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Method for detecting methyl sulfamate in free amino drug

A technology of methyl sulfamate and free amino groups, which is applied in the direction of measuring devices, material separation, instruments, etc., can solve the problems of difficult detection of methyl sulfamate, and achieve the advantages of quality control, good specificity, and simple operation Effect

Inactive Publication Date: 2022-05-27
BEIJING XINLINGXIAN MEDICAL TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The invention provides a detection method capable of accurately measuring methyl sulfamate in free amino drugs, which overcomes the difficulty in detection of residual methyl sulfamate due to the easy methylation reaction between free amino drugs and methyl sulfamate The problem

Method used

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  • Method for detecting methyl sulfamate in free amino drug
  • Method for detecting methyl sulfamate in free amino drug
  • Method for detecting methyl sulfamate in free amino drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 1 Sample processing

[0061] 1.1 Reference substance stock solution: Take about 3 mg of methyl sulfamate reference substance, accurately weigh it, put it in a 10 mL volumetric flask, add methanol to dissolve and dilute to the mark, and shake well.

[0062] 1.2 Reference substance solution: Precisely measure 0.13mL of the reference substance stock solution, put it in a 10mL volumetric flask, add 10% formic acid solution to dilute to the mark, shake well, accurately measure 2mL, put it in a separatory funnel, and accurately add 4mL of ethyl acetate, After sufficient shaking and standing for separation, the ethyl acetate layer was taken.

[0063] 1.3 Test solution: Accurately weigh 800 mg of the sample, put it in a separatory funnel, add 2 mL of 10% formic acid solution, mix well, accurately add 4 mL of ethyl acetate, shake fully, and after standing for stratification, take the ethyl acetate layer. .

[0064] 2 Experimental process

[0065] 2.1 Linear

[0066] Precisel...

Embodiment 2

[0089] The difference from Example 1 is that Example 2 is not treated with formic acid, and the solvent is methanol, and the operating process of detection is as follows:

[0090] 1 Sample processing

[0091] Reference substance stock solution: take about 3 mg of methyl sulfamate reference substance, accurately weigh it, place it in a 10 mL volumetric flask, add methanol to dissolve and dilute to the mark, shake well, accurately measure 0.3 mL, and place it in a 10 mL volumetric flask , dilute to volume with methanol and shake well.

[0092] Reference substance solution: Precisely measure 1mL of the reference substance stock solution, put it in a 10mL volumetric flask, dilute to the mark with methanol, and shake well.

[0093] Test solution: take about 200 mg of the test, accurately weigh it, put it in a centrifuge tube, add 2 mL of methanol accurately, ultrasonicate for 20 min, and centrifuge at 5000 r / min for 10 min to obtain the supernatant.

[0094] 100% recovery solutio...

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Abstract

The invention belongs to the technical field of drug analysis and detection, and discloses a method for detecting methyl sulfamate in a free amino drug, which is characterized in that the free amino drug is treated by adding formic acid and extracted by using ethyl acetate to prepare a sample solution, and then the content of the methyl sulfamate is detected by using a gas chromatography-mass spectrometer. According to the method, the influence of free amino drugs on the impurity determination of the methyl sulfamate is reduced, the detection sensitivity of the methyl sulfamate is improved, and the detection quantitation limit can reach 30ng / mL. The method is good in specificity, high in sensitivity and beneficial to quality control of free amino drugs.

Description

technical field [0001] The invention belongs to the technical field of drug analysis and detection, and in particular relates to a method for detecting methyl sulfamate in a free amino drug. [0002] technical background [0003] Methyl sulfamate, English name methyl sulfamate, chemical formula CH 5 NO 3 S, molecular weight 111.12, boiling point 199.9±23.0℃. [0004] In the pharmaceutical process, alkyl sulfonic acids are often used as salt-forming reagents for APIs to improve the stability and solubility of drugs, and the precursors of sulfonate esters (such as sulfonyl chlorides) are also commonly used as reagents or catalysts. Sulfonate esters may be formed. Reagents using similar derivatives of sulfamic acid in the reaction process may produce sulfamic acid ester by-products, and their content needs to be detected. Sulfonates are DNA-reactive substances that still present a mutagenic / carcinogenic risk at very low levels, and are defined as genotoxic impurities in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/86G01N30/88
CPCG01N30/02G01N30/72G01N30/06G01N30/8634G01N30/88G01N2030/062G01N2030/884
Inventor 郭硕董颖
Owner BEIJING XINLINGXIAN MEDICAL TECH DEV CO LTD
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