Method for analyzing related substances in avanafil and preparation thereof

A technology for avanafil and related substances, which is applied in the field of drug analysis, can solve the problem that the substance analysis method is not reported in literature, etc., and achieves the effects of strong specificity, high feasibility and simple operation process

Pending Publication Date: 2020-05-29
SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Avanafil and its preparations have not been marketed in China at present, and there are no literature reports on the analysis methods of related substances in its raw materials and preparations, and there are no standards for reference

Method used

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  • Method for analyzing related substances in avanafil and preparation thereof
  • Method for analyzing related substances in avanafil and preparation thereof
  • Method for analyzing related substances in avanafil and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Instrument and chromatographic conditions:

[0038] High performance liquid chromatography: Waters e2695, PDA detector

[0039] Chromatographic column: Waters C8, 4.6mm*250mm, 5μm

[0040] Mobile phase A: 0.02mol / L phosphate buffer, mobile phase B: acetonitrile, gradient elution, the gradient program is as follows:

[0041]

[0042]

[0043] Detection wavelength: 235nm

[0044] Flow rate: 1.0ml / min

[0045] Column temperature: 30°C

[0046] Injection volume: 10μl

[0047] Experimental steps:

[0048] Take appropriate amount of avanafil, starting material 1, starting material 2, intermediate 1, intermediate 2, intermediate 3, impurity 1, impurity 2, impurity 3 and impurity 4, dissolve and dilute with methanol to make 1ml Contains about 0.5mg of avanafil, each 1ml contains about starting material 1, starting material 2, intermediate 1, intermediate 2, intermediate 3, impurity 1, impurity 2, impurity 3 and impurity 4 respectively 15μg, 15μg, 15μg, 15μg, 15μg, ...

Embodiment 2

[0052] Instrument and chromatographic conditions:

[0053] High performance liquid chromatography: Waters e2695, PDA detector

[0054] Chromatographic column: Waters C8, 4.6mm*250mm, 5μm

[0055] Mobile phase A: 0.02mol / L phosphate buffer, mobile phase B: acetonitrile, gradient elution, the gradient program is as follows:

[0056]

[0057] Detection wavelength: 235nm

[0058] Flow rate: 1.0ml / min

[0059] Column temperature: 30°C

[0060] Injection volume: 10μl

[0061] Experimental steps:

[0062] System suitability solution: take appropriate amount of avanafil, impurity 1, impurity 2 and impurity 3, and make about 50 μg, 0.5 μg, 0.5 μg and 0.5 μg solution, as a system suitability solution.

[0063]Take an appropriate amount of avanafil, accurately weighed, dissolve and dilute to make a solution containing about 0.5-1 mg of avanafil per 1 ml, as the test solution. Precisely measure an appropriate amount of the test solution, dilute it into a solution containing abo...

Embodiment 3

[0069] Instrument and chromatographic conditions:

[0070] High performance liquid chromatography: Waters e2695, PDA detector

[0071] Chromatographic column: Waters C8, 4.6mm*250mm, 5μm

[0072] Mobile phase A: 0.02mol / L phosphate buffer, mobile phase B: acetonitrile, gradient elution, the gradient program is as follows:

[0073]

[0074] Detection wavelength: 235nm

[0075] Flow rate: 1.0ml / min

[0076] Column temperature: 30°C

[0077] Injection volume: 10μl

[0078] Experimental steps:

[0079] Take an appropriate amount of avanafil, impurity 1, impurity 2 and impurity 3 to make a solution containing 50 μg, 0.5 μg, 0.5 μg and 0.5 μg of avanafil, impurity 1, impurity 2 and impurity 3 respectively per 1 ml, As a system suitability solution. Precisely measure 10 μl of the system suitability solution, inject it into the high-performance liquid chromatograph, record the chromatogram, and see the results in Figure 5 .

[0080] result:

[0081] Figure 5 Among them...

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Abstract

The invention discloses a method for determining related substances in avanafil and a preparation thereof. The method is characterized in that a chromatographic column taking octyl bonded silica gel as a filler is adopted, phosphate buffer solution-acetonitrile is taken as a mobile phase, gradient elution is performed, and a diode array detector or an ultraviolet detector is adopted. The analysismethod is advantaged in that the avanafil and nine process impurities thereof can be separated, degraded impurities can further be effectively separated, and a blank solvent does not interfere with measurement, common instruments, equipment and the chromatographic column are used, the mobile phase is simple and easy to obtain, operation is simple and convenient, sensitivity is high, and the quality of avanafil and the preparation thereof can be better controlled.

Description

technical field [0001] The invention relates to a method for detecting related substances of avanafil and its preparation, belonging to the technical field of drug analysis. Background technique [0002] Avanafil (Avanafil), the chemical name is 4-[(3-chloro-4-methoxybenzyl)amino]-2-[2-(hydroxymethyl)-1-pyrrolidinyl]-N- (2-Pyrimidinylmethyl)-5-pyrimidinecarboxamide, CAS No. 330784-47-9. The chemical structural formula is as follows: [0003] [0004] Avanafil is a drug developed by Vivus Corporation of the United States authorized by Mitsubishi Tanabe Pharmaceutical Co., Ltd. of Japan for the treatment of male erectile dysfunction (ED). It was approved for marketing by the U.S. FDA on April 27, 2012. Specifications 50mg, 100mg and 200mg). The drug is an oral, fast-acting, highly selective phosphodiesterase-5 (PDE-5) inhibitor. [0005] Avanafil may introduce related substances such as starting materials, intermediates, and by-products during the synthesis process, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/74
CPCG01N30/02G01N30/06G01N30/54G01N30/74G01N2030/027G01N2030/062
Inventor 王帆刘延新杨琪李帅王业强刘敏廉贞霞
Owner SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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