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Method for detecting parecoxib sodium genotoxic impurities

A technology of parecoxib sodium and genotoxicity, which is applied in the field of detection of genotoxic impurities of parecoxib sodium, can solve the problems of unsatisfactory and high detection limit, and achieve simple operation, high specificity and durability, The effect of high detection precision

Pending Publication Date: 2020-05-01
SHANGHAI CHENPON PHARM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the detection limits of the three impurities are all high, reaching 1000ppm, which cannot meet the limits of 18ppm of ethyl 4-(5-methyl-3-phenyl-4-isoxazolyl)benzenesulfonate, 4- Methyl (5-methyl-3-phenyl-4-isoxazolyl)benzenesulfonate and isopropyl 4-(5-methyl-3-phenyl-4-isoxazolyl)benzenesulfonate Detection of these 3 genotoxic impurities

Method used

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  • Method for detecting parecoxib sodium genotoxic impurities
  • Method for detecting parecoxib sodium genotoxic impurities
  • Method for detecting parecoxib sodium genotoxic impurities

Examples

Experimental program
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Embodiment 1

[0065] The elution condition of embodiment 1 is:

[0066] Keep the volume fraction of 0.5% acetic acid aqueous solution at 80%, and keep the volume fraction of acetonitrile at 20%.

Embodiment 2

[0067] The elution condition of embodiment 2 is:

[0068] Within 0min-4.0min, the volume fraction of mobile phase A decreased from 80% to 20%, and the volume fraction of acetonitrile increased from 20% to 80%.

Embodiment 3

[0069] The elution condition of embodiment 3 is:

[0070] 0min-6.0min, the volume fraction of mobile phase A decreased from 80% to 20%, and the volume fraction of acetonitrile increased from 20% to 80%.

[0071] The elution condition of embodiment 4-8 is:

[0072] 0min-3.0min, the volume fraction of mobile phase A drops to 20% by 80%, and the volume fraction of acetonitrile rises to 80% by 20%.

[0073] Draw the following conclusions by the mass spectrogram of embodiment 1-8,

[0074] In Example 1, the main components and impurities were all peaked out within 8 minutes, and the separation between impurities was good, and the impurities R1-M could not be completely separated from the main components.

[0075] In embodiment 2, main component and impurity all go out peak and complete within 8 minutes, and each component peak shape is good, and main component and each impurity baseline are separated, and the degree of separation between impurities reaches 1.3. The mass spectrum...

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Abstract

The invention relates to a method for detecting parecoxib sodium genotoxic impurities. The detection method comprises the following steps of dissolving an R1-M reference substance, an R1-C reference substance and an R1-N reference substance separately to obtain three kinds of impurity reference substance solutions; dissolving parecoxib sodium to be tested to obtain a sample solution to be tested;performing liquid chromatography / mass spectrometry determination on the three kinds of impurity reference substance solutions and the sample solution to be tested; the chromatographic conditions include: the mobile phase A is volatile acid or buffer solution, and the mobile phase B is acetonitrile; and the mass spectrometry conditions include: selecting an electrospray ionization, a positive ion scanning mode, the declustering potential is 25 to 200V, the collision energy is 10 to 100eV, the capillary voltage is 2000 to 6000V, the capillary temperature is 250 to 400 DEG C, and the drying gas temperature is 250 to 600 DEG C. The detection limit of the above method reaches 0.3ppm, the limit of quantification reaches 1ppm, and the quality control of pareximab sodium bulk drugs can be well carried out.

Description

technical field [0001] The invention relates to the field of drug analysis and detection, in particular to a detection method of parecoxib sodium genotoxic impurities. Background technique [0002] Parecoxib sodium is a non-steroidal anti-inflammatory drug and is the first selective cyclooxygenase-2 inhibitor that can be used simultaneously intravenously and intramuscularly in the world. Compared with traditional non-selective cyclooxygenase inhibitors , has the characteristics of good analgesic effect, rapid onset, long-lasting effect, effective inhibition of hyperalgesia, high gastrointestinal safety, no effect on platelet function, and no additional cardiovascular risk. [0003] When synthesizing and preparing the bulk drug of Parecoxib Sodium, it was found that it would generate 3 arylsulfonate impurities, namely 4-(5-methyl-3-phenyl-4-isoxazolyl)benzenesulfonic acid Methyl ester (R1-M), ethyl 4-(5-methyl-3-phenyl-4-isoxazolyl)benzenesulfonate (R1-C), 4-(5-methyl-3-benz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 王晓维罗国军杜狄峥
Owner SHANGHAI CHENPON PHARM TECH CO LTD
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