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Method for determining related substances by utilizing high performance liquid chromatography in febuxostat synthesis process

A technology of high performance liquid chromatography and febuxostat, which is applied in the field of determination of related substances by high performance liquid chromatography, can solve the unfavorable quality control of the final product of febuxostat, inability to effectively detect component peaks, large polarity differences, etc. problem, to achieve the effect of good elution and separation effect, simple and fast method, and appropriate peak time

Inactive Publication Date: 2012-07-11
CISEN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, due to the low polarity of intermediate II, when using the above three mobile phases for determination, either no peak or peak time is particularly late, which is not conducive to the quality control of febuxostat final product; on the other hand, The polarity between some impurities and the product febuxostat is similar, and the polarity difference between some impurities and febuxostat is relatively large. In actual work, the above method cannot effectively detect the peaks of each component in the sample.

Method used

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  • Method for determining related substances by utilizing high performance liquid chromatography in febuxostat synthesis process
  • Method for determining related substances by utilizing high performance liquid chromatography in febuxostat synthesis process
  • Method for determining related substances by utilizing high performance liquid chromatography in febuxostat synthesis process

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Effect test

Embodiment 1

[0024] Instruments and Conditions

[0025] High performance liquid chromatography: Waters2695 pump; Waters2487 UV detector

[0026] Chromatographic column: Octadecylsilane bonded silica gel column (250mmx4.6mm, 5μm)

[0027] Mobile phase: acetonitrile-0.5% formic acid aqueous gradient elution see the table below

[0028] gradient elution table

[0029]

[0030] Flow rate: 1.0ml / min

[0031] Detection wavelength: 317nm

[0032] Column temperature: room temperature

[0033] Injection volume: 20μl

[0034] Implementation steps

[0035] Accurately weigh about 25 mg each of febuxostat, starting material, intermediate I, and intermediate II respectively, place in a 50ml measuring bottle, add acetonitrile to dissolve and dilute to the mark, shake well, and use it as the test solution. Get need testing solution, carry out HPLC analysis under above-mentioned chromatographic condition, record chromatogram, the result sees attached figure 1 .

[0036] figure 1 The chromatogr...

Embodiment 2

[0038] Instruments and Conditions

[0039] High performance liquid chromatography: Waters2695 pump; Waters2487 UV detector

[0040] Chromatographic column: Octadecylsilane bonded silica gel column (250mmx4.6mm, 5μm)

[0041] Mobile phase: acetonitrile-0.5% formic acid aqueous gradient elution see the table below

[0042] gradient elution table

[0043]

[0044] Flow rate: 1.0ml / min

[0045] Detection wavelength: 317nm

[0046] Column temperature: room temperature

[0047] Injection volume: 20μl

[0048] Implementation steps

[0049] Accurately weigh about 25mg of febuxostat, place it in a 50ml measuring bottle, add acetonitrile to dissolve and dilute to the mark, shake well, and use it as the test solution. Get need testing solution, carry out HPLC analysis under above-mentioned chromatographic condition, record chromatogram, the result sees attached figure 2 .

[0050] figure 2 The chromatographic peak whose retention time is 12.292 minutes is the chromatograph...

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Abstract

The invention discloses a method for determining related substances by utilizing high performance liquid chromatography in febuxostat synthesis process and belongs to the field of chromatographic analysis. According to the method, octadecylsilane chemically bonded silica gel is taken as the chromatographic column packing, a mixed solvent gradient elution taking organic phase and organic acid solution as aqueous phase serves as mobile phase, wherein the organic phase is acetonitrile or methanol; and the organic acid solution is formic acid solution with the volume percent of 0.1%-0.8% or acetic acid solution with the volume percent of 0.1%-0.8%. Compared with the prior art, the method for determining related substances by utilizing high performance liquid chromatography in febuxostat synthesis process has the characteristics of high analysis sensitiveness, accurate and reliable results and the like, and has good popularization and application values in the quality control field of febuxostat.

Description

technical field [0001] The invention relates to the field of chromatographic analysis, in particular to a method for determining related substances by high-performance liquid chromatography in the febuxostat synthesis process. Background technique [0002] Gout is a metabolic disease accompanied by severe pain in the joints. With the continuous improvement of living standards, the unbalanced diet structure causes purine metabolism disorder, leading to excessive production of uric acid or insufficient uric acid excretion, which leads to elevated blood uric acid, and uric acid crystals accumulate in the joints, soft tissues, kidneys and heart. severe pain. The use of drugs to reduce the concentration of uric acid in the blood is one of the common methods to prevent the occurrence of gout. Febuxostat is the first non-purinol new generation xanthine oxidase inhibitor, which inhibits the activity of xanthine oxidase, prevents and reduces the synthesis of uric acid from hypoxant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 李明丽薛晓霞李瑞明
Owner CISEN PHARMA
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