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A method for separating and detecting ambrisentan and its related substances

A technology related to substances and acetonitrile, which is applied in the field of drug analysis, can solve the problems affecting the precision and accuracy of sample quantitative analysis results, high requirements for chromatographic instruments, and reduced signal-to-noise ratio, so as to achieve accurate and reliable analysis results and a stable separation baseline , the effect of low instrument requirements

Active Publication Date: 2016-12-28
TIANJIN INSTITUTE OF PHARMA RESEARCH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] All in all, the analysis methods of ambrisentan and its related substances in the existing reports all adopt the gradient elution high-performance liquid phase method. The signal-to-noise ratio of the collected signal is reduced, which affects the precision and accuracy of the sample quantitative analysis results

Method used

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  • A method for separating and detecting ambrisentan and its related substances

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Experimental program
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Effect test

Embodiment 1

[0021] Containing ambrisentan, benzophenone, 2-hydroxy-3-methoxy-3,3-diphenylpropionic acid (SRS1), (S)-1-(4-nitrophenyl)-ethyl Amine (SRS2), methyl 3,3-diphenyl-2,3-epoxypropionate (SRS3), methyl 2-hydroxy-3-methoxy-3,3-diphenylmethylpropionate (SRS4 ), 4,6-dimethyl-2-methyl-sulfonylpyrimidine (SRS5) and 4,6-dimethyl-2-(2,2-diphenyl-vinyloxy)pyrimidine (DP1) Mixed samples were taken as an example, and an octadecyl-bonded C18 chromatographic column (Waters symmetry, C18, 5 μm, 150mmx4.6mm) was selected, the mobile phase was acetonitrile / water / glacial acetic acid=55 / 45 / 0.25, and the flow rate was 1.0mL / min, column temperature is 35°C, UV detector, detection wavelength is 220nm, see separation results figure 1 . Using this method, the analysis of ambrisentan and its seven related substances can be completed within 35 minutes, the main component peaks are obvious, the column pressure does not change significantly, the separation baseline is stable, and the separation results a...

Embodiment 2

[0023] Taking the determination of the purity of ambrisentan samples as an example, weigh 1.0 mg of ambrisentan solid sample, place it in a 2.0 mL volumetric flask, and add mobile phase to fully dissolve it. An octyl-bonded C8 chromatographic column (Dikma diamonsil, C8, 5 μm, 150mmx4.6mm) was selected, the mobile phase was acetonitrile / water / glacial acetic acid=60 / 40 / 0.25, the flow rate was 0.5mL / min, the column temperature was 30°C, and UV detector, the detection wavelength is 210nm. The method can be used to accurately determine the purity of the ambrisentan sample, the main component peak is obvious, and the trace impurities can be accurately detected.

Embodiment 3

[0025] Taking the determination of the purity of ambrisentan samples as an example, weigh 1.0 mg of ambrisentan solid sample, place it in a 2.0 mL volumetric flask, and add mobile phase to fully dissolve it. An octadecyl-bonded C18 chromatographic column (Waterssymmetry, C18, 5 μm, 150mmx4.6mm) was selected, the mobile phase was acetonitrile / water / glacial acetic acid=50 / 50 / 0.2, the flow rate was 0.8mL / min, and the column temperature was 30 ℃, ultraviolet detector, the detection wavelength is 190nm. The method can be used to accurately determine the purity of the ambrisentan sample, the main component peak is obvious, and the trace impurities can be accurately detected.

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Abstract

The invention belongs to the field of pharmaceutical analysis, and relates to a method of using isocratic elution high performance liquid chromatography to separate ambrisentan and seven related substances thereof. The main technology characteristics comprise taking a C8 or C18 chromatographic column as a stationary phase, taking an acetonitrile / water / glacial acetic acid mixture as a mobile phase, optimizing the flow velocity and the column temperature, and setting the detection wave length to be 190-230 nm, so as to establish a rapid excellent separation system which is suitable for simultaneously separating ambrisentan and seven related substances thereof. The system employs an isocratic elution method and helps to reduce consumption of separation apparatuses, the experiment separation baseline is stationary, the noise is small, and the separation result reappearance is good. The method is wide in separation object, high in practicality, low in cost, friendly to environment, simple in experiment operation and controllable in separation conditions, is a novel quality control method for ambrisentan, also is a new method for detection analysis on seven related substances of ambrisentan, and has wide application.

Description

technical field [0001] The invention belongs to the field of drug analysis, and specifically relates to establishing a novel high performance liquid chromatography separation method for the analysis and detection of ambrisentan and its seven related substances. Background technique [0002] Ambrisentan (ambrisentan), chemical name: (2S)-(4,6-dimethylpyrimidine-2-oxyl)-3-methoxy-3,3-diphenylpropionic acid, is produced by the United States A highly selective endothelin (ETA) receptor antagonist developed by Denver-based Myogen Biopharmaceuticals for the treatment of pulmonary arterial hypertension can potently inhibit endothelin-induced vasoconstriction. The drug was approved by the US FDA on June 15, 2007. It is clinically used for pulmonary arterial hypertension. Because of its high efficiency and low toxicity, it has become an anti-pulmonary hypertension drug with broad market prospects. [0003] According to current literature reports, ambrisentan is mainly obtained throu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
Inventor 张海枝刘鹏李川石玉李祎亮魏群超徐为人
Owner TIANJIN INSTITUTE OF PHARMA RESEARCH
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