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Analysis method of genotoxic impurity in moxifloxacin hydrochloride starting material

A technology of moxifloxacin hydrochloride and genotoxicity, which is applied in the directions of material separation, analysis materials, instruments, etc., can solve the problems such as no published reports on the determination method of genotoxic impurities, and achieves low detection cost, low toxicity, and improved work efficiency. The effect of efficiency

Active Publication Date: 2022-02-18
SHANDONG INST FOR FOOD & DRUG CONTROL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no published report on the determination method of genotoxic impurities in the starting material of moxifloxacin hydrochloride

Method used

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  • Analysis method of genotoxic impurity in moxifloxacin hydrochloride starting material
  • Analysis method of genotoxic impurity in moxifloxacin hydrochloride starting material
  • Analysis method of genotoxic impurity in moxifloxacin hydrochloride starting material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The investigation of embodiment 1 derivatization temperature

[0048] 1. Sample pretreatment

[0049] The test product (100% limit spiked) solution: take moxifloxacin hydrochloride starting material 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo -1 g of ethyl 3-quinolinecarboxylate, accurately weighed, put in a 50 ml measuring bottle, and accurately add the stock solution of impurity 2,4,5-trifluoro-3-methoxybenzoyl chloride (1.68 μg / ml) 2 ml, mix well, then precisely add 10ml of absolute ethanol, mix well. Prepare 3 copies in the same way, place them at 25°C, 30°C, and 35°C for 30 minutes, dissolve and dilute to the mark with dichloromethane, shake well, and obtain.

[0050] 2. Chromatographic conditions

[0051] Instrument: gas chromatography-mass spectrometry; chromatographic column: TG-5 ms (30 m × 0.25 mm × 0.25 μm); temperature program, the initial temperature is 100 ° C, maintained for 5 minutes, and the temperature is raised to 150 ° C at a rate of 1...

Embodiment 2

[0056] The investigation of embodiment 2 derivation time

[0057] 1. Sample pretreatment

[0058] The test product (100% limit spiked) solution: take moxifloxacin hydrochloride starting material 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo -1 g of ethyl 3-quinolinecarboxylate, accurately weighed, put in a 50 ml measuring bottle, and accurately add the stock solution of impurity 2,4,5-trifluoro-3-methoxybenzoyl chloride (1.68 μg / ml) 2 ml, mix well, then precisely add 10ml of absolute ethanol, mix well. Prepare 3 parts in the same way, place them in a water bath at 30°C for 5 minutes, 10 minutes, and 15 minutes respectively, dissolve and dilute to the mark with dichloromethane, shake well, and obtain.

[0059] Determine according to the chromatographic conditions set in Example 1.

[0060] 2. Results and conclusions

[0061] Table 2 Screening results of derivation time

[0062] Derivation time 5 minutes 10 minutes 15 minutes Derivative peak a...

Embodiment 3

[0064] Example 3 Investigation of the volume-to-mass ratio of the derivatization reagent to the moxifloxacin hydrochloride starting material

[0065] 1. Sample pretreatment

[0066] The test product (100% limit spiked) solution: take moxifloxacin hydrochloride starting material 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo - 1g of ethyl 3-quinolinecarboxylate, accurately weighed, put in a 50ml measuring bottle, and accurately add the stock solution of impurity 2,4,5-trifluoro-3-methoxybenzoyl chloride (1.68 μg / ml) 2ml, mix well, prepare 3 parts in the same way, then add 2ml, 5ml, 10ml of absolute ethanol respectively, and mix well. Heat in a water bath at 30°C for 10 minutes, dissolve and dilute to the mark with dichloromethane, shake well, and obtain.

[0067] The determination was carried out according to the chromatographic conditions determined in Example 1.

[0068] 2. Results and conclusions

[0069] Table 3 Screening results of derivatization reagent to sub...

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Abstract

The invention belongs to the technical field of drug analysis, in particular to a moxifloxacin hydrochloride starting material 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo- Quantitative analysis method for potential genotoxic impurities in ethyl 3‑quinolinecarboxylate. The structure types of potential genotoxic impurities include acid halides and unsaturated ketones. The present invention adopts absolute ethanol and 2,4,5-trifluoro-3-methoxybenzoyl chloride to carry out derivatization reaction to generate 2,4,5-trifluoro-3-methoxybenzoic acid ethyl ester, adopts ( 5% phenyl)-methyl polysiloxane is a fixed relative derivative 2,4,5-trifluoro-3-methoxy ethyl benzoate and impurity 3-(N,N-dimethylamino)acrylic acid Ethyl esters were separated and detected by mass spectrometry. The method can not only realize the effective separation of potential genotoxic impurities in the starting raw materials, but also can quantitatively detect the genotoxic impurities. The operation is simple and fast, with strong specificity, high sensitivity, accuracy and reliability. It is of great significance to the quality control and drug safety of preparations.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a derivatization gas chromatography-mass spectrometry analysis method for potential genotoxic impurities, which is used for moxifloxacin hydrochloride starting material 1-cyclopropyl-6,7-difluoro-1 , Potential genotoxic impurities 2,4,5-trifluoro-3-methoxybenzoyl chloride and 3- Analysis and detection of (N,N-dimethylamino) ethyl acrylate. Background technique [0002] Moxifloxacin hydrochloride, the 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-quinolinecarboxylate hydrochloride, molecular formula C 21 h 24 FN 3 o 4 HCl, its structural formula is: [0003] [0004] Moxifloxacin hydrochloride is an 8-methoxyfluoroquinolone antibacterial drug with broad-spectrum and antibacterial activity, mainly used in the treatment of upper and lower respiratory tract infections (such as: acute sinusitis, acute e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/067
Inventor 文松松徐玉文牛冲郭常川张雷刘琦郑静向宇杨书娟
Owner SHANDONG INST FOR FOOD & DRUG CONTROL
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