Detection method of p-methoxypropiophenone related substances

A technology of p-methoxybenzene and p-methoxybenzaldehyde, which is applied in the field of chemical analysis, can solve problems such as lack of effective detection, and achieve the effect of improving product quality, high practical value, and good reproducibility

Active Publication Date: 2022-08-05
SHIJIAZHUANG NO 4 PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the technical problem of lack of effective detection of related substances in p-methoxypropiophenone in the prior art, the invention provides a kind of related substances of p-methoxypropiophenone detection method

Method used

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  • Detection method of p-methoxypropiophenone related substances
  • Detection method of p-methoxypropiophenone related substances
  • Detection method of p-methoxypropiophenone related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1.1 Preparation of solution:

[0042] Blank solvent: methanol.

[0043] Preparation of mixed reference stock solution: take p-methoxybenzaldehyde, methyl 2-chloropropionate, 4-methoxy-3-methylpropiophenone, 2-methoxypropiophenone, 3-methoxypropiophenone Appropriate amount of Propiophenone reference substance, accurately weighed, quantitatively diluted with methanol to prepare approximately p-methoxybenzaldehyde, 2-chloropropionate methyl ester, 4-methoxy-3-methyl propiophenone, 2 -Methoxypropiophenone, 3-methoxypropiophenone solution of 200 μg each, as a mixed reference stock solution.

[0044] Mixed reference substance solution: Take the mixed reference substance stock solution prepared above, and quantitatively dilute it with methanol to prepare approximately p-methoxybenzaldehyde, methyl 2-chloropropionate, 4-methoxy-3-methyl-4-methoxybenzaldehyde in 1 mL. Propiophenone, 2-methoxypropiophenone, and 3-methoxypropiophenone each had a solution of 20 μg as a mixed refe...

Embodiment 2

[0057] Methodological validation:

[0058] 2.1 Exclusivity

[0059] Take the blank solvent, the above-mentioned mixed reference solution and the standard solution for testing according to the above-mentioned gas chromatographic conditions, and record the chromatogram. The results are as follows: Figure 1-Figure 3 shown, where, figure 1 is the chromatogram of the blank solvent, figure 2 is the chromatogram of the mixed reference solution, image 3 For the chromatogram of the spiked test solution. The test results of the separation degree of each component are shown in Table 1-Table 2.

[0060] Table 1 Test results of the separation degree of each component in the mixed control solution

[0061] Element degree of separation methanol - Methyl 2-chloropropionate 14.78 p-Methoxybenzaldehyde 115.26 2-Methoxypropiophenone 25.85 3-Methoxypropiophenone 19.77 4-Methoxy-3-methylpropiophenone 18.56

[0062] Table 2 The separation...

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Abstract

The invention relates to the technical field of chemical analysis, and particularly discloses a method for detecting p-methoxypropiophenone related substances. According to the method, ZB-1 (60m * 0.25 mm * 1.0 [mu] m) is adopted as a detection chromatographic column, the column temperature is set to be 38-42 DEG C and maintained for 2-10 min, then the temperature is increased to 170-190 DEG C at the rate of 38-42 DEG C/min and maintained for 30-40 min, the temperature of a sample inlet is 175-185 DEG C, the temperature of a detector is 245-255 DEG C, and the split ratio is (5-10): 1, so that simultaneous quantitative detection of various known impurities and unknown impurities in p-methoxypropiophenone is realized, and the detection accuracy is high. Compared with the prior art, the method has the advantages that the quality of the p-methoxypropiophenone can be truly reflected, the monitoring of the synthesis process of the p-methoxypropiophenone can be realized, the quality of the formoterol fumarate product can be improved, the medication risk can be reduced, and the practical value is high.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a detection method for p-methoxypropiophenone related substances. Background technique [0002] Formoterol fumarate, chemical name: (±)-N-[2-hydroxy-5-[(1RS)-hydroxy-2[[(1RS)-2-(4-methoxybenzyl)- 1-Methylethyl]amino]ethyl]phenyl]carboxamide fumarate dihydrate, a beta2-adrenoceptor agonist for the treatment of bronchial asthma, acute bronchitis or asthmatic bronchitis and other airway obstructive pulmonary disease. At present, the Chinese asthma prevention and treatment guidelines, the American Thoracic Society (ATS) and the European Respiratory Society (ERS) have listed formoterol fumarate as the preferred long-acting β2-agonist as a bronchodilator for asthma control. [0003] p-methoxypropiophenone is an important starting material in the synthesis of formoterol fumarate. p-methoxypropiophenone is synthesized from p-methoxybenzaldehyde and methyl 2-chloropropionate. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/30G01N30/38G01N30/60
CPCG01N30/02G01N30/30G01N30/38G01N30/60G01N2030/3015G01N2030/3046
Inventor 张旭宗莹莹祝春英马明卓杨俊免毕贺骆会茹韩倩茹王亚静相雅婷
Owner SHIJIAZHUANG NO 4 PHARMA
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