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Method for detecting parecoxib sodium sulfate genotoxic impurities

A technology of parecoxib sodium and a detection method, which is applied in the detection field of parecoxib sodium sulfate genotoxic impurities, can solve the problem that no reports of dimethyl sulfate diisopropyl sulfate and no simultaneous detection of sulfuric acid have been found. Ester impurities and other problems, to achieve the effect of high detection sensitivity, easy operation, high specificity and durability

Pending Publication Date: 2020-07-14
SHANGHAI CHENPON PHARMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] After literature search, at present, no literature and patents have been found to simultaneously detect these three sulfuric acid ester impurities, and no reports have been made that the impurity limit of dimethyl sulfate, diethyl sulfate, and diisopropyl sulfate is less than 18ppm, and the lower limit of quantitation is less than 1.8 The detection method of ppm

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1) Preparation of solution

[0058] Accurately weigh R1-O reference substance, R1-B reference substance, R1-P reference substance and parecoxib sodium reference substance, add DMSO, dissolve and dilute to the concentration of R1-O reference substance is 1 μg / ml, R1- The concentration of the B reference substance is 1 μg / ml, the concentration of the R1-P reference substance is 1 μg / ml, and the concentration of the parecoxib sodium reference substance is 25 mg / ml, which is used as the resolution solution.

[0059] 2) Instruments and testing conditions:

[0060] Instrument: Agilent5975B MSD in series with 6890GC

[0061] Chromatographic column: gas chromatography column SE-54

[0062] Constant flow mode, the carrier gas is helium, the auxiliary gas is hydrogen and air, the carrier gas flow rate: 1ml / min.

[0063] Column temperature: heating program, the initial temperature is 40°C, the temperature continues to rise to 300°C, and the temperature of the injection port is ...

Embodiment 2

[0071] 1) Preparation of solution

[0072] Accurately weigh R1-O reference substance, R1-B reference substance, R1-P reference substance and parecoxib sodium reference substance, add methanol, dissolve and dilute to the concentration of R1-O reference substance is 1 μg / ml, R1- The concentration of the B reference substance is 1 μg / ml, the concentration of the R1-P reference substance is 1 μg / ml, and the concentration of the parecoxib sodium reference substance is 25 mg / ml, which is used as the resolution solution.

[0073] 2) Instruments and testing conditions:

[0074] Instrument: Agilent5975B MSD in series with 6890GC

[0075] Chromatographic column: gas chromatography column DB-624

[0076] Constant flow mode, the carrier gas is helium, the auxiliary gas is hydrogen and air, the carrier gas flow rate: 1ml / min.

[0077] Column temperature: heating program, the initial temperature is 40°C, the temperature continues to rise to 300°C, and the temperature of the injection por...

Embodiment 3

[0085] 1) Preparation of solution

[0086] Accurately weigh R1-O reference substance, R1-B reference substance, R1-P reference substance and parecoxib sodium reference substance, add tetrahydrofuran, dissolve and dilute to the concentration of R1-O reference substance is 1 μg / ml, R1- The concentration of the B reference substance is 1 μg / ml, the concentration of the R1-P reference substance is 1 μg / ml, and the concentration of the parecoxib sodium reference substance is 1 mg / ml, which is used as the resolution solution.

[0087] 2) Instruments and testing conditions:

[0088] Instrument: Agilent5975B MSD in series with 6890GC

[0089] Chromatographic column: gas chromatography column DB-5

[0090] Constant flow mode, the carrier gas is helium, the auxiliary gas is hydrogen and air, the carrier gas flow rate: 5ml / min.

[0091] Column temperature: heating program, the initial temperature is 60°C, the temperature continues to rise to 350°C, and the temperature of the injection...

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Abstract

The invention relates to a method for detecting parecoxib sodium sulfate genotoxic impurities. The method comprises the following steps of dissolving a dimethyl sulfate reference substance, a diethylsulfate reference substance and a diisopropyl sulfate reference substance to obtain a sulfate impurity reference substance solution, dissolving parecoxib sodium to be detected to obtain a sample solution to be detected, and carrying out gas chromatography-mass spectrometry determination on the sulfate impurity reference substance solution and the sample solution to be detected. The chromatographicconditions are as follows: a filler of the gas chromatographic column is selected from one of a non-polar filler, a weak polar filler and a medium polar filler; and mass spectrum conditions comprisethat an electrospray ion source and a positive ion scanning mode are selected. The method is high in detection precision, has very high specificity and durability, and is simple and convenient to operate. The separation degree between genotoxic impurities is greater than 2.0, and the method can be used for quality control of parecoxib sodium bulk drugs.

Description

technical field [0001] The invention relates to the field of drug analysis and detection, in particular to a detection method for parecoxib sodium sulfate 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 is found that it can generate 3 sulfate impurities, which are respectively dimethyl sulfate (R1-B): diethyl sulfate (R1-O), diisopropyl sulfate ( R1-P). Sulfate is a recognized warning structure in the industry, accor...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/54
CPCG01N30/02G01N30/06G01N30/72G01N30/54G01N2030/025G01N2030/062
Inventor 王晓维罗国军
Owner SHANGHAI CHENPON PHARMA TECH
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