufloxacin mesylate bulk drugs is characterized in that high performance liquid chromatography is adopted for detection, and a mobile phase is acetonitrile-10% triethylamine methanesulfonate solution-1.0 mol/L dipotassium hydrogen phosphate-water with a volume ratio of 45:10:7: 138;
the method comprises the following steps:
preparing a test solution of pazufloxacin mesylate raw material medicine by taking a mobile phase as a solvent;
diluting the test solution with a mobile phase to obtain a control solution;
respectively injecting the test solution and the control solution into a high performance liquid chromatograph, and recording the retention time of the characteristic peak of pazufloxacin mesylate, the time of which is 7 times that of the chromatogram;
and comparing the peak area of the impurity with the retention time of the pazufloxacin mesylate characteristic peak in the obtained test solution spectrogram with the characteristic peak area of the pazufloxacin mesylate in the control solution spectrogram, thereby determining the content of the impurity relative to the pazufloxacin mesylate.
2. The method of claim 1, wherein the control solution is obtained by diluting a test solution 100-fold.
3. The method of claim 2, wherein the concentration of pazufloxacin mesylate drug substance in the test solution is 0.3 mg/ml.
4. The method of claim 1, wherein the sample size of the hplc is 20 μ l.
5. The method of any one of claims 1-4, wherein the chromatographic conditions of high performance liquid chromatography 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.
6. The method of claim 1, wherein the high performance liquid chromatography separation is 1.6.
7. The method of claim 1, wherein the theoretical plate number of the high performance liquid chromatography is not less than 2000 calculated from a characteristic peak of pazufloxacin mesylate.
8. The method of any one of claims 1-6, wherein prior to separately taking the test solution and the control solution for injection into the high performance liquid chromatograph, the method further comprises:
and (3) injecting 20 mu l of the control solution into a liquid chromatograph, and adjusting the detection sensitivity to ensure that the peak height of the main component chromatographic peak is 10-25% of the full range.
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| CN202110738109.5A CN113702517A (en) | 2021-06-30 | 2021-06-30 | Method for detecting small-polarity impurities in pazufloxacin mesylate raw material medicine |
| PCT/CN2021/119262 WO2023272962A1 (en) | 2021-06-30 | 2021-09-18 | Method for detecting small polar impurities in pazufloxacin mesylate bulk drug |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| CN115919761B (en) * | 2023-01-29 | 2023-07-21 | 浙江莎普爱思药业股份有限公司 | Pazufloxacin mesylate liquid preparation and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101897666A (en) * | 2009-05-31 | 2010-12-01 | 北京四环科宝制药有限公司 | Pazufloxacin mesilate injection preparation and detection method thereof |
| CN105287371A (en) * | 2015-11-24 | 2016-02-03 | 河北智同生物制药有限公司 | Pazufloxacin mesilate injection composition and preparation method thereof |
| CN105388221A (en) * | 2015-10-13 | 2016-03-09 | 康普药业股份有限公司 | Pazufloxacin mesilate quality detection method |
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| CN102295652A (en) * | 2011-06-27 | 2011-12-28 | 辽宁海神联盛制药有限公司 | Improvement method for pazufloxacin mesylate synthesis process |
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| CN113640403A (en) * | 2021-07-12 | 2021-11-12 | 海南海神同洲制药有限公司 | Content detection method of pazufloxacin mesilate bulk drug |
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2021
- 2021-06-30 CN CN202110738109.5A patent/CN113702517A/en active Pending
- 2021-09-18 WO PCT/CN2021/119262 patent/WO2023272962A1/en unknown
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| CN101897666A (en) * | 2009-05-31 | 2010-12-01 | 北京四环科宝制药有限公司 | Pazufloxacin mesilate injection preparation and detection method thereof |
| CN105388221A (en) * | 2015-10-13 | 2016-03-09 | 康普药业股份有限公司 | Pazufloxacin mesilate quality detection method |
| CN105287371A (en) * | 2015-11-24 | 2016-02-03 | 河北智同生物制药有限公司 | Pazufloxacin mesilate injection composition and preparation method thereof |
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| PHAPALE PB 等: "Analysis of Pazufloxacin Mesilate in Human Plasma and Urine by LC with Fluorescence and UV Detection, and Its Application to Pharmacokinetic Study", 《CHROMATOGRAPHIA》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20211126 |