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Method for analyzing latent genotoxic impurities of lamotrigine

A technique for detecting lamotrigine and a detection method, which is applied in the field of chemical analysis, and can solve problems such as insufficient detection sensitivity and inability to accurately quantify impurities

Pending Publication Date: 2021-05-18
ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Using GC-MS or LC-MS method to directly detect the limit of 2,3-dichlorobenzoylnitrile within 2ppm, it is found that due to insufficient detection sensitivity, or decomposition or polymerization at high temperature, it cannot be within 2ppm Accurate quantification of this impurity within limits

Method used

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  • Method for analyzing latent genotoxic impurities of lamotrigine
  • Method for analyzing latent genotoxic impurities of lamotrigine
  • Method for analyzing latent genotoxic impurities of lamotrigine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044]Chromatographic conditions

[0045]Instrument: High Performance Liquid Chromatograph Equipped with Mass Spectrometry Detector

[0046]Column: Waters Xbridge Shield, RP18, 150 × 4.6mm, 3.5μm

[0047]Mobile phase a: 0.1% formic acid aqueous solution

[0048]Mobile phase B: acetonitrile

[0049]Flow speed: 1.0ml / min

[0050]Inject volume: 5μL

[0051]Column temperature: 25 ° C

[0052]Running time: 30min

[0053] Time / min Mobile phase a / % Mobile phase B / % 08515 38515 152080 222080 22.18515 308515

[0054]The mass spectrometry detector parameters are as follows:

[0055]

[0056]

[0057]Diluent: dichloromethane

[0058]Derived reagent solution: It is weighed in 25 mg of waterless copiperazine to 25 mL volumetric flask, followed by dilution to the scale with dilution. (Derived reagent concentration: 1.0mg / ml)

[0059]White solution: Accurately remove 0.5 ml of dilution, derivatized reagent 0.5 ml to 1.5 ml into spots, mix well, sealed the cap, 2 hours under 40 ° C, and then removed to room temperature.

[0060]2,3-di...

Embodiment 2

[0067]Chromatographic conditions

[0068]Instrument: High Performance Liquid Chromatograph Equipped with Mass Spectrometry Detector

[0069]Column: ACE 3C18, 150mm * 4.6mm; 3.0μm

[0070]Mobile phase a: 0.1% formic acid aqueous solution

[0071]Mobile phase B: acetonitrile

[0072]Flow speed: 1.0ml / min

[0073]Inject volume: 5μL

[0074]Column temperature: 35 ° C

[0075]Running time: 40min

[0076] Time / min Mobile phase a / % Mobile phase B / % 08020 108020 252080 352080 35.18020 408020

[0077]The mass spectrometry detector parameters are as follows:

[0078]

[0079]Diluent: dichloromethane

[0080]Derived reagent solution: It is weighed in 25 mg N-methylpiperazine to 25 mL volumetric flask, followed by dilution to the scale with a dilution. (Derived reagent concentration: 1.0mg / ml)

[0081]Blank solution, 2,3-dichlorobenzyl nitrile stock solution (2,3-dichlorobenzyl nitrile concentration: 42.8 ng / ml), sensitivity solution (2,3-dichloride) concentration: 6.4 Ng / mL), standard solution (2,3-dichlorodyl) concentr...

Embodiment 3

[0084]Chromatographic conditions

[0085]Instrument: High Performance Liquid Chromatograph Equipped with Mass Spectrometry Detector

[0086]Column: ACE 3C18, 150mm * 4.6mm; 3.0μm

[0087]Mobile phase a: 0.1% aqueous trifluoroacetic acid solution

[0088]Mobile phase B: methanol

[0089]Test wavelength: 210nm

[0090]Flow speed: 1.0ml / min

[0091]Inject volume: 5μL

[0092]Column temperature: 35 ° C

[0093]Running time: 30min

[0094] Time / min Mobile phase a / % Mobile phase B / % 08020 155545 182080 212080 258020 308020

[0095]The mass spectrometry detector parameters are as follows:

[0096]

[0097]

[0098]Diluent: dichloromethane

[0099]Derived reagent solution: It is weighed in 25 mg of waterless copiperazine to 25 mL volumetric flask, followed by dilution to the scale with dilution. (Derived reagent concentration: 1.0mg / ml)

[0100]Blank solution, 2,3-dichlorobenzyl nitrile stock solution (2,3-dichlorobenzyl nitrile concentration: 42.8 ng / ml), sensitivity solution (2,3-dichloride) concentration: 6.4 Ng / ml), st...

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Abstract

The invention provides a method for detecting the content of a trace potential genotoxic impurity 2, 3-dichlorobenzoyl nitrile (I) in a lamotrigine finished product and an intermediate thereof by an LC-MS pre-column derivatization method, and the method provided by the invention is strong in specificity, good in durability, low in sensitivity and wide in detection linear range.

Description

Technical field[0001]The present invention relates to the field of chemical analysis, and more particularly to a method of analyzing a potential genetic toxic impurity of straamazine.Background technique[0002]Lamotrigine is mainly used for the treatment of partial epilepsy, especially for refractory partial epilepsy that cannot be controlled by other monoes or combined drugs, and its effect is safe and effective. There are more than 50% of patients with abortion, or non-typical vaporization, and muscle quotation can be controlled. At the same time, Lamo triazine is also suitable as auxiliary drug for the treatment of Lennox-Gastant syndrome in refractory epilepsy, as well as secondary and idiopathic whole body, and its structural formula is as follows:[0003][0004]In the synthesis process of Ramozazine, there are 1 active intermediate compound 2,3-dichlorobenzyl (I) containing a benzyl nitrile group, which belongs to a potential warning structure, which may belong to Potential geneti...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 林金生徐薇梁俊鹤陆彩虹叶丹凤陈文斌朱文泉李敏
Owner ZHEJIANG HUAHAI PHARMACEUTICAL CO LTD
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