ABSTRACT
OBJECTIVE: To develop a sensitive and selective HPLC-UV method for the determination of Copen in rat plasma. METHODS: After a simple sample preparation procedure by one-step protein precipitation with acetonitrile, Copen and the internal standard paeonol were separated on a Symmetry(4.6 mm×150 mm, 5 μm) column with detection wavelength at 318 nm. The mobile phase consisted of acetonitrile-water containing 0.1% phosphoric acid (50:50). The flow rate was 1.0 mL·min at room temperature. RESULTS: The calibration curve was demonstrated to be linear over the concentration range of 0.101-20.2 μg·mL-1. The method had a lowest limit of quantification of 0.101 μg·mL-1. The extraction recoveries were in the range of 69.19% -77.19%. The intra-day and inter-day RSDs were below 5.20%. CONCLUSION: The method was proved to be convenient, sensitive, rapid and suitable for pharmacokinetic study. Copyright 2012 by the Chinese Pharmaceutical Association.
ABSTRACT
This study presents a rapid, specific and sensitive liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay for determination of risperidone (RIS) in human serum using paroxetine as an internal standard (IS). An Alltima-C18 column (2.1 mmx100 mm, 3 microm) and a mobile phase consisting of 0.1% formic acid-acetonitrile (40:60, v/v) were used for separation. The analysis was performed by selected reaction monitoring (SRM) method, and the peak area of the m/z 411.3-->191.1 transition for RIS was measured versus that of the m/z 330.1-->192.1 transition for IS to generate the standard curves. The assay linearity of RIS was confirmed over the range 0.25 approximately 50.00 ng/ml and the limit of quantitation was 0.05 ng/ml. The linear range corresponds well with the serum concentrations of the analytes obtained in clinical pharmacokinetic studies. Intraday and interday relative standard deviations were 1.85% approximately 9.09% and 1.56% approximately 4.38%, respectively. The recovery of RIS from serum was in the range of 70.20% approximately 84.50%. The method was successfully applied to investigate the bioequivalence between two kinds of tablets (test versus reference products) in 18 healthy male Chinese volunteers. The result suggests that two formulations are bioequivalent.
Subject(s)
Adolescent , Adult , Humans , Male , Antipsychotic Agents , Blood , Pharmacokinetics , Area Under Curve , China , Chromatography, High Pressure Liquid , Methods , Drug Stability , Mass Spectrometry , Methods , Reference Standards , Reproducibility of Results , Risperidone , Blood , Pharmacokinetics , Time FactorsABSTRACT
<p><b>OBJECTIVE</b>To study the determination of desloratadine in human serum and its pharmacokinetics in healthy volunteers.</p><p><b>METHODS</b>A single oral dose of 10 mg desloratadine was given to 18 healthy volunteers. The serum concentrations of desloratadine were determined by HPLC-MS assay. The pharmacokinetics parameters of desloratadine tablets were calculated with program 3P97.</p><p><b>RESULT</b>The main pharmacokinetics parameters of desloratadine tablets were as followsút(max)(1.611 +/-0.366)h, C(max) (4.455+/-1.990)microg x L(-1), AUC(0-t) (58.50+/-21.34)microg x L(-1) x h(-1), AUC(0-infinity) (60.59+/-22.32)microg x L(-1) x h(-1), t(1/2(ke)) (20.303+/-5.833)h, Ke (0.0372+/-0.0116)h(-1) and CL(0.1838+/-0.0563)L x h(-1).</p><p><b>CONCLUSION</b>Desloratadine tablet is absorbed quicker in the 18 healthy volunteers than the reports and its peak blood concentration reached at 1.5 h after oral administration with t(1/2) 20 h.</p>