Journal: Journal of Pharmacy Research

Article Id: JPRS-PC-0000212
Title: Structural Elucidation of Potential Impurities of Raloxifene Hydrochloride by LC/ESI-MS and NMR#
Category: Pharmaceutical Chemistry
Section: Research Article
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    Three impurities were detected during the impurity profile study of raloxifene hydrochloride by reverse phase gradient high performance liquid chromatographic method (HPLC) whose area percentage ranged from 0.06 to 0.15%. The product ion spectrum of these impurities and Raloxifene was recorded in LCMS and the fragmentation patterns of these impurities were observed and these three impurities displayed identical molecular ion at m/z 488. A thorough study was undertaken to characterize these impurities. They were isolated from enriched mother liquors by preparative HPLC. Based on the spectral data (1H,13C NMR, 1D NOE, 2D NMR and Mass), the structure of these impurities 1-3 were characterized as 1-(2-(4-(6-hydroxy-2-(4-hydroxyphenyl)benzo[b]thiophene-3 carbonyl) phenoxy) ethyl)-1-methylpiperidin-1-ium (Impurity-1), [6-Hydroxy-2-(4-methoxy phenyl)-benzo[b]thiophen-3-yl]-[4-(2-piperidin-1-yl-ethoxy) phenyl]-methanone (Impurity-2) and [2-(4-hydroxy-phenyl)-6-methoxy-benzo[b]thiophen-3-yl]-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-methanone (Impurity-3).

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    Author(s) Name:

    N. Jagadeesh*,a, b, Y. Ravindra Kumara, A. Jayashreeb and Sandeep Mohantya

    Affiliation(s) Name:

    aDr. Reddy’s Laboratories Ltd., Hyderabad 500 072, A.P., India
    bCentre for chemical sciences & Technology, Institute of Science and Technology,Jawaharlal Nehru Technological University, Kukatpally, Hyderabad 500 072, A.P., India

    *Corresponding author.
    N Jagadeesh
    Scientist,
    Analytical Research & Development
    Dr Reddy’s Laboratories Ltd.,
    Hyderabad-500072, AP., India
    Received on:21-03-2014; Revised on: 08-04-2014; Accepted on:11-05-2014

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    Author:

    N. Jagadeesh*,a, b, Y. Ravindra Kumara, A. Jayashreeb and Sandeep Mohantya

    Title:Structural Elucidation of Potential Impurities of Raloxifene Hydrochloride by LC/ESI-MS and NMR#
    Journal:Journal of Pharmacy Research
    Vol(issue):8 (June)
    Year:2014
    Page No: (718-727)
  • Experimental Methods Keywords

    Methodology:LC/ESI-MS and NMR#
    Research Materials:Raloxifene Hydrochloride

Keywords

Raloxifene; Preparative Isolation; NMR; Liquid chromatography-mass spectrometry; Characterization

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