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Quantitative determination method for trace genotoxic impurity trifluoromethanesulfonate in medicine

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

Active Publication Date: 2021-05-11
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 for trace genotoxic impurity trifluoromethanesulfonate in medicine
  • Quantitative determination method for trace genotoxic impurity trifluoromethanesulfonate in medicine
  • Quantitative determination method for trace genotoxic impurity trifluoromethanesulfonate in medicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] This example provides a method for the quantitative determination of triflate, including:

[0059] (1) Drawing of standard curve: add triflate solution into diluent, be made into the triflate standard solution of different concentrations, and measure through headspace-gas chromatography-mass spectrometry, obtain the standard solution The mass spectrometry signal peak area of ​​derivative product and the concentration of standard solution draw standard curve;

[0060] (2) Determination of triflate: put 20mg of drug in a 20ml headspace vial, 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 Area compares with standard curve, obtains the content of trifluoromethanesulfonate in the sample;

[0061] The diluent includes a derivatizing agent and a co-solvent with a volume ratio of 1:4, the derivatizing agent is n-butanol, the co-solven...

Embodiment 2

[0064] This example provides a method for the quantitative determination of triflate, including:

[0065] (1) Drawing of standard curve: add triflate solution into diluent, be made into the triflate standard solution of different concentrations, and measure through headspace-gas chromatography-mass spectrometry, obtain the standard solution The mass spectrometry signal peak area of ​​derivative product and the concentration of standard solution draw standard curve;

[0066] (2) Determination of triflate: put 20mg of drug in a 20ml headspace vial, 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 Area compares with standard curve, obtains the content of trifluoromethanesulfonate in the sample;

[0067] Described diluent comprises derivatizing agent and cosolvent, and volume ratio is 1:4, and described derivatizing agent is n-hexanol, and...

Embodiment 3

[0070] This example provides a method for the quantitative determination of triflate, including:

[0071] (1) Drawing of standard curve: add triflate solution into diluent, be made into the triflate standard solution of different concentrations, and measure through headspace-gas chromatography-mass spectrometry, obtain the standard solution The mass spectrometry signal peak area of ​​derivative product and the concentration of standard solution draw standard curve;

[0072] (2) Determination of triflate: put 20mg of drug in a 20ml headspace vial, 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 Area compares with standard curve, obtains the content of trifluoromethanesulfonate in the sample;

[0073] The diluent includes a derivatizing agent and a co-solvent with a volume ratio of 1:4, the derivatizing agent is n-butanol, the co-solven...

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Abstract

The invention relates to the technical field of drug detection, and especially relates to a quantitative determination method for trace genotoxic impurity trifluoromethanesulfonate in a medicine. The method comprises the following steps: (1) drawing of a standard curve; and (2) determination of the trifluoromethanesulfonate. The problem that trifluoromethanesulfonic acid esters are difficult to detect at present can be solved, and effective technical support is provided for risk monitoring of genotoxic impurities of pharmaceutical enterprises; a derivatization agent and the trifluoromethanesulfonate react, so that the provided determination method is simple, convenient, efficient and accurate, and the problems of instability and more interference in the trifluoromethanesulfonate determination process are avoided; the method can be used for determining trace impurity trifluoromethanesulfonate in the medicine such as azacitidine, also has a good determination effect, and has good accuracy, repeatability and reliability; and when a derivative product is subjected to headspace-gas chromatography-mass spectrometry determination, the method has the characteristics of fast peak appearance, high separation degree and good peak shape, and high sensitivity and specificity can be obtained by adopting mass spectrometry for detection.

Description

technical field [0001] The invention relates to the technical field of drug detection, and more specifically, the invention relates to a method for quantitatively determining trace amounts of genotoxic impurity triflate 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 sulfonate esters, such as methyl trifluoromethanesulfonate Esters, ethyl trifluoromethanesulfonate, methyl methanesulfonate, ethyl methanesulfonate, etc.; arylsulfonate esters such as methyl benzenesulfonate, ethyl benzenesulfonate, etc., are considered as potential alkyl Chemical reagents have been identified as genotoxic substances that cause carcinogenesis. Therefore, it is very important to control the threshold of toxicological concern (TTC) level of such impurities in drugs. [0003] Trifluoromethanesulfonate is a...

Claims

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Application Information

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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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