Quantification of Palbociclib in Spiked Human Plasma Using Liquid Chromatography- Electro Spray Ionization-tandem Mass Spectrophotometry- an Application to Pharmacokinetic Study

Abstract

Objectives: The present method was developed for the estimation of palbociclib in spiked human plasma using Liquid chromatographic mass spectroscopy.Methods: The liquid-liquid extraction method was adopted and chromatographic separation was performed on a waters symmetry shield, C18 (4.6mm id x 50 mm) analytical column using (methanol: ultrapure water, pH 4.2 in the volume ratio of 60:40) as mobile phase. Positive ion mode was selected to obtain the product m/z +447.5 (parent) → 380.3 (product) for palbociclib and m/z +434.5 (parent) → 322.7 (product) for internal standard.Results: Calibration curve was linear over the range of 3-600 ng/ml. The intra and interday accuracy with % nominal 95 → 98.4 %, precision %CV ≤ 2% in all quality control levels, The percentage extraction recovery (96.15 % → 98.34 %), demonstrated excellent matrix and analyte selectivity (% interference = 0), and satisfactory stability study results in all types (% nominal 93.91 % → 99.58 %). The pharmacokinetic parameters was studied in the rabbit model, and the area under the curve (AUC0-∞) for palbociclib was 2632 ± 6.98 hr.ng/ml. The elimination half-life (t1/2) is 11.3 ± 5.3 hr.Conclusion: Based on the experimental findings the current developed method was considered a novel validated bioanalytical method, and applied in rabbit blood samples for pharmacokinetic studies of marketed formulations.

Keywords: Palbociclib; Bioanalytical; Pharmacokinetic study; LCMS/MS; method development