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Quantitative determination method of trace genotoxic impurity triflate in medicine

A trifluoromethanesulfonate, quantitative determination technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult detection, difficult storage, high reactivity, etc., to achieve good measurement effect, high sensitivity and specificity, fast peak effect

Active Publication Date: 2022-07-12
上海微谱检测科技集团股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since trifluoromethanesulfonic acid is a very good leaving group, the reactivity of trifluoromethanesulfonate is higher than that of other alkylsulfonate and arylsulfonate, it is not easy to store, and it is sensitive to water in the air , may react chemically with conventional solvents, etc. It is more difficult to detect other alkyl sulfonates and aryl sulfonates
At present, the detection of triflate impurities has not been reported

Method used

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  • Quantitative determination method of trace genotoxic impurity triflate in medicine
  • Quantitative determination method of trace genotoxic impurity triflate in medicine
  • Quantitative determination method of trace genotoxic impurity triflate in medicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] This example provides a quantitative determination method for trifluoromethanesulfonate, including:

[0059] (1) Drawing of the standard curve: adding the trifluoromethanesulfonate solution to the diluent to prepare standard solutions of trifluoromethanesulfonate with different concentrations, and measuring by headspace-gas chromatography-mass spectrometry to obtain the standard solution in the standard solution. Draw a standard curve of the peak area of ​​the mass spectrum signal of the derivative product and the concentration of the standard solution;

[0060] (2) Determination of trifluoromethanesulfonate: put 20mg of the drug in a 20ml headspace bottle, add 1ml of diluent to obtain a sample solution, use headspace-gas chromatography-mass spectrometry to measure, and obtain the mass spectrum signal peak of the derivative product in the sample Compare the area with the standard curve to obtain the content of trifluoromethanesulfonate in the sample;

[0061] The dilue...

Embodiment 2

[0064] This example provides a quantitative determination method for trifluoromethanesulfonate, including:

[0065] (1) Drawing of the standard curve: adding the trifluoromethanesulfonate solution to the diluent to prepare standard solutions of trifluoromethanesulfonate with different concentrations, and measuring by headspace-gas chromatography-mass spectrometry to obtain the standard solution in the standard solution. Draw a standard curve of the peak area of ​​the mass spectrum signal of the derivative product and the concentration of the standard solution;

[0066] (2) Determination of trifluoromethanesulfonate: put 20mg of the drug in a 20ml headspace bottle, add 1ml of diluent to obtain a sample solution, use headspace-gas chromatography-mass spectrometry to measure, and obtain the mass spectrum signal peak of the derivative product in the sample Compare the area with the standard curve to obtain the content of trifluoromethanesulfonate in the sample;

[0067] The dilue...

Embodiment 3

[0070] This example provides a quantitative determination method for trifluoromethanesulfonate, including:

[0071] (1) Drawing of the standard curve: adding the trifluoromethanesulfonate solution to the diluent to prepare standard solutions of trifluoromethanesulfonate with different concentrations, and measuring by headspace-gas chromatography-mass spectrometry to obtain the standard solution in the standard solution. Draw a standard curve of the peak area of ​​the mass spectrum signal of the derivative product and the concentration of the standard solution;

[0072] (2) Determination of trifluoromethanesulfonate: put 20mg of the drug in a 20ml headspace bottle, add 1ml of diluent to obtain a sample solution, use headspace-gas chromatography-mass spectrometry to measure, and obtain the mass spectrum signal peak of the derivative product in the sample Compare the area with the standard curve to obtain the content of trifluoromethanesulfonate in the sample;

[0073] The dilue...

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Abstract

The invention relates to the technical field of drug detection, and more particularly, to a method for quantitative determination of trifluoromethanesulfonate, a trace amount of genotoxic impurity in drugs. Including: (1) Drawing of standard curve; (2) Determination of trifluoromethanesulfonate. It can solve the problem that trifluoromethanesulfonates are difficult to detect at present, and provide effective technical support for the risk monitoring of genotoxic impurities in pharmaceutical companies; the reaction of derivatizing agents and trifluoromethanesulfonates provides a simple, efficient and accurate determination method , which avoids the problems of instability and more interference during the determination of trifluoromethanesulfonate; it can be used for the determination of trace impurities in drugs, such as azacitidine, trifluoromethanesulfonate, and also has a good determination effect. Good accuracy, repeatability and reliability; when headspace-gas chromatography-mass spectrometry is used for the determination of derivative products, it has the characteristics of fast peak output, high resolution and good peak shape. sensitivity and specificity.

Description

technical field [0001] The invention relates to the technical field of drug detection, and more particularly, to a method for quantitative determination of trifluoromethanesulfonate, a trace amount of genotoxic impurity in drugs. Background technique [0002] Alkyl sulfonic acid and aryl sulfonic acid are often used in the steps of drug synthesis, recrystallization and salt formation, while methanol and ethanol are commonly used solvents, which may generate sulfonic acid esters, such as alkyl sulfonic acid esters such as methane trifluoromethanesulfonate Esters, ethyl trifluoromethanesulfonate, methyl methanesulfonate, ethyl methanesulfonate, etc.; aryl sulfonates such as methyl benzenesulfonate, ethyl benzenesulfonate, etc., are considered as potential alkyl groups chemical agents, which have been identified as carcinogenic genotoxic substances. Therefore, it is very important to control the Threshold of Toxicological Concern (TTC) level of such impurities in pharmaceutica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06
CPCG01N30/02G01N30/72G01N30/06G01N2030/067
Inventor 邵红霞秦秋明汪辉刘婷
Owner 上海微谱检测科技集团股份有限公司
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