Method for detecting genotoxic impurities 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 problems that the detection sensitivity cannot meet the content requirements and the like

Active Publication Date: 2021-09-14
HEBEI GUOLONG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

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  • Method for detecting genotoxic impurities in safinamide mesylate
  • Method for detecting genotoxic impurities in safinamide mesylate
  • Method for detecting genotoxic impurities in safinamide mesylate

Examples

Experimental program
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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]

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Abstract

The invention relates to the technical field of pharmaceutical analysis, and particularly discloses a method for detecting genotoxic impurities in safinamide mesylate. The detection method comprises the following steps: a test solution and a reference solution are prepared; and the test solution and the reference solution are detected by adopting a liquid chromatography-mass spectrometry method, and the chromatographic conditions of liquid chromatography are as follows: a C18 chromatographic column is adopted, a formic acid aqueous solution with the volume concentration of 0.1% is taken as a mobile phase A, a methanol solution of formic acid with the volume concentration of 0.1% is taken as a mobile phase B, and gradient elution is performed; and the mass spectrum adopts an ESI ion source and a positive ion detection mode. The detection method provided by the invention has the advantages of being simple, convenient, stable, high in precision, good in reproducibility and the like, can be used for rapidly and accurately detecting the toxic impurities in the safinamide mesylate raw material medicine, and accords with 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

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Application Information

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Patent Type & Authority Applications(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
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