Determination of oxatomide in human plasma by high‐performance liquid chromatography–electrospray ionization mass spectrometry

Abstract

A rapid, sensitive and specific high-performance liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method has been developed and validated for the determination of oxatomide in human plasma. Flunarizine hydrochloride was employed as the internal standard (IS). The analytes were chromatographically separated on a Shimadzu Shim-pack VP-ODS C18 column (250 x 2.0 mm i.d.) with a mobile phase consisting of methanol and aqueous ammonium acetate solution (10 mm, pH 4.0; 85:15, v/v). Detection was performed on a single quadrupole mass spectrometer using an electrospray ionization interface with the selected-ion monitoring (SIM) mode. The method showed excellent linearity (r = 0.9995) over the concentration range of 0.5-500 ng/mL with good accuracy and precision. The intra- and inter-batch precisions were within 10% relative standard deviation. The recoveries were more than 90%. The validated method was successfully applied to a preliminary pharmacokinetic study of oxatomide in Chinese healthy male volunteers.

In Vitro and In Vivo Evaluation of Oxatomide β-Cyclodextrin Inclusion Complex

“…Plasma samples were analyzed for oxatomide concentration by using a validated LC-MS assay [16] with some modifications. Briefly, LC-MS analysis was performed on an Agilent 1100 series LC/MSD chromatographic system (Agilent, USA) consisting of a water HPLC system equipped with an on-line solvent degasser, binary solvent delivery system, autosampler, and an Agilent technologies single quadrupole mass spectrometer with an electrospray ionization (ESI) interface.…”

Dodging matrix effects in liquid chromatography tandem mass spectrometric assays—compilation of key learnings and perspectives

“…Over the years, several researchers have proposed interesting views, ranging from the identification of matrix effects to possibly controlling or eliminating such matrix effects. This note summarizes the key learnings and opens up another important area for introspection.It is now customary for LC/MS/MS assays to evaluate the interference of the matrix as the key first step during the method development stage itself since this has a bearing on the scope of method development and validation procedures (Layek et al, 2008;Bharathi et al, 2008;She et al, 2008;Jung et al, 2007; Chakradhar et al, 2007). While it is a good practice to adhere to the basic principles of matrix effect evaluation (Hubert et al, 1999;Dams et al, 2003;Taylor, 2005;Chambers et al, 2007), it is equally important to develop a method without having to go through a rigorous sample preparation to suit the need of the day (i.e.…”