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Analytical method for related substances of roxadustat

A technique for roxadustat and related substances, which is applied in the field of roxadustat related substance analysis, and can solve problems such as methods for determining roxadustat related substances that have not been seen

Active Publication Date: 2022-06-24
JIANGSU WANBANG BIOPHARMLS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, there is no method for the determination of related substances of roxadustat reported in the literature

Method used

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  • Analytical method for related substances of roxadustat
  • Analytical method for related substances of roxadustat

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Choice of diluent.

[0042] Purpose of the test: Due to the difference in polarity of different impurities, different polar solvents can dissolve impurities differently. Therefore, in order to ensure that the impurities in the sample are completely dissolved, the dilution solution is studied.

[0043] Test process: Take roxadustat, impurity A, impurity B, impurity C, impurity D, impurity E, impurity F, impurity H, and impurity I, and dilute them with acetonitrile respectively to prepare a solution with a concentration of 0.2 mg / ml, wherein Impurity D, impurity H, and impurity I cannot be completely dissolved. Use a mixture of acetonitrile and water with a volume ratio of 4:1 as the diluent, then roxadustat and its related substances can be completely dissolved, see figure 1 .

[0044] Impurity A is 4-hydroxyl-N, N-dimethyl-7-phenoxyisoquinoline-3-carboxamide; impurity B is [4-hydroxyl-1-(hydroxymethyl)-7-phenoxy Isoquinolin-3-yl] (morpholinyl) ketone; Impurity C is [...

Embodiment 2

[0047] Column screening.

[0048] Purpose of the test: to select a suitable chromatographic column to effectively separate roxadustat and related substances.

[0049] Instrument equipment and chromatographic conditions: Liquid chromatography: Thermo UltiMate 3000; UV variable wavelength detector; gradient elution with 0.1% trifluoroacetic acid aqueous solution-acetonitrile as mobile phase, see Table 1; column temperature 30°C; detection wavelength 230nm; flow rate 1ml per minute; injection volume 10μl;

[0050] Table 1 Gradient elution program

[0051]

[0052] Sample preparation: Take roxadustat, impurity A, impurity B, impurity C, impurity D, impurity E, impurity F, impurity H, impurity I, and use acetonitrile and water with a volume ratio of 4:1 as the diluent Diluted to prepare a solution containing 0.2 mg of roxadustat per 1 ml and 0.2 μg of each impurity. See Table 2 for column selection.

[0053] Table 2 Screened column list

[0054] serial number Man...

Embodiment 3

[0057] Impurity localization study

[0058] Purpose of the test: to determine the retention time of roxadustat and each known impurity.

[0059]Instrument equipment and chromatographic conditions: liquid chromatograph: Thermo UltiMate 3000; UV variable wavelength detector; chromatographic column: Ultimate XB-C8, 250mm*4.6mm, 3μm; 0.1% trifluoroacetic acid aqueous solution-acetonitrile as mobile phase Gradient elution, see Table 3; column temperature 30°C; detection wavelength 230nm; flow rate 1ml per minute; injection volume 10μl;

[0060] Table 3 Gradient elution program

[0061]

[0062] Sample preparation: Take roxadustat, impurity A, impurity B, impurity C, impurity D, impurity E, impurity F, impurity H, and impurity I, and dilute them with acetonitrile and water at a volume ratio of 4:1. The solution was diluted, and prepared into solutions containing 0.2 mg of roxadustat and each related substance per 1 ml, respectively, as each positioning solution. Take roxadusta...

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Abstract

The invention relates to a method for analyzing related substances of roxadustat. The method is carried out on a high-performance liquid chromatograph, using an Ultimate XB chromatographic column, using trifluoroacetic acid aqueous solution and an organic solvent as mobile phases, and a liquid phase diode array detector Or ultraviolet detector carries out gradient elution detection, effectively separates and detects roxadustat related substances, the analytical method of the present invention can fully control the related substances in roxadustat, improves drug safety, and is for formulating roxadustat Provide the basis for the quality standard of Sestat API.

Description

technical field [0001] The invention relates to a method for analyzing related substances of roxadustat, which belongs to the field of medicine and chemical industry. Background technique [0002] Roxadustat, the chemical name is [(4-hydroxy-1-methyl-7-phenoxy-isoquinoline-3-formyl)-amino]-acetic acid, and its chemical structure is: [0003] [0004] is a potent inhibitor of hypoxia-inducible factor (HIF) prolyl hydroxylase, of use in increasing the stability and / or activity of HIF, and in particular for the treatment and prevention of HIF-related disorders, including anemia and Use in ischemia and hypoxia-related disorders. The commonly used synthetic route of roxadustat is as follows: [0005] [0006] So far, there is no literature report on the method for the determination of related substances of roxadustat. Contents of the invention [0007] Aiming at the deficiencies in the prior art, the present invention provides a method for analyzing related substances ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/89G01N30/06G01N30/74G01N30/64
CPCG01N30/89G01N30/06G01N30/74G01N30/64
Inventor 王克艳梁慧李兴刘跃跃
Owner JIANGSU WANBANG BIOPHARMLS
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