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Detection method of moxifloxacin hydrochloride related substances

A technology of moxifloxacin hydrochloride and detection method, applied in the field of drug analysis and detection, can solve problems such as poor resolution

Active Publication Date: 2021-11-02
SHANDONG LUKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006]Related substances are one of the important quality control points for drug safety. Moxifloxacin hydrochloride is listed in USP43 (United States Pharmacopoeia), EP10.5 (European It is recorded in British Pharmacopoeia), among which, in terms of general impurities, by reproducing the analysis methods of various pharmacopoeias, it was found that the peaks of impurity L and impurity M in the detection method of related substances in BP2021 moxifloxacin hydrochloride raw material drug did not appear; for USP43 The detection method of related substances in moxifloxacin hydrochloride tablets was reproduced, and the results showed that the peaks of impurity C and impurity V overlapped, and the separation of impurity B, impurity C, impurity V, impurity D, and impurity E was poor

Method used

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  • Detection method of moxifloxacin hydrochloride related substances
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  • Detection method of moxifloxacin hydrochloride related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The detection method for related substances of moxifloxacin hydrochloride raw material in Pharmacopoeia BP2021 is reproduced, and the chromatographic conditions are shown in Table 4.

[0062] Table 4 Reproducibility of detection method for related substances in raw materials of BP2021 moxifloxacin hydrochloride

[0063]

[0064] Adopt the standards of moxifloxacin hydrochloride, impurity A, impurity B, impurity C, impurity D, impurity E, impurity F, impurity L and impurity M to prepare impurity mixed solution, solvent is the diluent shown in Table 4, mixed solution The concentration of each substance in the formula is: moxifloxacin hydrochloride 1mg / mL, the concentration of impurity A ~ impurity M are all 10μg / mL;

[0065] Adopt the standard products of impurity A, impurity B, impurity C, impurity D, impurity E, impurity F, impurity L and impurity M to prepare positioning solution, the solvent is the diluent shown in Table 4; the concentration of positioning solution...

Embodiment 2

[0072] The detection method of related substances in Moxifloxacin Hydrochloride Tablets in Pharmacopoeia USP43 was reproduced.

[0073] Chromatographic conditions: using the chromatographic column, sample volume, concentration of tetrabutylammonium bisulfate (0.5g / L) in the mobile phase buffer solution and the concentration of the test substance in BP2021 moxifloxacin hydrochloride API related substances detection method, the USP43 The mobile phase ratio and gradient of the detection method for related substances in moxifloxacin tablets were reproduced, and the specific chromatographic conditions are shown in Table 6.

[0074] Table 6 Reproducibility of detection method for related substances in moxifloxacin tablets in USP43

[0075]

[0076]

[0077] Use moxifloxacin hydrochloride, impurity P, impurity H, impurity F, impurity A, impurity B, impurity V, impurity C, impurity D, impurity E, impurity L, impurity M and impurity J to prepare impurity mixed solution, solvent i...

Embodiment 3

[0084] The mobile phase A, mobile phase B and gradient elution method of the detection method in UPS43 were changed, and the changed scheme was recorded as optimization-1. The specific detection conditions are shown in Table 8.

[0085] Table 8 Chromatographic conditions for the detection method of related substances of moxifloxacin hydrochloride

[0086]

[0087] Using the diluent in Table 8 as the solvent, prepare the mixed impurity solution according to the method in Example 2, take 10 μL of the mixed impurity solution, inject it into the liquid chromatograph, and record the chromatogram. The results are shown in image 3 .

[0088] according to image 3 It can be seen that under the conditions of optimization-1, the separation degree of impurity C and impurity V is greater than 1.5, and the separation degree of impurity E and previously unknown impurities is greater than 1.5. During the laboratory process monitoring, it is found that impurity B and impurity V cannot re...

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Abstract

The invention relates to the technical field of drug analysis and detection, and provides a detection method of moxifloxacin hydrochloride related substances. The related substances of moxifloxacin hydrochloride are detected by adopting high performance liquid chromatography, and the detection conditions are as follows: octadecylsilane chemically bonded silica is used as a filling agent of a chromatographic column; the wavelength of the UV detector is 291 nm to 319 nm; the column temperature is 25-40 DEG C; the flow velocity of the mobile phase is 0.8-1.3 mL / min; the sample injection volume is 10-50 [mu]L; the mobile phase A is a phosphate buffer solution-acetonitrile-methanol mixed solution; the mobile phase B is a phosphate buffer solution-acetonitrile-methanol mixed solution; the elution mode is gradient elution; and the diluent is a phosphate buffer-sulfate mixed solution. The method can realize effective separation between the main component and various impurities, is high in sensitivity, good in accuracy and relatively good in reproducibility, and can be used for qualitatively and quantitatively detecting various impurities in the moxifloxacin hydrochloride raw material.

Description

technical field [0001] The invention relates to the technical field of drug analysis and detection, in particular to a detection method for moxifloxacin hydrochloride related substances. Background technique [0002] Moxifloxacin hydrochloride, chemical name is 1-cyclopropyl-7-{(S,S)-2,8-diazo-bicyclo[4.3.0]nonan-8-yl}-6-fluoro-8- Methoxy-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid hydrochloride, the compound structural formula is: [0003] [0004] Moxifloxacin hydrochloride was originally developed by Bayer, and its moxifloxacin hydrochloride tablets and moxifloxacin hydrochloride sodium chloride injection have been imported into China. The tablet size is 400mg, and its trade name is The injection specification is 250mL: moxifloxacin 0.4g and sodium chloride 2.0g, the trade name is [0005] Moxifloxacin is an 8-methoxyfluoroquinolone antibacterial drug with broad-spectrum action and antibacterial activity. Moxifloxacin has broad-spectrum antibacterial activit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027Y02A50/30
Inventor 宋倩孔令兰刘蕊
Owner SHANDONG LUKANG PHARMA