Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of detection method of genotoxic impurity in safinamide mesylate

A technology of saphiramide mesylate and genotoxicity, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problem that the detection sensitivity cannot meet the content requirements, and achieves the effect of high sensitivity

Active Publication Date: 2022-04-08
HEBEI GUOLONG PHARMA CO LTD
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Aiming at the problem that the existing detection sensitivity of (S)-4-(((1-amino-1-oxypropane-2-methyl)amino)methyl)benzene mesylate cannot meet the content requirements of impurities in raw materials , the invention provides a method for detecting genotoxic impurities in safinamide mesylate

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of detection method of genotoxic impurity in safinamide mesylate
  • A kind of detection method of genotoxic impurity in safinamide mesylate
  • A kind of detection method of genotoxic impurity in safinamide mesylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The embodiment of the present invention provides a kind of detection method of genotoxic impurity in safinamide mesylate, described detection method comprises the following steps:

[0050] Step 1, preparing the test solution, reference solution, blank solution and mixed solution;

[0051] The preparation method of the above-mentioned reference substance solution is: take (S)-4-(((1-amino-1-oxypropane-2-methyl)amino)methyl)benzene mesylate as reference substance, and methanol as solvent to obtain a concentration of 305.45ng / mL stock solution, and then dilute the above stock solution to obtain a concentration of 15ng / mL reference substance solution.

[0052] The preparation method of above-mentioned need testing solution is: get need testing 10mg and place in 10mL volumetric flask, adopt methanol to dissolve and dilute value scale, obtain the need testing solution that concentration is 1mg / mL.

[0053] The blank solution is methanol;

[0054] The preparation method of t...

Embodiment 2

[0064] Embodiment 2 detection limit and quantitative limit

[0065] Detection limit: the concentration of 15ng / mL reference substance solution prepared in Example 1 is quantitatively diluted step by step with methanol, and then detected by liquid chromatography-mass spectrometry, the specific conditions of liquid chromatography and mass spectrometry are as described in Example 1 , record the spectrogram, and obtain the detection limit according to the signal-to-noise ratio not lower than 3:1, and the results are shown in Table 1.

[0066] Limit of quantification: the concentration prepared in Example 1 is that the 15ng / mL reference substance solution is quantitatively diluted step by step with methanol, and then the liquid chromatography-mass spectrometry method is used to detect the limit of quantification solution. The specific conditions of liquid chromatography and mass spectrometry are as follows: As described in Example 1, record the spectrogram, and obtain the quantific...

Embodiment 3

[0072] Example 3 Linearity

[0073] The concentration of 305.45ng / mL reference substance stock solution prepared in Example 1 was diluted with methanol to obtain concentrations of 1.53ng / mL, 3.05ng / mL, 9.16ng / mL, 15.27ng / mL, 21.38ng / mL, 30.54ng / mL linear solution.

[0074] Adopt liquid chromatography-mass spectrometry to detect linear solution, the specific conditions of liquid chromatography and mass spectrometry are as described in Example 1, record spectrogram information, then take the concentration (ng / mL) of reference substance impurity O as abscissa , take the peak area as the ordinate, draw the standard curve, and calculate the regression equation, the results are shown in Table 3, and the linear graph is shown in Figure 5 . From Figure 5 It can be seen that the impurity O has a good linear relationship within the concentration range of 1.53-30.54 ng / mL.

[0075] Table 3 Impurity O linearity test results

[0076]

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
concentrationaaaaaaaaaa
concentrationaaaaaaaaaa
Login to View More

Abstract

The invention relates to the technical field of drug analysis, and specifically discloses a detection method for genotoxic impurities in safinamide mesylate. Described detection method comprises the following steps: prepare need testing solution and reference substance solution; Adopt liquid chromatography-mass spectrometry to detect described need testing solution and described reference substance solution, the chromatographic condition of described liquid chromatography Be: adopt C18 chromatographic column, take the formic acid aqueous solution that volume concentration is 0.1% as mobile phase A, the formic acid methanol solution that volume concentration is 0.1% is mobile phase B, gradient elution; Described mass spectrometry adopts ESI ion source, positive ion detection mode. The detection method provided by the invention has the advantages of simple method, stability, high precision, good reproducibility, etc., can quickly and accurately detect the toxic impurities in the safinamide mesylate bulk drug, and conforms to the guiding principle of ICH M7 .

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting genotoxic impurities in safinamide mesylate. Background technique [0002] Parkinson's is the second most common chronic neurodegenerative disease in the elderly after Alzheimer's disease, and it is more common in middle-aged and elderly people. Amine oxidase B (MAO-B) inhibitors can be used as monotherapy in patients with early Parkinson's disease or added to treatment regimens in patients with advanced Parkinson's disease to better control symptoms and reduce the need for additional Parkinson's disease The dosage of the drug. Safinamide mesylate is also known as safinamide mesylate, and its active ingredient, safinamide, is an α-aminoamide derivative, which is a highly selective, efficient and reversible third-generation amine oxidase B (MAO -B) Inhibitors can not only reduce the degradation of dopamine to control the concentration of dopamine in ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/482G01N30/32G01N30/30G01N30/7266G01N30/8679G01N2030/062G01N2030/484G01N2030/324G01N2030/3007
Inventor 董海峰杨俊免王亚静范燕龙徐黎明张龙梅李彤周雅洁荣孜杭
Owner HEBEI GUOLONG PHARMA CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com