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Method for separation and determination of brexpiprazole and impurities thereof by liquid chromatography

A technology of ebiprazole and liquid chromatography, which is applied in the field of analytical chemistry, can solve the problems affecting the quality control of ebiprazole and its preparations, and the difficulty in achieving effective separation of ebiprazole, and achieve enhanced retention, high column efficiency, and increased efficiency. The effect of large resolution

Active Publication Date: 2017-12-29
CHONGQING PHARMA RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventors found that it is difficult to effectively separate ebiprazole from impurities and impurities from impurities using the method of CN105399736 and conventional detection methods, which will affect the quality control of ebiprazole and its preparations

Method used

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  • Method for separation and determination of brexpiprazole and impurities thereof by liquid chromatography
  • Method for separation and determination of brexpiprazole and impurities thereof by liquid chromatography
  • Method for separation and determination of brexpiprazole and impurities thereof by liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Instruments and Conditions

[0055] Agilent 1200 liquid chromatograph and chemical workstation; automatic sample injection; Agilent Eclipse Plus C18 column (5μm, 250×4.6mm) as separation column; UV detector wavelength: 225nm; mobile phase: 0.01mol / L phosphoric acid Potassium dihydrogen solution (adjust the pH value to 3.0 with phosphoric acid solution) as mobile phase A, methanol-acetonitrile (15:85) as mobile phase B, gradient elution; 0 minutes, mobile phase A is 90%, mobile phase B 10%; from 0 minutes to 5 minutes, the mobile phase A is 90%, and the mobile phase B is 10%; from 5 minutes to 35 minutes, the mobile phase A linearly decreases to 20%, and the mobile phase B linearly increases to 80%; 35 minutes Up to 45 minutes, the mobile phase A is 20%, and the mobile phase B is 80%; both mobile phase A and mobile phase B are volume percentages. The column temperature is 25°C, the flow rate is 1.0ml / min, and the injection volume is 20μl.

[0056] Operation method:

...

Embodiment 3

[0062] Determination of impurities in ebiprazole bulk drug.

[0063] Take about 10mg of ebiprazole, weigh it accurately, put it in a 50ml measuring bottle, add a diluent (methanol:water=80:20) and sonicate to dissolve and dilute to the mark, shake well, and use it as the test solution; Weigh 10mg of ebiprazole reference substance, put it in a 50ml measuring bottle, add diluent (methanol: water = 80:20) and sonicate to dissolve and dilute to the mark, shake well, accurately measure 1ml, put it in a 100ml measuring bottle, and use Diluent is diluted to scale, shakes up, as contrast solution; Carry out liquid chromatography analysis according to the chromatographic condition of embodiment 1, if impurity peak (except solvent peak) is arranged in the chromatogram of need testing solution, known impurity is multiplied by The peak area after the correction factor shall not be greater than 0.15%, calculated by the external standard method of the main component, and shall not be greate...

Embodiment 4

[0065] Determination of impurities in ebiprazole tablets by liquid chromatography.

[0066] Take an appropriate amount of this product (approximately equivalent to ebiprazole 10mg), put it in a 50ml measuring bottle, add a diluent (methanol: water = 80:20) and ultrasonically treat it to dissolve and dilute to the mark, shake well, and use it as the test solution ; In addition, accurately weigh 10 mg of ebiprazole reference substance, put it in a 50 ml measuring bottle, add diluent (methanol: water = 80: 20) and sonicate to dissolve and dilute to the scale, shake well, and accurately measure 1 ml and place it in 100 ml bottle, dilute to the mark with diluent, shake well, and use it as a contrast solution; in addition, take an appropriate amount of blank adjuvant according to the prescription ratio, and prepare the blank adjuvant test solution according to the same method as the test solution; carry out liquid phase according to the chromatographic conditions of Example 1 For ch...

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Abstract

The invention discloses a method for separation and determination of brexpiprazole or preparations and impurities thereof by liquid chromatography. According to the method, a chromatographic column takes octadecylsilane bonded silica gel as a filler, a buffer solution is used as a mobile phase A, a mixed solvent of methanol and acetonitrile is used as a mobile phase B, the mobile phases adopt a gradient elution method, and the brexpiprazole and preparation impurities are determined. The method can effectively separate and determine the brexpiprazole with known impurities and unknown impurities. The method has the advantages of high specificity, high accuracy and easy operation, and can effectively control the quality of the pipiprazole and the preparations thereof.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for separating and measuring ebiprazole and its impurities by liquid chromatography. Background technique [0002] Brexpiprazole (Brexpiprazole) is used for the treatment of severe depression and schizophrenia. Its molecular formula is C25H27N3O2S, and its structural formula is shown in the following formula (a) compound. [0003] The chemical name of ebiprazole is: 7-(4-(4-(benzo[b]thiophen-4-yl-piperazin-1-yl)butoxy)-1H-quinolin-2-one. In the process of synthesizing this compound, there are several important intermediates and unknown impurities that may affect the purity and quality of the drug due to incomplete removal. These known intermediates, unknown impurities and the resulting degradation products are the quality control of the drug Commonly referred to as related substances (i.e. impurities). There are eight known impurities that are mainly controlled for t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/74G01N30/06
CPCG01N30/06G01N30/74
Inventor 代广会陈志锋万娟张道林
Owner CHONGQING PHARMA RES INST
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