Simultaneous quantitation of rosuvastatin and gemfibrozil in human plasma by high-performance liquid chromatography and its application to a pharmacokinetic study

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 x 150 mm, 5.0 microm). 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 microg/mL, respectively. Linearity was excellent (r(2) = 0.999) in the 0.03-10 microg/mL and 0.3-100 microg/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 microg/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 microg/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.

Liquid chromatography/negative ion electrospray tandem mass spectrometry method for the quantification of rosuvastatin in human plasma: Application to a pharmacokinetic study

“…In recent years, several methods including HPLC-UV [9,10] and LC-MS/MS [11][12][13][14] have been reported for the quantification of rosuvastatin in plasma. Most of the published LC-MS/MS methods [11][12][13][14] were based on positive electrospray detection, which provided a sensitivity at LLOQ of ≥0.1 ng/ml, using a plasma sample volume of 0.25-1.7 ml.…”

Lc Determination of Rosuvastatin and Ezetimibe in Human Plasma

“…Rosuvastatin is very effective in reducing low density lipoprotein cholesterol [5] and many studies have demonstrated its efficacy greater than other drugs of its class such as atorvastatin, simvastatin and pravastatin [5][6][7]. During literature review many methods were found reporting separation of rosuvastatin like capillary zone electrophoresis [8], Spectrophotometry [9][10] and HPLC [11][12][13][14].…”

“…Rosuvastatin is very effective in reducing low density lipoprotein cholesterol [5] and many studies have demonstrated its efficacy greater than other drugs of its class such as atorvastatin, simvastatin and pravastatin [5][6][7]. During literature review many methods were found reporting separation of rosuvastatin like capillary zone electrophoresis [8], Spectrophotometry [9-10] and HPLC [11][12][13][14].formulations.We are currently engaged in the development of simple HPLC methods for the determination of binary combinations of different classes of drugs including antihyperlipidemic drugs [21,22,[36][37][38][39][40][41][42][43][44][45][46]. The present work was therefore planned to develop a simple HPLC method to determine rosuvastatin and ezetimibe simultaneously in human plasma.…”

Simultaneous determination of timolol maleate, rosuvastatin calcium and diclofenac sodium in pharmaceuticals and physiological fluids using HPLC-UV

“…Various analytical methods have been reported for the determination of RST including, spectrophotometric and HPLC-UV [13,14]. The simultaneous quantification of RST with gemfebrozil in human plasma [15], and with other statins in pharmaceutical preparations has been reported [16]. The simultaneous analysis of RST and atorvastatin in human plasma using HPLC-UV has been reported [14].…”