Journal : Acta Chromatographica
Article : Forced degradation study and validated stability-indicating RP-LC method for determination of nilotinib in bulk and capsules

Authors :
Kuc, J.
Cracow University of Technology Department of Chemical Engineering and Technology, Department of Analytical Chemistry Warszawska 24 31-155 Cracow Poland, jkuc@chemia.pk.edu.pl,
Grochowalski, A.
Cracow University of Technology Department of Chemical Engineering and Technology, Department of Analytical Chemistry Warszawska 24 31-155 Cracow Poland,
Mach, S.
Institute of Public Health Ostrava Centre of Hygienic Laboratories Dobrá 240 739 51 Frýdek-Místek Czech Republic,
Placha, D.
VŠB-Technical University of Ostrava Centrum Nanotechnology 17 Listopadu 15/2172 708 33 Ostrava Czech Republic,
Furusawa, N.
Osaka City University Graduate School of Human Life Science Osaka 558-8585 Japan,
Stoilova, N.
Bulgarian Food Safety Agency Central Laboratory of Veterinary Control and Ecology (CLVCE) 5 “Iskarsko shousse” str., 1528 Sofia Bulgaria, nadqstoilova@abv.bg,
Surleva, A.
University of Chemical Technology and Metallurgy Analytical Chemistry Department 8 “St. Kl. Ohridski” blvd., 1756 Sofia Bulgaria,
Stoev, G.
Bulgarian Food Safety Agency Central Laboratory of Veterinary Control and Ecology (CLVCE) 5 “Iskarsko shousse” str., 1528 Sofia Bulgaria,
Popovic, N.
Lafayette College Department of Chemistry Easton PA USA,
Sherma, J.
Lafayette College Department of Chemistry Easton PA USA, shermaj@lafayette.edu,
Dixit, S.
Yeungnam University Department of Chemistry Gyeongsan 712-749 South Korea, drdixit.shuchi@gmail.com,
Dubey, R.
riturajdubey0@gmail.com,
Bhushan, R.
Indian Institute of Technology Roorkee Department of Chemistry Roorkee 247667 India, rbushfcy@iitr.ernet.in,
Fouad, M. A.
Cairo University Pharmaceutical Chemistry Department, Faculty of Pharmacy Kasr El-Aini St. Cairo 11562 Egypt, merro911@yahoo.com,
Elkady, E. F.
Cairo University Pharmaceutical Chemistry Department, Faculty of Pharmacy Kasr El-Aini St. Cairo 11562 Egypt,
Abstract : 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.

Keywords : nilotinib, reversed-phase liquid chromatography, stability-indicating assay, capsules, anticancer drugs,
Publishing house : University of Silesia in Katowice
Publication date : 2014
Number : Vol. 26, no. 4
Page : 637 – 647

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DOI :
Qute : Kuc, J. ,Grochowalski, A. ,Mach, S. ,Placha, D. ,Furusawa, N. ,Stoilova, N. ,Surleva, A. ,Stoev, G. ,Popovic, N. ,Sherma, J. ,Dixit, S. ,Dubey, R. ,Bhushan, R. ,Fouad, M. A. ,Elkady, E. F. ,Elkady, E. F. , Forced degradation study and validated stability-indicating RP-LC method for determination of nilotinib in bulk and capsules. Acta Chromatographica Vol. 26, no. 4/2014
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