Application of GC–EI-MS for the identification and investigation of positional isomer in primaquine, an antimalarial drug

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• 作者：Vaijanath G. Dongre ; Pravin P. Karmuse ; M.M. Nimbalkar ; Dharmendra Singh and Ashok Kumar
• 关键词：GC– ; EI-MS ; Positional isomer ; Precursor
• 刊名：Journal of Pharmaceutical and Biomedical Analysis
• 出版年：2005
• 出版时间：2005
• 年：2005
• 卷：39
• 期：1-2
• 页码：111-116
• 全文大小：285 K

文摘

A major impurity associated with primaquine drug samples obtained from European Pharmacopoeia (EP) and other commercial sources was detected and identified using HPLC, photo diode array (PDA), LC–MS/MS and gas chromatograph–electron impact-mass spectrometer (GC–EI-MS). PDA and LC–ESI-MS/MS data provided an evidence for it being isomeric in nature. However, spectral data obtained from the newly developed GC–EI-MS method has been utilised for structural elucidation and found to be conclusive to characterize this impurity as positional isomer, i.e. 8-(4-amino-4-methylbutyl amino)-6 methoxyquinoline. The structure of this impurity has been confirmed by its synthesis. Precursor of primaquine was also investigated using GC–EI-MS. The data obtained confirmed the origin of isomeric impurity in precursor.