Determination of LBPT in human plasma by high performance liquid chromatography-tandem mass spectrometry

J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Aug 15:965:238-43. doi: 10.1016/j.jchromb.2014.02.033. Epub 2014 Mar 18.

Abstract

A rapid and selective HPLC-MS/MS method was developed for the determination of LBPT in human plasma. The analyte was extracted from plasma samples by solid-phase extraction and then chromatographed on a C18 analytical column. The mobile phase consisted of acetonitrile-10mM ammonium formate in 0.1% formic acid (30:70, v/v) and the flow rate was 0.2 mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reactions monitoring (MRM) mode using positive electrospray ionization (ESI). The method was validated over the concentration range of 0.2-100 ng/mL. Inter- and intra-day precision (RSD %) were less than 9.2% and the accuracy (RE %) ranged from 0 to 11.0%. The lower limit of quantitation (LLOQ) was 0.2 ng/mL. The extraction recovery was on average 75% and the detection was not affected by the matrix. The method was successfully applied to the pharmacokinetic study of LBPT in healthy Chinese subjects.

Keywords: Chinese; HPLC–MS/MS; LBPT; Pharmacokinetics.

Publication types

  • Clinical Trial, Phase I
  • Randomized Controlled Trial
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Chromatography, High Pressure Liquid / methods*
  • Double-Blind Method
  • Drug Stability
  • Female
  • Humans
  • Linear Models
  • Male
  • Piperidines / blood*
  • Piperidines / chemistry
  • Piperidines / pharmacokinetics
  • Platelet Membrane Glycoproteins / antagonists & inhibitors*
  • Receptors, G-Protein-Coupled / antagonists & inhibitors*
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Tandem Mass Spectrometry / methods*

Substances

  • Piperidines
  • Platelet Membrane Glycoproteins
  • Receptors, G-Protein-Coupled
  • ethyl 1-(5-(4-chlorophenyl)-3-oxopent-4-enyl)piperidine-4-carboxylate
  • platelet activating factor receptor