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A kind of detection method of 3-dimethylamino ethyl acrylate in moxifloxacin hydrochloride

A technology of ethyl dimethylamino acrylate and moxifloxacin hydrochloride is applied in measuring devices, resisting vector-borne diseases, instruments, etc., and can solve the problems of being unsuitable for analyzing biochemical samples under pressure, polluting the environment, and high cost, and achieving The effect of low cost, high resolution and high accuracy

Active Publication Date: 2022-07-08
珠海润都制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the prior art uses HPLC to measure related impurities in moxifloxacin hydrochloride. HPLC detection has the disadvantages of using a variety of solvents as mobile phase, high cost, and polluting the environment, which is not suitable for analysis. Biochemical samples with biological activity that are decomposed under pressure and denatured. In order to solve the above problems, the invention provides a gas chromatography-mass spectrometry method to detect the content of 3-dimethylaminoethyl acrylate in moxifloxacin hydrochloride. Gas chromatography-mass spectrometry The combined method is easy to operate and takes a short time. It does not use a large amount of solvent for column elution, which saves costs and does not pollute the environment.

Method used

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  • A kind of detection method of 3-dimethylamino ethyl acrylate in moxifloxacin hydrochloride
  • A kind of detection method of 3-dimethylamino ethyl acrylate in moxifloxacin hydrochloride
  • A kind of detection method of 3-dimethylamino ethyl acrylate in moxifloxacin hydrochloride

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Experimental program
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Effect test

Embodiment 1

[0037] (1) Experimental materials and instrument conditions

[0038] Experimental materials: methanol, manufacturer: Merck Co., Ltd.; sodium hydroxide, manufacturer: Tianjin Damao Chemical Reagent Factory; 3-dimethylaminoethyl acrylate, manufacturer: Zhuhai Rundu Pharmaceutical Co., Ltd.; Moxifloxacin hydrochloride, manufacturer: Zhuhai Rundu Pharmaceutical Co., Ltd.; ultrapure water, manufacturer: Zhuhai Rundu Pharmaceutical Co., Ltd.

[0039] Instrument: gas chromatography mass spectrometer: 7890B+7000D; electronic analytical balance: XSE205DU; chromatographic column: DB-1701, 30m x 0.25mm, 1.00μm.

[0040]Detection method: inject blank solution, reference solution and test solution into gas chromatography-mass spectrometer respectively, record the chromatogram, and the chromatographic conditions are as follows: (14%-cyanopropyl-phenyl) methyl polysiloxane fixed solution ( Such as: Agilent DB-1701, 30m x 0.25mm, 1.00μm, or a chromatographic column with equivalent performanc...

Embodiment 2

[0055] Example 2 System suitability test of the detection method of the present invention

[0056] The system applicability is achieved by the RSD of 3-dimethylaminoethyl acrylate peak area in 5 needles of the reference solution. It is required that the RSD of 5 needles of the reference solution based on the peak area of ​​3-dimethylaminoethyl acrylate should not be greater than 10.0 %. Prepare blank solution and reference solution as described in Example 1. Under the chromatographic conditions described in Example 1, add 1 injection of blank solution and 5 injections of reference solution, and record the spectrum, as shown in figure 1 and figure 2 , according to the formula, the conversion results are shown in the following table:

[0057]

Embodiment 3

[0058] Example 3 Specificity test of the detection method of the present invention

[0059] Specificity is determined by determining whether the blank solution interferes with the detection of 3-dimethylaminoethyl acrylate; before and after sample addition, the resolution and recovery of 3-dimethylaminoethyl acrylate in the selective solution rate achieved. It is required that the blank solution should not interfere with the detection of 3-dimethylaminoethyl acrylate; the separation degree of 3-dimethylaminoethyl acrylate and adjacent peaks in the selective solution should not be less than 1.5; - The recovery of ethyl dimethylaminoacrylate should be between 70.0% and 130.0%. Prepare blank solution, reference solution, moxifloxacin hydrochloride test solution (positioning solution) and moxifloxacin hydrochloride selective solution as described in Example 1. After the system is balanced, add 1 injection of blank solution, 3 injections of reference solution, 1 injection of moxi...

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Abstract

3-Dimethylamino ethyl acrylate is the starting material for the synthesis of moxifloxacin hydrochloride 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxoquinoline- The starting material of ethyl 3-carboxylate has a genotoxic warning structure, so the researchers of our company independently developed a method for the detection of 3-dimethylaminoethyl acrylate residues in moxifloxacin hydrochloride. The detection of 3-dimethylaminoethyl acrylate in moxifloxacin hydrochloride is realized by GCMS / MS detection. It has been verified that the detection method has high system applicability, and at the same time, the specificity, precision, limit of quantification are improved. and detection limit, linearity and range, accuracy and solution stability are all within the standard.

Description

technical field [0001] The invention belongs to the field of pharmaceutical analytical chemistry, in particular to a method for detecting ethyl 3-dimethylaminoacrylate in moxifloxacin hydrochloride by GCMS / MS method. Background technique [0002] Moxifloxacin Hydrochloride (CAS No.: 186826-86-8) is a fluoroquinolone antibiotic, the English name is: Moxifloxacin Hydrochloride, and the Chinese name of the compound 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 Salt. Moxifloxacin hydrochloride is a fourth-generation extended-spectrum quinolone drug developed by Bayer in Germany in 1999. It is the best in terms of pharmacokinetics, safety, antibacterial activity, and antibacterial spectrum and application. It has broad-spectrum antibacterial activity against Gram-positive, Gram-negative, anaerobic, acid-fast and atypical microorganisms such as Mycoplasma, Chlamydia and Legionella, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/047Y02A50/30
Inventor 李达胜汤伟彬籍利军郭锐蔡强王晴晴
Owner 珠海润都制药股份有限公司