title: A validated stability-indicative UPLC method for nilotinib hydrochloride for the determination of process-related and degradation impurities.
abstract: A novel stability-indicating ultra performance liquid chromatographic (UPLC) method has been developed for quantitative determination of nilotinib hydrochloride in active pharmaceutical ingredients along with four impurities (imp-1, imp-2, imp-3 and imp-4). The method is applicable to the quantification of related compounds and assay of nilotinib hydrochloride drug. Efficient chromatographic separation was achieved on a Shim-pack XR-ODS II, 75 × 3.0 mm, 1.8-µm column with a gradient mobile phase combination. Quantification was carried at 260 nm at a flow rate of 0.6 mL min(-1). Stress degradation conditions were established for nilotinib hydrochloride by subjecting it to acid, base, oxidation, humidity, thermal and photolysis. The stress samples were assayed against a qualified reference standard and the mass balance was found close to 97.0%. The developed UPLC method was validated according to the present International Conference on Harmonisation guidelines for specificity, detection limit, quantitation limit, linearity, accuracy, precision, intermediate precision and robustness. The resolution between nilotinib hydrochloride and four potential impurities is found to be >2.0. Regression analysis shows as r value (correlation coefficient) of >0.999 for nilotinib hydrochloride and four potential impurities.
authors.affiliation: Department of Chemistry, Sri Krishna Devaraya University, Anantapur 515003, India.
authors.forename: Sudhakar Babu
authors.initials: SB
authors.lastname: Kondra
authors.affiliation: Department of Chemistry, Sri Krishna Devaraya University, Anantapur 515003, India Hetero Labs Limited, Hetero House, Sanathnagar, Hyderabad 500078, India venky75@gmail.com.
authors.forename: Venkataramanna
authors.initials: V
authors.lastname: Madireddy
authors.affiliation: Department of Chemistry, Sri Krishna Devaraya University, Anantapur 515003, India Hetero Labs Limited, Hetero House, Sanathnagar, Hyderabad 500078, India.
authors.forename: Mohanareddy
authors.initials: M
authors.lastname: Chilukuri
authors.affiliation: Hetero Labs Limited, Hetero House, Sanathnagar, Hyderabad 500078, India.
authors.forename: Narayanareddy
authors.initials: N
authors.lastname: Papadasu
authors.affiliation: Faculty in Biotechnology, Sri Krishna Devaraya University, Anantapur 515003, India.
authors.forename: Latha
authors.initials: L
authors.lastname: Jonnalagadda
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004355:Drug Stability; D011743:Pyrimidines / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results
chemical_list: D011743:Pyrimidines; C498826:nilotinib