Synthesis and characterization of oxitropium bromide related substances and novel stability indicating HPLC methods

Publication date: Available online 5 February 2020Source: Journal of Pharmaceutical and Biomedical AnalysisAuthor(s): Esen Bellur Atici, Çağan Ağtaş, Yücel Yazar, Nurten RıdvanoğluAbstractThe European Pharmacopoeia (Ph. Eur.) described two separate HPLC methods for determination of organic impurities in oxitropium bromide, a synthetic anticholinergic agent used by inhalation in the treatment of asthma and other bronchial disorders, and a potentiometric titration assay method which is not a stability indicating method. During synthetic process development and analytical studies of oxitropium; besides known Ph. Eur.-impurities new process related and degradation impurities were determined, identified by LC-MS, synthesized, characterized, and then used in development and validation studies of oxitropium analytical methods. As a result of these studies, a single HPLC related substances method was developed and validated according to international conference on harmonisation (ICH) guidelines for determination of all oxitropium related substances by using an inertsil ODS-4 (250 mm × 4.6 mm, 5 µm) column at 15 °C with 50 µL injection volume at a wavelength of 210 nm with gradient elution of phosphate-buffer/acetonitrile mixture flowing at a rate of 1.2 mL/min during 60 min. Also, a stability indicating HPLC assay method was developed and validated by using an XBridge C18 (150 mm × 4.6 mm, 3.5 μm) column at 25 °C with 10 µL injection v...
Source: Journal of Pharmaceutical and Biomedical Analysis - Category: Drugs & Pharmacology Source Type: research