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Method for separating moxifloxacin hydrochloride and impurities thereof by high performance liquid chromatography

A technology of moxifloxacin hydrochloride and high performance liquid chromatography, which is applied in the field of separation of moxifloxacin hydrochloride and its impurities by high performance liquid chromatography, and can solve problems such as evaluating the quality of moxifloxacin hydrochloride and monitoring important impurities of moxifloxacin hydrochloride

Active Publication Date: 2020-04-17
JIANGSU CHIA TAI FENGHAI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the quality control of moxifloxacin hydrochloride in the prior art is usually difficult to monitor its important impurities one by one, and it is difficult to evaluate the quality of moxifloxacin hydrochloride well.

Method used

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  • Method for separating moxifloxacin hydrochloride and impurities thereof by high performance liquid chromatography
  • Method for separating moxifloxacin hydrochloride and impurities thereof by high performance liquid chromatography
  • Method for separating moxifloxacin hydrochloride and impurities thereof by high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Chromatographic conditions:

[0078] Mobile phase: the aqueous phase is 0.01% heptafluorobutyric acid aqueous solution; the organic phase is methanol;

[0079] The elution procedure is as follows:

[0080]

[0081] Chromatographic column: Eclipse XDB phenyl bonded silica gel packed column (0.46cm*25cm, 5um)

[0082] Detection wavelength: 293nm

[0083] Flow rate: 1.3ml / min

[0084] Column temperature: 45°C

[0085] Injection volume: 10μl

[0086] Experimental steps:

[0087] 1) Weigh about 10mg of moxifloxacin hydrochloride reference substance, place it in a 10ml measuring bottle, add appropriate amount of each impurity stock solution (impurity M, H, A, B, C, D, E, J, I), so that each ml The mixed solution contains 1 ug of each impurity and 1 mg of moxifloxacin hydrochloride, and dilutes to the mark with methanol as a system suitability solution.

[0088] 2) Inject the system suitability solution into the liquid chromatograph, and record the test results.

[...

Embodiment 2

[0093] Chromatographic conditions:

[0094] Mobile phase: the aqueous phase is 0.01% heptafluorobutyric acid / trifluoroacetic acid mixture, wherein the volume ratio of heptafluorobutyric acid to trifluoroacetic acid is 2:1;

[0095] The organic phase is acetonitrile;

[0096] The elution procedure is as follows:

[0097]

[0098] Chromatographic column: Pentafluorophenyl bonded silica gel packed column (0.46cm*25cm, 5um)

[0099] Detection wavelength: 293nm

[0100] Flow rate: 1.3ml / min

[0101] Column temperature: 45°C

[0102] Injection volume: 10μl

[0103] Experimental procedure

[0104] 1) Weigh 10mg of moxifloxacin hydrochloride reference substance, place it in a 10ml measuring bottle, add appropriate amount of each impurity stock solution (impurity M, H, A, B, C, D, E, J, I), so that each ml mixes The solution contains 1 ug of each impurity and 1 mg of moxifloxacin hydrochloride, and dilutes to the mark with methanol as a system suitability solution.

[0105] ...

Embodiment 3

[0110] Chromatographic conditions:

[0111] Mobile phase: the aqueous phase is 0.002% nonafluorovaleric acid aqueous solution; the organic phase is methanol;

[0112] The elution procedure is as follows:

[0113]

[0114] Chromatographic column: Eclipse XDB phenyl bonded silica gel packed column (0.46cm*25cm, 5um)

[0115] Detection wavelength: 293nm

[0116] Flow rate: 1.3ml / min

[0117] Column temperature: 45°C

[0118] Injection volume: 10μl

[0119] Experimental steps:

[0120] 4) Weigh about 10 mg of Moxifloxacin Hydrochloride Sodium Chloride Injection Reference Substance, place it in a 10ml measuring bottle, add each impurity stock solution (impurity M, H, A, B, C, D, E, J, I) ) in an appropriate amount so that each milliliter of the mixed solution contains 1 ug of each impurity and 1 mg of moxifloxacin hydrochloride, and dilute to the mark with methanol as a system suitability solution.

[0121] 2) Inject the system suitability solution into the liquid chromat...

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Abstract

The invention discloses a method for separating moxifloxacin hydrochloride and impurities thereof by high performance liquid chromatography. The method comprises the following steps: taking alkyl bonded silica gel or phenyl bonded silica gel as a filler; wherein a mixed solution of a water phase and an organic phase is used as a mobile phase, the water phase is an aqueous solution of fluorinated organic acid, and the organic phase is methanol or acetonitrile; gradient elution is performed; the method has good specificity, linearity and system durability, can be used for detecting nine impurities including impurities A, B, C, D, E, H, I and J and an impurity M introduced in the moxifloxacin hydrochloride synthesis process, and has certain practicability.

Description

technical field [0001] The invention relates to a method for separating moxifloxacin hydrochloride and its impurities by high performance liquid chromatography. Background technique [0002] Moxifloxacin is the latest representative drug of the fourth generation quinolones, its molecular formula C 21 h 24 FN 3 o 4 , the molecular weight is 401.44, and the structural formula is as follows: [0003] [0004] Moxifloxacin hydrochloride is an ultra-broad-spectrum quinolone anti-infective drug developed by Bayer Company of Germany in 1999. This product was first listed in Germany. It was approved by FDA on December 10, 1999. Its trade name is "Avelox". Countries and regions are used clinically. In April 2003, the Moxifloxacin eye drops developed by Alcon was also approved by the FDA. [0005] Moxifloxacin hydrochloride is usually composed of 1-cyclopropyl-6,7-difluoro-8-methoxy-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid and (S,S) -Octahydro-6H-pyrrolo[3,4-b]pyridine i...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02Y02A50/30
Inventor 朱永强杜柳辉宋慧关众仲丽茹杨杨叶海英
Owner JIANGSU CHIA TAI FENGHAI PHARMA
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