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Method for detecting isomers in 4-(3-fluorobenzyloxy) benzaldehyde

A fluorobenzyloxy, detection method technology, applied in the field of analysis and detection, can solve the problems affecting the purity of safinamide mesylate, etc., and achieve the effect suitable for practical application and promotion, strong specificity, and good linear relationship

Active Publication Date: 2022-02-25
SHIJIAZHUANG NO 4 PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This isomer directly affects the follow-up reaction of synthesizing safinamide mesylate, and then affects the purity of safinamide mesylate

Method used

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  • Method for detecting isomers in 4-(3-fluorobenzyloxy) benzaldehyde
  • Method for detecting isomers in 4-(3-fluorobenzyloxy) benzaldehyde
  • Method for detecting isomers in 4-(3-fluorobenzyloxy) benzaldehyde

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Embodiment 1

[0038] The embodiment of the present application provides a method for detecting isomers in 4-(3-fluorobenzyloxy)benzaldehyde, the detection method comprising the following steps:

[0039] Step 1, preparing a blank solution, a reference substance solution and a spiked sample solution for the test;

[0040] Blank solution is acetonitrile solvent;

[0041] Preparation of reference substance solution: take 4-(4-fluorobenzyloxy)benzaldehyde reference substance and prepare a reference substance solution with a concentration of 8 μg / ml with acetonitrile solvent;

[0042] Preparation of the standard-added sample for the test solution: take the 4-(3-fluorobenzyloxy)benzaldehyde sample and the 4-(4-fluorobenzyloxy)benzaldehyde reference substance, and prepare the standard-added sample for the test with acetonitrile Solution, wherein the concentration of 4-(3-fluorobenzyloxy)benzaldehyde sample is 4mg / ml, and the concentration of 4-(4-fluorobenzyloxy)benzaldehyde reference substance is...

Embodiment 2

[0051] Embodiment 2 detection limit and quantitative limit

[0052] Limit of detection: the reference substance solution prepared in Example 1 is detected by gas chromatography, the specific conditions of gas chromatography are as described in Example 1, and the spectrogram is recorded. When the peak height is 3 times of the baseline noise, the limit of detection is obtained. The results are shown in Table 2.

[0053]Limit of quantitation: the reference substance solution prepared in Example 1 is detected by gas chromatography, the specific conditions of gas chromatography are as described in Example 1, and the spectrogram is recorded. When the peak height is 10 times of the baseline noise, the limit of quantification is obtained. The results are shown in Table 2.

[0054] Table 2 detection limit, limit of quantitation detection result

[0055]

[0056] According to the above method, prepare 6 parts of reference substance solution in parallel, then adopt gas chromatograph...

Embodiment 3

[0059] Embodiment 3 linear relationship

[0060] Accurately measure 4-(4-fluorobenzyloxy) benzaldehyde, dissolve and quantitatively dilute with acetonitrile to make a series of concentration solutions, and detect by gas chromatography, the gas chromatography conditions are specifically as shown in Example 1, record the spectrogram, Take concentration (μg / ml) as abscissa, take peak area as ordinate, draw standard curve, and calculate regression equation, the results are shown in Table 4 and Figure 4 . It can be seen from the results that 4-(4-fluorobenzyloxy)benzaldehyde has a good linear relationship within the concentration range of 1.64 μg / ml to 9.81 μg / ml.

[0061] Table 44-(4-fluorobenzyloxy)benzaldehyde linearity test results

[0062]

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Abstract

The invention relates to the technical field of analysis and detection, and particularly discloses a method for detecting isomers in 4-(3-fluorobenzyloxy) benzaldehyde. The detection method comprises the following steps: a test solution and a reference solution are prepared; the test solution and the reference substance solution are detected by adopting gas chromatography, and the chromatographic conditions of the gas chromatography are as follows: a stationary liquid of a chromatographic column is 2, 3-di-O-methyl-6-tert-butylsilyl modified beta cyclodextrin, a detector is a flame ionization detector, the temperature of the detector is 225-235 DEG C, the initial temperature is 48-52 DEG C, the temperature is raised to 175 DEG C to 185 DEG C at the temperature raising rate of 28 DEG C / min to 32 DEG C / min, the constant temperature is kept for 35 min, and the temperature of a sample inlet is 175 DEG C to 185 DEG C. the detection method provided by the invention has the advantages of strong specificity, high sensitivity and wide application prospect.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to a method for detecting isomers in 4-(3-fluorobenzyloxy)benzaldehyde. Background technique [0002] 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, which can be used as monotherapy in patients with early Parkinson's disease, or added to the treatment regimen of patients with advanced Parkinson's disease to better control symptoms and reduce the required dose of other Parkinson's disease drugs. [0003] 4-(3-fluorobenzyloxy)benzaldehyde with structural formula shown in formula I is an important intermediate for the synthesis of safinamide mesylate. In the process of synthesizing 4-(3-fluorobenzyloxy)benzaldehyde in the existing technology, its isomer 4-(4-fluorobenzyloxy)benzaldehy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679
Inventor 宗莹莹毕贺杨俊免马明卓陈碧楚孙朝利韩倩茹骆会茹王亚静马宏思耿玉王肖
Owner SHIJIAZHUANG NO 4 PHARMA
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