title: Validated stability indicating RP-HPLC for quantitation of nitazoxanide in presence of its alkaline degradation products and their characterization by HPLC-tandem mass spectrometry.
abstract: A simple and sensitive stability indicating HPLC method was developed and validated for quantitative determination of Nitazoxanide (NTZ), a new antiprotozoal drug, in presence of degradation products generated under forced alkaline hydrolysis. Chromatographic separation was achieved on Inertsil C8-3 column (150 × 4.6 mm i.d.) using a mobile phase composed of acetonitrile: 50 mM ammonium acetate buffer (50:50, v/v, pH 5.0 adjusted with acetic acid) at a flow rate of 1 mL/min. Quantification was achieved with UV detection at 298 nm based on relative peak area. The method was linear over the concentration range of 0.8-50 µg/mL (r = 0.9999) with a limit of detection and quantification 0.0410 and 0.1242 µg/mL, respectively. The developed method has the requisite accuracy, selectivity, sensitivity and precision to assay NTZ in presence of its degradation products either in bulk powder or in pharmaceutical formulations. The degradation products were then identified by HPLC-MS/MS analysis using an electrospray ionization source and an ion trap analyzer.
authors.affiliation: Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini Street, 11562 Cairo, Egypt mahahgazy@yahoo.com.
authors.forename: Maha
authors.initials: M
authors.lastname: Hegazy
authors.affiliation: Pharmaceutical Chemistry Department, Faculty of Pharmacy, Misr International University, KM 28 Cairo - Ismailia Road (Ahmed Orabi District), Cairo, Egypt.
authors.forename: Amira
authors.initials: A
authors.lastname: Kessiba
authors.affiliation: Pharmaceutical Chemistry Department, Faculty of Pharmacy, Misr International University, KM 28 Cairo - Ismailia Road (Ahmed Orabi District), Cairo, Egypt.
authors.forename: Ahmed Emad
authors.initials: AE
authors.lastname: El Gindy
authors.affiliation: Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini Street, 11562 Cairo, Egypt.
authors.forename: Mohamed
authors.initials: M
authors.lastname: Abdelkawy
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004355:Drug Stability; D006868:Hydrolysis; D057230:Limit of Detection; D009574:Nitro Compounds; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000295:instrumentation / Q000379:methods; D013607:Tablets / Q000032:analysis; D053719:Tandem Mass Spectrometry / Q000295:instrumentation / Q000379:methods*; D013844:Thiazoles / Q000032:analysis* / Q000737:chemistry
chemical_list: D000097:Acetonitriles; D009574:Nitro Compounds; D013607:Tablets; D013844:Thiazoles; C041747:nitazoxanide; C032159:acetonitrile