Method for simultaneously determining contents of three impurities in tadalafil

• Main Authors: YANG HAIQING, ZHOU XIANG, LAI CANLIN, WANG TIANYING, LV LILI, PING XIATING, HU LINSHUI, WU JIAN
• Format: Patent
• Language: Chinese; English
• Published: 14.10.2022
• Subjects: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIRCHEMICAL OR PHYSICAL PROPERTIES; MEASURING; PHYSICS; TESTING

The invention provides a method for simultaneously determining the content of three impurities in tadalafil, and particularly relates to a method for simultaneously qualitatively and quantitatively detecting chloroacetyl chloride, (1R, 3R)-1-(1, 3-benzodioxolane-5-yl)-2-(chloracetyl)-2, 3, 4, 9-tetrahydro-1H-pyridino [3, 4-B] indole-3-carboxylic acid methyl ester and an isomer thereof in tadalafil by adopting high performance liquid chromatography tandem mass spectrometry. The method comprises the following specific steps: adding an acetonitrile solution of an amino compound into a tadalafil test sample for derivatization to prepare a test sample solution; the three impurities are subjected to same derivatization and diluted into standard solutions with different concentrations, and a high performance liquid chromatography-tandem mass spectrometry standard curve is obtained; the test solution is subjected to high performance liquid chromatography tandem mass spectrometry detection to obtain characteristic ion