Sensitive and selective liquid chromatography-tandem mass spectrometry method for the determination of metoclopramide in human plasma: application to a bioequivalence study.

摘要

A simple, sensitive and rapid method has been developed and validated for determination of the metoclopramide (MCP) in 100 microL human plasma. The analytical procedure involves a liquid-liquid extraction method using tramadol as an internal standard (IS). Chromatographic separation was carried out on a HyPURITY ADVANCE column using a mobile phase consisting of acetonitrile and 10 mm ammonium acetate buffer in the ratio of 80:20 (v/v) at a flow rate of 0.3 mL/min. The total run time of analysis was 2.5 min and elution of MCP and IS occurred at 0.9 and 1.3 min, respectively. A linear response function was established for the range of concentrations 0.53-42.07 ng/mL (r > 0.99). The intra- and inter-day precision values for MCP met the acceptance as per FDA guidelines. MCP was stable in a battery of stability studies viz., bench-top, auto-sampler and freeze-thaw cycles. The developed assay method was successfully applied to an oral bioequivalence study in humans.