Method for detecting methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate residues

A technology of ethyl trifluoromethanesulfonate and methyl trifluoromethanesulfonate, which is applied in the field of analytical chemistry, can solve problems such as poor detection accuracy, and achieve the effects of stable baseline, avoiding interference, and strong selectivity

Active Publication Date: 2021-08-13
英格尔检测技术服务(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the embodiments of the present invention is to provide a detection method for methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate residues, ai...

Method used

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  • Method for detecting methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate residues
  • Method for detecting methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate residues
  • Method for detecting methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate residues

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Embodiment 1

[0041] The specific research of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate residual determination in embodiment 1 crude drug:

[0042] Accurately weigh about 100mg of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate into a 100mL volumetric flask containing about 10mL of isopropanol (IPA), shake well after distilling to the mark with isopropanol, respectively Labeled methyl triflate-IPA solution, ethyl triflate-IPA solution. Methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate are respectively reacted with isopropanol in a solution of isopropanol, and the reaction is as follows:

[0043]

[0044] The methyl trifluoromethanesulfonate-IPA solution and the ethyl trifluoromethanesulfonate-IPA solution were analyzed by GC-MS respectively, and the chromatographic conditions and mass spectrometry conditions were as follows:

[0045] The chromatographic conditions are:

[0046] The chromatographic column adopts DB-FFAP ca...

Embodiment 2

[0056] Sensitivity, precision, linearity, accuracy and stability research of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate residual determination in embodiment 2 crude drug:

[0057] Accurately weigh about 100mg of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate into a 100mL volumetric flask containing about 10mL of isopropanol, shake up to the mark with isopropanol, and precisely pipette 0.25 Put mL of this solution into a 100mL volumetric flask, dilute to the mark with isopropanol, shake well, and mark it as the reference substance stock solution.

[0058] The chromatographic conditions and mass spectrometry conditions of the GC-MS analysis method are as follows:

[0059] The chromatographic conditions are:

[0060] The chromatographic column adopts DB-FFAP capillary gas chromatography column, the column length is 30m, the inner diameter is 0.32mm, and the film thickness is 1.0μm;

[0061] Helium was used as the carrier gas, and ...

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Abstract

The invention is applicable to the technical field of analytical chemistry, and provides a method for detecting methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate residues. The method comprises the steps of dissolving a sample to be detected with alcohol, and fixing the volume to obtain a sample solution; dissolving methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate reference substances with alcohol, and carrying out volume metering to acquire a plurality of reference substance solutions with concentration gradients; sequentially injecting the reference substance solutions and the sample solution according to chromatographic conditions and mass spectrum conditions for analysis to acquire spectrum data; and drawing a linear correlation working curve according to the spectrum data, and calculating the residues of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate in the sample to be detected. The sample treatment process is simple and convenient, alcohol serves as a solvent and a derivatization reagent, the derivatization reaction is mild, rapid and complete, interference of a complex derivatization reagent on detection is avoided, the detection specificity, precision and accuracy are improved, and the method has an important research value in the aspects of bulk drug quality research, impurity analysis and control research and the like.

Description

Technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for detecting methyl triflate and ethyl triflate residues. Background technique [0002] Pharmaceutical impurities are chemical components that are undesirable in active pharmaceutical ingredients (APIs) or pharmaceutical preparations. Impurities in raw materials may originate from the synthesis process or starting materials, intermediates, solvents, catalysts, reaction by-products, unstable ingredients of the raw materials, incompatibility with excipients, or reactions with packaging materials, etc. Various impurities in drugs have a great impact on the safety of the final drug. Among them, Genotoxic Impurity (GTI) refers to the compound itself that directly damages the DNA of cells, produces genetic mutations or mutagenesis in the body, and has the possibility or tendency to cause cancer. Its characteristic is that it can cause damage to human...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/067
Inventor 樊华军张振洋
Owner 英格尔检测技术服务(上海)有限公司
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