Sci Pharm. 2008; 76: 653–661.
Spectral Characterization of Degradation Impurities of Paroxetine Hydrochloride Hemihydrate
Nirmala MUNIGELA 1, J. Moses BABU 1, Anjaneyulu YERRAMILLI 3, Naveen Kumar KOLLA 2, Vyas KRISHNAMURTHY 1, Vijay Vittal MATHAD 2
1 Department of Analytical Research, Discovery Research, Dr. Reddy’s Laboratories, Bollaram Road, Miyapur, Hyderabad 500 049, India.
2 Research and development, Dr. Reddy’s Laboratories Ltd., Integrated Product Development, Unit-III, Plot No.116, S.V. Co-Op.Indl. Estate, Bollaram, Jinnaram, Medak-502 325, India.
3 Jawaharlal Nehru Technological University, Kukatpally, Hyderabad-500 072, India.
* Corresponding author. E-mail: nirmalam@drreddys.com (N. Munigela)
Abstract
Two unknown impurities were detected in stressed samples (by hydrochloric acid and hydrogen peroxide) of paroxetine hydrochloride hemihydrate (an active pharmaceutical ingredient – API) using a gradient reversed-phase high performance liquid chromatography (HPLC). These impurities were enriched and were present up to 30% in the degraded sample. The impurities were isolated from the degraded sample by column purification. Spectral data of the isolated impurities were collected. Based on the spectral data of two dimensional nuclear magnetic spectroscopy (2D-NMR) and mass spectrometry (MS) Impurity-1 and Impurity-2 were characterized as (3S,4R)-3-{[(6-chloro-1,3-benzodioxol-5-yl)oxy]methyl}-4-(4-fluorophenyl)piperidine and [(3S,4R)-4-(4-fluorophenyl)piperidin-3-yl]methanol respectively.
Keywords
Paroxetine •·Degradation·• NMR·• HPLC •·LC-MS
Received August 10th, 2008 | Accepted September 14th, 2008 | Published Online September 23rd, 2008
