فصل المصاوغات الشائبة و شوائب الإصطناع المرافقة اليدوكسابان Edoxaban باستعمال الاستشراب السائل مع مكشاف طيف الكتلة MS-LC

الملخص EN

Edoxaban is a novel anticoagulant drug acting as a direct and reversible inhibitor of the coagulation factor Xa.

The purpose of this work was to separate isomers & related production impurities of Edoxaban in active pharmaceutical ingredient (API), by Using LC-MS, then to validate these methods.

The analysis and detection were carried out by using UV detector at 291 nm, and by using Mass Spectrometer detector with Electro- Spray Ionization ESI, the column oven temperature was at 25°C.

The Edoxaban impurities were determined on a Shimadzu Shim-pack XR-ODS II column, with a mobile phase containing water and acetonitrile in gradient program at a flow rate of 0.15ml/min, and the Edoxaban Isomers were separated on CHIRALCEL OD-R column, with a mobile phase containing water and methanol in gradient program at a flow rate of 1.8ml/min.

The method was validated according to USP 35 guideline recommendations and to the ICH guidelines for validation.

The method is suitable for practical routine analysis of API.