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Method for detecting brexpiprazole related substance

Active Publication Date: 2020-11-10
四川弘远药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN105399736A uses octadecylsilane bonded silica gel as a chromatographic column, mobile phase A is sodium octane sulfonate solution, mobile phase B is acetonitrile, detection wavelength is 290nm, flow rate is 1.0ml / min for linear gradient elution, The quinoline dimer can be detected, but the inventor repeated the method in the application to detect ebiprazole and its 6 related substances, only 5 impurities could be detected, and the peaks of the related substances overlapped with the peaks of the drug, This method cannot effectively separate ebiprazole and its related substances
CN107525877A discloses a chromatographic column with octadecylsilane bonded silica gel as filler, phosphate buffer as mobile phase A, mixed solvent of methanol and acetonitrile as mobile phase B, detection wavelength of 225nm, and flow rate of 1.0ml / min, using the gradient elution method to detect ebiprazole and its 6 related substances, but the inventor repeated the application conditions to detect ebiprazole and its 6 related substances, and the separation of related substances could not meet the methodological requirements

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  • Method for detecting brexpiprazole related substance
  • Method for detecting brexpiprazole related substance
  • Method for detecting brexpiprazole related substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0109] Embodiment 1 System suitability experiment

[0110] 1. Instruments and conditions

[0111] Chromatographic column: InertsilODS-3C18 column (4.6×150mm, 3μm)

[0112] Mobile phase: mobile phase A: 0.1% formic acid-acetonitrile solution, mobile phase B: 0.1% formic acid-0.04mol / L ammonium chloride solution

[0113] Flow rate: 1.0ml / min

[0114] Column temperature: 35°C

[0115] Detection wavelength: 254nm

[0116] Carry out gradient elution according to the table below:

[0117]

[0118] 2. Operation steps

[0119] Accurately weigh appropriate amounts of ebiprazole reference substance and impurity BPZ-8, BPZ-9, BPZ-16, BPZ-23, BPZ-20, BPZ-29 reference substance, and diluent [0.02mol / LNa 2 SO 4 -acetonitrile-methanol-glacial acetic acid (56:33:11:1)] was dissolved and quantitatively diluted to make a mixed solution containing about 0.4 mg of ebiprazole and 0.8 μg of BPZ impurity per 1 ml as a system suitability solution. Inject 20 μl into the liquid chromatogra...

Embodiment 2

[0124] Example 2 Ebiprazole bulk drug accelerated test (40°C ± 2°C temperature, 75% ± 5% relative humidity) sample detection

[0125] 1. Instruments and conditions

[0126] Chromatographic column: InertsilODS-3C18 column (4.6×150mm, 3μm)

[0127] Mobile phase: mobile phase A: acetonitrile solution, mobile phase B: 0.04mol / L ammonium chloride solution

[0128] Wavelength: 254nm;

[0129] Flow rate: 1.0ml / min;

[0130] Column temperature: 35°C;

[0131] Injection volume: 20ul;

[0132] The elution gradient is shown in the table below:

[0133]

[0134] 2. Operation method: Accurately weigh about 10 mg of ebiprazole crude drug after the accelerated test, put it in a 25ml measuring bottle, add an appropriate amount of diluent and shake to dissolve, dilute to the mark with diluent to obtain the test solution. Precision measures need testing solution 0.5ml, puts in 100ml measuring bottle, with diluent [0.02mol / LNa 2 SO 4 -acetonitrile-methanol-glacial acetic acid (56:33:11:...

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Abstract

The invention provides a method for detecting a brexpiprazole related substance, and the method adopts a chromatographic column with octadecylsilane chemically bonded silica as a filler, an acetonitrile solution as a mobile phase A and an ammonium chloride solution as a mobile phase B, and adopts gradient elution to determine brexpiprazole and related substances thereof. According to the method, brexpiprazole can be effectively separated from adjacent impurities and various impurities, the separation degree is high, brexpiprazole and related substances thereof can be accurately detected, the problem that brexpiprazole and related substances thereof are difficult to separate and detect is effectively solved, and therefore it is guaranteed that the quality of brexpiprazole is controllable.

Description

technical field [0001] The invention relates to a method for detecting related substances of ebiprazole, which belongs to the field of pharmaceutical analytical chemistry. Background technique [0002] Brexpiprazole (Brexpiprazole) is a dopamine, partial 5-HT1A receptor agonist and 5-HT2A receptor antagonist compound used for the treatment of severe depression and schizophrenia. The chemical name of ebiprazole is 7-(4-(4benzo[b]thiophen-4-ylpiperazin-1-yl)butoxy-1H-quinolin-2-one, molecular formula: C 25 h 27 N 3 o 2 S, molecular weight: 433.57, its chemical structural formula is: [0003] [0004] In the process of compound synthesis, important intermediates and impurities may affect the purity and quality of the drug due to incomplete removal. These known intermediates and impurities and the resulting degradation products are related substances. The research on related substances is one of the key items in drug quality research, which affects the stability and safe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 柯潇张伟
Owner 四川弘远药业有限公司
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