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Method for separating and determining compound A and imidazole in amisulpride by gas chromatography

A technology of gas chromatography and amisulpride, which is applied in the field of separation and determination of compound A and imidazole in the final product of amisulpride by gas chromatography, can solve the problems affecting the purity and quality of drugs, incomplete removal of harmful impurities, etc., and achieve The effect of reducing the yield

Pending Publication Date: 2021-10-19
BEIJING VENTUREPHARM BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Incomplete removal of harmful impurities in amisulpride will affect the purity and quality of the drug

Method used

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  • Method for separating and determining compound A and imidazole in amisulpride by gas chromatography
  • Method for separating and determining compound A and imidazole in amisulpride by gas chromatography
  • Method for separating and determining compound A and imidazole in amisulpride by gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Instruments and Conditions

[0041] Chromatograph: Agilent 7890A gas chromatograph;

[0042] Detector: hydrogen flame ionization detector;

[0043] Chromatographic column: CAM capillary column (Agilent, 30m´0.32mm, 0.5μm);

[0044] Column temperature: initial temperature 70°C, to 110°C with a temperature rise rate of 5°C per minute, to 180°C with a temperature rise rate of 30°C per minute, constant temperature for 20min;

[0045] Injection port temperature: 220°C;

[0046] Detector temperature: 300°C;

[0047] Carrier gas (nitrogen) flow rate: 1.5mL / min;

[0048] Split ratio: 50:1;

[0049] Injection volume: 2μL

[0050] Experimental procedure

[0051] Take 10mg~20mg of the final product of amisulpride, dissolve it with a solvent, and prepare a test solution containing 10~20mg of amisulpride per 1mL; take an appropriate amount of compound A and imidazole, dissolve it with a solvent, and prepare Prepare a reference substance solution containing 0.01~0.0.02mg of c...

Embodiment 2

[0053] Instruments and Conditions

[0054] Chromatographic column: CAM capillary column (Agilent, 30m´0.32mm, 0.5μm);

[0055] Column temperature: initial temperature 70°C, to 110°C with a temperature rise rate of 5°C per minute, to 180°C with a temperature rise rate of 30°C per minute, constant temperature for 20min;

[0056] Inlet temperature: 225°C;

[0057] Detector temperature: 300°C;

[0058] Carrier gas (nitrogen) flow rate: 1.5mL / min;

[0059] Split ratio: 50:1;

[0060] Injection volume: 2μL

[0061] Experimental procedure

[0062]Take an appropriate amount of compound A and imidazole, dissolve them in a solvent, and prepare a reference solution containing 0.01~0.0.02mg of compound A and 0.01~0.0.02mg of imidazole per 1mL; take another 10mg~20mg of the final product of amisulpride, add Dissolve 1ml of the reference substance solution in a solvent, shake well, and prepare a system suitability solution containing 10mg~20mg of amisulpride per 1mL. Analyze accordin...

Embodiment 3

[0064] Instruments and Conditions

[0065] Chromatographic column: CAM capillary column (Agilent, 30m´0.32mm, 0.5μm);

[0066] Column temperature: initial temperature 65°C, constant temperature for 10min, to 140°C at a heating rate of 20°C per minute, constant temperature for 5min, to 180°C at a heating rate of 20°C per minute, constant temperature for 20min;

[0067] Injection port temperature: 220°C;

[0068] Detector temperature: 300°C;

[0069] Carrier gas (nitrogen) flow rate: 1.0mL / min;

[0070] Split ratio: 20:1;

[0071] Injection volume: 1μL

[0072] Experimental procedure

[0073] Take an appropriate amount of compound A and imidazole, dissolve them in a solvent, and prepare a reference solution containing 0.01~0.0.02mg of compound A and 0.01~0.0.02mg of imidazole per 1mL; take another 10mg~20mg of the final product of amisulpride, add Dissolve 1ml of the reference substance solution in a solvent, shake well, and prepare a system suitability solution containing...

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Abstract

The invention belongs to the field of analytical chemistry, and discloses a method for separating and determining a compound A[(2RS)-1-ethyl pyrrolidinone-2-yl-methylamine] and imidazole in an amisulpride final product {4-amino-N-[[(2RS)1-ethyl pyrrolidinone-2-yl] methyl]-5-(ethyl sulfonyl)-2-methoxybenzamide} by using a gas chromatographic method. According to the method, a capillary chromatographic column filled with polyethylene glycol and a hydrogen flame ionization detector are adopted, and the content of impurities A[(2RS)-1-ethyl pyrrolidone-2-yl-methylamine] and imidazole in a final product of amisulpride can be quantitatively determined, so that the purity of reactants in the process of synthesizing amisulpride is effectively controlled, side reactions and impurities are reduced, and the product yield is improved. The method is high in specificity, high in accuracy and simple and convenient to operate.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring compound A and imidazole in the final product of amisulpride by gas chromatography. Background technique [0002] Amisulpride is an aniline substitute neuroleptic, which selectively binds to the D2 and D3 dopaminergic receptors of the limbic system, and is mainly used for treating positive symptoms (such as delirium, hallucinations, cognitive impairment) and / or negative symptoms (such as Responsiveness, apathy, and social withdrawal), acute or chronic schizophrenia, including schizophrenia characterized by negative symptoms. The chemical name of amisulpride is 4-amino-N-[[(2RS)1-ethylpyrrolidin-2-yl]methyl]-5-(ethylsulfonyl)-2-methoxybenzamide , the molecular formula is C 17 h 27 N 3 o 4 S, the structural formula is: [0003] [0004] In the process of synthesizing amisulpride, some materials will be used, and these ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02C07D207/09C07D233/58
CPCG01N30/02C07D207/09C07D233/58C07B2200/07
Inventor 丁欣刘秋叶
Owner BEIJING VENTUREPHARM BIOTECH
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