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Method for separating and determining two genotoxic impurities in flurbiprofen axetil

A flurbiprofen axetil, genotoxic technology, applied in the field of analytical chemistry, can solve the problems of inability to achieve detection sensitivity, method repeatability and precision, difficult separation and determination, impurity separation and detection, etc., achieves good peak shape, avoids Solvent peak interference, low cost effect

Pending Publication Date: 2021-06-22
YAOPHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] It should be noted that, in the methodological research process, the inventors found that it is difficult to separate vinyl acetate and benzene well by using prior art and conventional GC methods
Vinyl acetate and benzene belong to different structural classes of compounds, but it is really difficult to separate them for determination
For example, the simultaneous determination of three residual monomers in acrylate pressure-sensitive adhesives established by Hu Jing et al. Body - HPLC method for the content of vinyl acetate, propylene vinyl ester and n-butyl acrylate, the mobile phase is acetonitrile-water (40:60), isocratic or gradient can not be the two genes in flurbiprofen axetil Effective separation of toxic impurities
Another example is that the conventional analysis methods of these two compounds, vinyl acetate and benzene, are both GC-FID methods. However, it is difficult to separate and detect these two impurities by using conventional GC-FID assay methods, which cannot achieve good detection sensitivity and method. Repeatability and Precision

Method used

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  • Method for separating and determining two genotoxic impurities in flurbiprofen axetil
  • Method for separating and determining two genotoxic impurities in flurbiprofen axetil
  • Method for separating and determining two genotoxic impurities in flurbiprofen axetil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Instruments and Conditions

[0052] Instrument: Agilent 1200 HPLC

[0053] Chromatographic column: SB-C18, 4.6×150mm, 3.5μm;

[0054] Injection volume: 10μl;

[0055] Flow rate: 1.0ml / min;

[0056] Column temperature: 30°C;

[0057] Detection wavelength: 205nm;

[0058] Diluent: Acetonitrile

[0059] Mobile phase A: 0.1% phosphoric acid in water; mobile phase B: acetonitrile

[0060] The gradient is shown in Table 3 below:

[0061] Table 3 Elution gradient

[0062] .

[0063] Experimental steps:

[0064] Vinyl acetate stock solution: Weigh about 385mg of vinyl acetate, weigh it accurately, put it in a 20ml measuring bottle, dissolve it with acetonitrile and dilute to the mark, shake well; accurately measure 1ml of the above solution, put it in a 50ml measuring bottle, and dilute it with acetonitrile To the scale, shake well, that is.

[0065] 1,1-Ethylene glycol diacetate stock solution: Accurately weigh about 750mg of 1,1-ethylene glycol diacetate, put it ...

Embodiment 2

[0076] Embodiment 2 durability experiment

[0077] Vinyl acetate stock solution: Weigh about 385mg of vinyl acetate, weigh it accurately, put it in a 20ml measuring bottle, dissolve it with acetonitrile and dilute to the mark, shake well; accurately measure 1ml of the above solution, put it in a 50ml measuring bottle, and dilute it with acetonitrile To the scale, shake well, that is.

[0078] 1,1-Ethylene glycol diacetate stock solution: Accurately weigh about 750mg of 1,1-ethylene glycol diacetate, put it in a 20ml measuring bottle, dissolve it with acetonitrile and dilute to the mark, shake well to obtain .

[0079] Benzene stock solution: Weigh about 200mg of benzene, weigh it accurately, put it in a 20ml measuring bottle, dissolve it with acetonitrile and dilute to the mark, and shake well; accurately measure 1ml of the above solution, put it in a 100ml measuring bottle, dilute it to the mark with acetonitrile, shake Uniform, that is.

[0080] Reference substance stock ...

Embodiment 3

[0089] Embodiment 3 solution stability experiment

[0090] Vinyl acetate stock solution: Weigh about 385mg of vinyl acetate, weigh it accurately, put it in a 20ml measuring bottle, dissolve it with acetonitrile and dilute to the mark, shake well; accurately measure 1ml of the above solution, put it in a 50ml measuring bottle, and dilute it with acetonitrile To the scale, shake well, that is.

[0091] 1,1-Ethylene glycol diacetate stock solution: Accurately weigh about 750mg of 1,1-ethylene glycol diacetate, put it in a 20ml measuring bottle, dissolve it with acetonitrile and dilute to the mark, shake well to obtain .

[0092] Benzene stock solution: Weigh about 200mg of benzene, weigh it accurately, put it in a 20ml measuring bottle, dissolve it with acetonitrile and dilute to the mark, and shake well; accurately measure 1ml of the above solution, put it in a 100ml measuring bottle, dilute it to the mark with acetonitrile, shake Uniform, that is.

[0093] Reference substanc...

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Abstract

The invention discloses a method for separating and determining genotoxic impurities vinyl acetate and benzene in flurbiprofen axetil. According to the method, liquid chromatography is adopted, an octadecyl silica gel chromatographic column is used as a stationary phase, acetonitrile-phosphoric acid-water is used as a mobile phase, vinyl acetate and benzene can be effectively separated, all impurities are good in peak shape, the column efficiency is high, specificity is good, and the quality of flurbiprofen axetil is well controlled.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to an analysis method for two genotoxic impurities in flurbiprofen axetil. Background technique [0002] Flurbiprofen axetil (hereinafter referred to as "FLUR") is a prodrug of flurbiprofen, which can inhibit cyclooxygenase (COX-1 and COX-2), reduce the synthesis of prostaglandins (PGs) physiologically, Achieve antipyretic, analgesic, anti-inflammatory and other effects. [0003] According to ICH M7, the present inventors conducted a genotoxic impurity study on flurbiprofen axetil. It was found that flurbiprofen axetil has many types of related substances, and the number of impurities is quite large and complicated. The specific research contents are as follows: [0004] First, the genotoxic impurity profile analysis of flurbiprofen axetil is shown in Table 1 below. Divided into aromatic amines, nitroso compounds, Michael addition reaction acceptors, aldehydes, alk...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/54
CPCG01N30/02G01N30/74G01N30/34G01N30/54G01N30/36G01N30/06G01N2030/027
Inventor 李雪郭云程刘强陈佳江钟家庆
Owner YAOPHARMA CO LTD
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