A simple, selective, and precise stability-indicating reversed-phase liquid chromatographic method was developed and validated for the determination of nilotinib. Nilotinib was subjected to acid and alkali hydrolysis, oxidation, thermal, and photo-degradation. The degradation products were well separated from the pure drug. The method was based on isocratic elution of nilotinib and its degradation products on reversed phase C18 column (100 mm × 4.6 mm, 3.5 μm) — Zorbax Eclipse Plus using a mobile phase consisting of 10 mM KH2PO4:acetonitrile (54.5:45.5%, v/v) at a flow rate of 1 mL min−1. Quantitation was achieved with UV detection at 265 nm. Linearity, accuracy and precision were found to be acceptable over the concentration range of 0.1–80 μg mL−1. The drug was found to be susceptible to acid and base hydrolysis but resistant to oxidation, dry heat degradation, and photodegradation. The proposed method was successfully applied to the determination of nilotinib in bulk and in its pharmaceutical preparation.
Authors:E.M. Yilmaz, Z. Aydoğmuş, and H.Y. Aboul-Enein
A precise and sensitive reversed phase high-performance thin-layer chromatography (RP-HPLC) method was developed for the determination of nilotinib (NTB) in spiked plasma, urine, and pharmaceutical capsule formulation. The method was based on derivatization NTB with 4-chloro-7-nitrobenzofurazan (NBD-Cl) in the borax buffer (pH 9). The method employs an isocratic elution using acetonitrile and 10 mM orthophosphoric acid (40:60 v/v) as a mobile phase and an C18 column (4.6 mm × 250 mm, 5 μm, Waters Symmetry), with a fluorescence detector (λex: 447 nm, λem: 530 nm). The method validation was performed with respect to linearity, recovery, accuracy, precision, and stability. The linear ranges were 100–600 ng mL−1 in standard solution, plasma, and urine. Correlation coefficients (r2) were higher than 0.9997 for all of the analytes, indicating good linear relationship. The percentage recovery was 87.89% for plasma, 95.35% for urine, and 96.07% for capsules.
tyrosine kinase inhibitors imatinib and nilotinib used in the treatment of
oncohematological diseases. [Az onkohematológiai betegségek kezelésében használt
tirozinkináz-gátló imatinib és nilotinib csonthatásainak
Authors:Jassó András, Bertha László, Gyökeres Tibor, Takács Imre Géza, and Bursics Attila
Ray , D Moreno , PW Manley , D Fabbro , E Hall-Meyers , L Catley , K Podar , AL Kung , JD Griffin : 2006 Effects of PKC412, nilotinib, and imatinib against GIST-associated PDGFRA mutants with differential imatinib sensitivity
” S. G. Newman , K. F. Jensen * Green Chemistry 2013 , 15 , 1456 – 1472 .
“The synthesis of Bcr-Abl inhibiting anticancer pharmaceutical agents imatinib, nilotinib and dasatinib” B. J. Deadman , M. D. Hopkin , I. R