Detection method of parecoxib sodium genotoxicity impurity and application thereof

A parecoxib sodium and detection method technology, which is applied in the field of drug analysis, can solve problems such as unretrieved, and achieve the effects of simple operation, high sensitivity and specificity

Active Publication Date: 2016-03-02
TIANJIN INSTITUTE OF PHARMA RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among the published patents, CN104749288A discloses a liquid chromatography analysis method for related substances of parecoxib sodium, which controls 4-(5-methyl

Method used

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  • Detection method of parecoxib sodium genotoxicity impurity and application thereof
  • Detection method of parecoxib sodium genotoxicity impurity and application thereof
  • Detection method of parecoxib sodium genotoxicity impurity and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation method of the parecoxib sodium genotoxic impurity detection solution of the present invention.

[0032] This test chooses water, acetonitrile, methanol, water: acetonitrile (1:1) to dissolve the sample, the sample is slightly soluble in water, slightly soluble in acetonitrile, and easily soluble in methanol, water: acetonitrile (1:1). Since 3 genotoxic impurities need to be added to the parecoxib sodium sample during the investigation of chromatographic conditions, the structures of impurity A, impurity B, and impurity C are all ester substances, which are easily hydrolyzed, and the solvent should not contain water, so methanol is preferred solvent for dissolving the sample.

[0033] In this test, the parecoxib sodium sample was prepared into a 0.5mg / ml-4mg / ml solution for investigation. The results showed that the impurity response at 0.5mg / ml was small, and the asymmetry of the main peak at 4mg / ml was serious, which affected the detection of impurities...

Embodiment 2

[0035] The detection method of parecoxib sodium genotoxic impurity of the present invention

[0036] 1) Instruments and testing conditions

[0037] Instrument: WatersE2695 high performance liquid chromatography-ultraviolet detector;

[0038] Chromatographic column: C8 column (4.6×150mm, 5μm);

[0039] Mobile phase: water: acetonitrile (50:50);

[0040] Column temperature: 25°C; flow rate: 1.0mL / min;

[0041] Detection wavelength: 230nm; injection volume: 10μl.

[0042] 2) Solution preparation

[0043] Accurately weigh an appropriate amount of impurity A, impurity B, and impurity C reference substances, add methanol to dissolve and dilute to a 0.5mg / ml solution, and use it as an impurity stock solution; accurately weigh 40mg of parecoxib sodium into a 10ml volumetric flask, and accurately weigh Measure 1ml of each impurity stock solution into the volumetric flask, add methanol to dissolve and dilute to the mark, and use it as the chromatographic condition screening solutio...

Embodiment 3

[0047] The detection method of parecoxib sodium genotoxic impurity of the present invention

[0048] 1) Instruments and testing conditions

[0049] Instrument: WatersE2695 high performance liquid chromatography-ultraviolet detector;

[0050] Chromatographic column: C8 column (4.6×150mm, 5μm);

[0051] Mobile phase: pH3.0 dilute phosphoric acid: acetonitrile (70:30);

[0052] Column temperature: 30°C; flow rate: 2mL / min;

[0053] Detection wavelength: 290nm; injection volume: 40μl.

[0054] 2) Solution preparation

[0055] Accurately weigh an appropriate amount of impurity A, impurity B, and impurity C reference substances, add methanol to dissolve and dilute to a 0.5mg / ml solution, and use it as impurity stock solution; accurately weigh 10mg of parecoxib sodium into a 10ml volumetric flask, and accurately weigh Measure 1ml of each impurity stock solution into the volumetric flask, add methanol to dissolve and dilute to the mark, and use it as the chromatographic condition...

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Abstract

The present invention provides a detection method of parecoxib sodium genotoxicity impurity and application thereof. The method uses a reversed-phase liquid chromatography method. The chromatography conditions are as follows: the chromatographic column comprise a C18 column, a C8 column, a phenyl column and a Hilic column; a mobile phase consists of water-acetonitrile, dilute phosphoric acid-acetonitrile, and phosphate-acetonitrile; a flow phase comprises an aqueous phase and an organic phase in the ratio of 90:10-10:90; the column temperature is 25-40 DEG C; the flow rate of the mobile phase is 0.2-2ml / min; detection wavelength is 205-290nm; a detector is a UV detector or a photodiode array (PDA) detector; and the sample size is 0.1-40 mul. The detection method of parecoxib sodium genotoxicity impurity achieves the separation of parecoxib sodium and three genotoxicity impurities in a short period of time, has high sensitivity and specificity, and simple operation, reaches the separation rate of the main component and genotoxicity impurities, and the separation rate of genotoxicity impurities both greater than 1.5; and the method can be used for quality control of parecoxib sodium, and has practical value.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for detecting the genotoxic impurity of parecoxib sodium, and more particularly to a reversed-phase liquid chromatography analysis and detection method for the genotoxic impurity of parecoxib sodium. Background technique [0002] Non-steroidal anti-inflammatory drugs (NSAIDs), as an analgesic, are usually used to treat acute and chronic pain. Their mechanism of action is to inhibit the synthesis and release of prostaglandins by inhibiting cyclooxygenase (COX), thereby producing an analgesic effect. Traditional non-steroidal anti-inflammatory drugs (such as naproxen, indomethacin, diclofenac, nimesulide, etc.) have been used clinically for decades, but the side effects of long-term use are more obvious, such as indigestion, abdominal pain and other gastric Intestinal side effects, leading to gastric perforation, duodenal ulcer and other diseases in severe cases, its...

Claims

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Application Information

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IPC IPC(8): G01N30/89
Inventor 郝英魁闫少杰蒋庆峰黄汉忠
Owner TIANJIN INSTITUTE OF PHARMA RESEARCH
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