DETERMINATION OF PALBOCICLIB IN HUMAN PLASMA USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY – ULTRAVIOLET DETECTIONAbstract
A simple, sensitive, and high-performance liquid chromatography ultraviolet detection (HPLC-UV) method was developed and validated for the quantification of palbociclib in human plasma. Plasma samples were processed by solid phase extraction using an Oasis hydrophilic-lipophilic balance extraction cartridge (1 mL, 30 mg). Commercial imatinib was used as an internal standard. Palbociclib and imatinib (IS) in human plasma were analyzed using a mobile phase of acetonitrile and 0.1% Triethylamine TEA (pH 3.3; adjusted with 50% Ortho-phosphoric acid) (70:30, v/v), on a Agilent Zorbax C18 column (150 × 4.6 mm i.d., 5 µm) using isocratic elution at a flow rate of 1.0 mL/min with ultraviolet detection at 266 nm. The method was validated over a concentration range of 0.1-3.0 µg/mL (r2 ≥ 0.998) with coefficient of variation for intraday precision of 3.92%, 3.56% and 2.28% for 0.5, 1.5, and 2.5 µg/mL respectively. The lower limit of detection was 50 ng/mL. The extraction recovery rates for palbociclib ranged from 66.69% to 80.97%. The intra- and inter-day precision was below 5.0%, and the accuracy ranged from 89.40 – 112% over the linear range. No notable matrix effects were observed. The proposed RP-HPLC method was successfully applicable for clinical therapeutic drug monitoring programs and found suitable application in design pharmacokinetic studies.
R. B. Nalanda, A. S. Rao * and D. Gowri Sankar
Department of Pharmaceutical Analysis and Quality Assurance, Shri Vishnu College of Pharmacy, Vishnupur, Bhimavaram, West Godavari, Andhra Pradesh, India.
17 December, 2017
21 February, 2018
04 March, 2018
01 September, 2018