کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1222307 1494668 2012 8 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Identification, characterization and quantification of a new impurity in deferasirox active pharmaceutical ingredient by LC–ESI–QT/MS/MS
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
Identification, characterization and quantification of a new impurity in deferasirox active pharmaceutical ingredient by LC–ESI–QT/MS/MS
چکیده انگلیسی

An unknown impurity was detected in deferasirox drug substance by a newly developed high performance liquid chromatography (HPLC) method. The unknown impurity was identified by liquid chromatography–tandem mass spectrometry using electrospray ionization source and Q-trap mass analyzer (LC–ESI–QT/MS/MS). Based on LC–MS/MS data and knowledge of the synthetic scheme of deferasirox, this impurity was proposed as the regio-isomer of deferasirox. Structural confirmation of this impurity was unambiguously carried out by synthesis followed by characterization using nuclear magnetic resonance (NMR), infrared spectroscopy (IR), mass spectrometry, elemental analysis (EA) and the impurity was confirmed as 2-[3,5-bis(2-hydroxy-phenyl)-[1,2,4]-triazol-1-yl]-benzoic acid (Imp-1). The newly developed method was validated according to ICH guidelines. The resolution between Imp-1 and deferasirox was found to be more than 6.0 and the detection limit of impurities was in the range of 0.0005–0.01%, indicating high selectivity and sensitivity of the newly developed method.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Pharmaceutical and Biomedical Analysis - Volume 63, 7 April 2012, Pages 112–119
نویسندگان
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