Author/Authors :
Karagiannidou، Evrykleia G. نويسنده Research & Development Department, Pharmathen Industrial S.A., API Operations Unit, Building Thermi 1, 9th km Thessaloniki – Thermi, P.O. Box 60499, GR 570 01, Thessaloniki, Greece. , , Panagiotidis، Elli Vastardi Theodoros نويسنده Pharmathen, API Operations Unit, Building Thermi 1, 9th km Thessaloniki – Thermi, P.O. Box 60499, GR 570 01, Thessaloniki, Greece. , , Tsatsas، Theodoros نويسنده Pharmathen, API Operations Unit, Building Thermi 1, 9th km Thessaloniki – Thermi, P.O. Box 60499, GR 570 01, Thessaloniki, Greece. , , Neokosmidis، Efstratios نويسنده Pharmathen, API Operations Unit, Building Thermi 1, 9th km Thessaloniki – Thermi, P.O. Box 60499, GR 570 01, Thessaloniki, Greece. ,
Abstract :
The characterization of process related impurities associated with the synthesis of Duloxetine HCl active pharmaceutical ingredient was performed. This paper discusses the structure elucidation of Duloxetine HCl and its impurities on the basis of 1H-NMR, 13C-NMR, IR, Mass Spectroscopy and High Resolution Mass Spectroscopy. The polymorph of Duloxetine hydrochloride API was characterized with X-Ray Powder Diffraction analysis, Differential Scanning Calorimetry and Hot Stage Polarizing Optical Microscopy. A selective and stability indicating reversed phase high performance liquid chromatographic method (RP-HPLC) with PDA detector was developed for the purity determination of Duloxetine hydrochloride Active Pharmaceutical Ingredient in the presence of its ten process related impurities. Chromatography was carried out on a Symmetry C18 (250*4.6mm, 5?m) column, using a gradient elution of A: buffer/methanol / acetonitrile (35:52:13v/v/v) and B: methanol/ acetonitrile (80:20v/v) at a flow rate of 1.0ml/min.
