Premium
Simultaneous quantitation of rosuvastatin and gemfibrozil in human plasma by high‐performance liquid chromatography and its application to a pharmacokinetic study
Author(s) -
Vittal Shivva,
Shitut Nikhil R.,
Kumar Thammera Ranjit,
Vinu Me C. A.,
Mullangi Ramesh,
Srinivas Nuggehally R.
Publication year - 2006
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.692
Subject(s) - chromatography , chemistry , analyte , detection limit , calibration curve , analytical chemistry (journal) , acetonitrile , high performance liquid chromatography , extraction (chemistry) , ammonium acetate
Abstract A simple, sensitive and specific high‐performance liquid chromatography method is described for simultaneous determination of rosuvastatin (RST) and gemfibrozil (GFZ) in human plasma using celecoxib as an internal standard (IS). The assay procedure involved extraction of RST, GFZ and IS from plasma into acetonitrile. Following separation and evaporation of the organic layer the residue was reconstituted in the mobile phase and injected onto an X‐Terra C 18 column (4.6 × 150 mm, 5.0 µm). The chromatographic run time was less than 20 min using flow gradient (0.0–1.60 mL/min) with a mobile phase consisting of 0.01 M ammonium acetate:acetonitrile:methanol (50:40:10, v/v/v) and UV detection at 275 nm. Nominal retention times of RST, GFZ and IS were 6.7, 13.9 and 16.4 min, respectively. Absolute recovery of both analytes and IS was greater than 90%. The lower limit of quantification (LLOQ) of RST and GFZ was 0.03 and 0.30 µg/mL, respectively. Linearity was excellent ( r 2 = 0.999) in the 0.03–10 µg/mL and 0.3–100 µg/mL ranges for RST and GFZ, respectively. The inter‐ and intra‐day precisions in the measurement of RST quality control (QC) samples 0.03, 0.09, 2.50 and 8.00 µg/mL were in the range 2.37–9.78% relative standard deviation (RSD) and 0.92–10.08% RSD, respectively. Similarly, the inter‐ and intra‐day precisions in the measurement of GFZ quality control (QC) samples 0.30, 0.90, 25.0 and 80.0 µg/mL were in the ranges 2.79–6.27 and 0.96–9.69% RSD, respectively. Accuracies in the measurement of QC samples for RST and GFZ were in the range 85.43–107.23 and 84.98–102.35% respectively, of the nominal values. RST and GFZ were stable in the array of stability studies viz., bench‐top, auto‐sampler and freeze–thaw cycles. Stability of RST and GFZ was established for 1 month at −80C. The application of the assay in an oral pharmacokinetic study in rats co‐administered with RST and GFZ is described. Copyright © 2006 John Wiley & Sons, Ltd.