تطوير طريقة ذات مصدوقيه لتعيين شائبة 5-Amino 2-Methyl Benzoic Acid في مركب كاناغليفلوزين Canagliflozin باستعمال الاستشراب السائل بالنمط المدروج المزود بمكشاف طيف الكتلة

Abstract EN

In this research, 5-Amino 2-Methyl Benzoic Acid Impurity in Canagliflozin in active pharmaceutical ingredient (API) and the product are detected and identified.

5-Amino 2-Methyl Benzoic Acid is the moft important Parting material in Canagliflozin synthesis, but it is recommended to determine it and calculate the exposure rate according to ICH because it is genotoxic impurity.

The method was developed to separate Canagliflozin from 5-Amino 2-Methyl Benzoic Acid and this method was applied on the ftandard of Canagliflozin, the .active pharmaceutical ingredient and the product The work was done in parallel once by using UV detector at 290 nm wavelength and Mass Spectrometer and Electro-Spray Ionization (ESI) mode, using a mobile phase composed of water, and acetonitrile in a gradient mode, and ftationary phase Shim-pack XR- ODS II column (100 x 3.0mm, 2.2^m particle size) with a relatively short analysis time, where the impurity 5-Amino 2-Methyl Benzoic Acid was detected at time of 3.4 minutes and was found in each sample of the product Invokana, and in the ftandard and in the raw material but in a trace level.

The method was validated according to USP 38 guideline recommendations and .the ICH guidelines for validation too