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A method for determining febuxostat and impurities in an oral preparation by HPLC

A technology for oral preparations and related substances, which is applied in the detection field of febuxostat and related substances in oral preparations, can solve the problems of undegraded products, process side reaction impurities control, etc., achieve good elution and separation effects, convenient operation, The effect of high precision

Active Publication Date: 2014-08-06
湖北潜龙药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN102565225A discloses a method for determining related substances by high performance liquid chromatography during the synthesis of febuxostat, targeting the intermediate I (3-cyano-4-isobutoxysulfur benzamide) and intermediate II (2-[3-cyano-4-isobutoxyphenyl]-4-methylthiazole-5-ethyl carboxylate) (impurity 7 referred to in this patent) control, but the two documents did not fully control the degradation products and process side reaction impurities in febuxostat and oral preparations

Method used

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  • A method for determining febuxostat and impurities in an oral preparation by HPLC
  • A method for determining febuxostat and impurities in an oral preparation by HPLC
  • A method for determining febuxostat and impurities in an oral preparation by HPLC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Instrument: Agilent1100 HPLC, 1100 UV detector

[0049] Chromatographic column: a chromatographic column (150×4.6mm, 5μm) filled with octadecylsilane bonded silica gel;

[0050] Mobile phase A: 0.01mol / L potassium dihydrogen phosphate solution (adjust the pH value to 3.0 with phosphoric acid):methanol=50:50(v / v)

[0051] Mobile Phase B: Acetonitrile

[0052] See the table below for gradient elution;

[0053] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

60

40

10

60

40

14

40

60

22

40

60

23

60

40

27

60

40

[0054] Flow rate: 1.0mL / min

[0055] Detection wavelength: 220nm

[0056] Column temperature: 30°C

[0057] Injection volume: 10μl

[0058] Diluent: acetonitrile: water = 80:20 (v / v)

[0059] Test steps: Accurately weigh about 15 mg each of impurity 1, impurity 2, impurity 3, impurity 4, impurity 5, impurity 6, impurity 7, and impurity 8, and ...

Embodiment 2

[0064] Instrument: Agilent1100 HPLC, 1100 UV detector

[0065] Chromatographic column: a chromatographic column (150×4.6mm, 5μm) filled with octadecylsilane bonded silica gel;

[0066] Mobile phase A: 0.01mol / L potassium dihydrogen phosphate solution (adjust the pH value to 3.2 with phosphoric acid):methanol=50:50(v / v)

[0067] Mobile Phase B: Acetonitrile

[0068] See the table below for gradient elution;

[0069] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

60

40

10

60

40

14

40

60

22

40

60

23

60

40

27

60

40

[0070] Flow rate: 1.0mL / min

[0071] Detection wavelength: 220nm

[0072] Column temperature: 30°C

[0073] Injection volume: 10μl

[0074] Diluent: acetonitrile: water = 80:20 (v / v)

[0075] Test steps: Accurately weigh about 2 mg each of impurity 1, impurity 2, impurity 3, impurity 7, impurity 8, and impurity 9, and 30 mg of febuxostat, and ...

Embodiment 3

[0080] Instrument: Agilent1100 HPLC, 1100 UV detector

[0081] Chromatographic column: a chromatographic column (150×4.6mm, 5μm) filled with octadecylsilane bonded silica gel;

[0082] Mobile phase A: 0.01mol / L potassium dihydrogen phosphate solution (adjust the pH value to 3.0 with phosphoric acid): Methanol=50:50(v / v)

[0083] Mobile Phase B: Acetonitrile

[0084] See the table below for gradient elution;

[0085] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

60

40

10

60

40

14

40

60

22

40

60

23

60

40

27

60

40

[0086] Flow rate: 1.0mL / min

[0087] Detection wavelength: 220nm

[0088] Column temperature: 30°C

[0089] Injection volume: 10μl

[0090] Diluent: acetonitrile: water = 80:20 (v / v)

[0091] Test procedure: Accurately weigh 0.2532g of febuxostat tablet ground powder in a 100ml volumetric flask, add an appropriate amount of diluent, ultrasoni...

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Abstract

The present invention discloses a method for determining febuxostat and impurities in an oral preparation by HPLC, wherein octadecylsilane chemically bonded silica is selected as a stationary phase, and a mixed solvent of an organic phase and a buffer is used as a mobile phase for gradient elution. By using the method of the invention, febuxostat and impurities in the oral preparation can be separated quickly and efficiently under the same chromatographic conditions, effectively controlling the quality of an active ingredient and the preparation. The detection method is specific, high in precision, high in accuracy, and easy to operate, and can effectively control the quality of medicines.

Description

technical field [0001] The invention relates to a detection method for related substances in febuxostat and oral preparations, in particular to a method for determining degradation products, process side reaction impurities and intermediates of febuxostat and oral preparations by using HPLC (high performance liquid chromatography) . Background technique [0002] Gout is a heterogeneous disease with increased blood uric acid due to purine metabolism disorder and uric acid excretion disorder, including hyperuricemia, recurrent gouty acute arthritis, characteristic chronic arthritis, and joint deformities. Often the kidneys are involved causing chronic intermittent nephritis and the formation of uric acid stones. In recent years, with the improvement of living standards, prolongation of life expectancy, unbalanced diet structure, and increase of obese people, the prevalence of gout has continued to rise. Gout, as a metabolic disease accompanied by severe joint pain, seriously...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/34
Inventor 夏艳开
Owner 湖北潜龙药业有限公司
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