Simultaneous quantitation of the BACE1 inhibitor AZD3293 and its metabolite AZ13569724 in human matrices by LC-MS/MS

Bioanalysis. 2017 May;9(10):813-826. doi: 10.4155/bio-2017-0003. Epub 2017 Apr 24.

Abstract

Aim: AZD3293 is a novel BACE1 inhibitor in Phase III development for Alzheimer's disease. Sensitive and robust bioanalytical methods were required to quantitate AZD3293 and its metabolite AZ13569724 in human biological matrices.

Methodology/results: Human plasma was prepared by protein precipitation. Linearity for both analytes was in the range of 0.5-500 ng/ml with up to 100-fold dilution. Plasma ultrafiltrate samples were prepared using Centrifree® ultrafiltration device. Urine and CSF samples were analyzed directly after dilution. A 27% decrease in AZD3293 concentrations in the CSF collection apparati was found due to nonspecific binding. Incurred sample reanalysis was acceptable.

Conclusion: Methods for simultaneous quantitation of AZD3293 and its metabolite AZ13569724 in human biological matrices have been validated and successfully applied to clinical studies.

Keywords: AZD3293; BACE1; LC–MS/MS; PUF; cerebrospinal fluid; plasma; urine.

MeSH terms

  • Amyloid Precursor Protein Secretases / antagonists & inhibitors*
  • Aspartic Acid Endopeptidases / antagonists & inhibitors*
  • Blood Chemical Analysis / methods*
  • Chromatography, Liquid / methods*
  • Enzyme Inhibitors / blood
  • Enzyme Inhibitors / metabolism
  • Enzyme Inhibitors / pharmacology
  • Humans
  • Imidazoles / blood*
  • Imidazoles / metabolism*
  • Imidazoles / pharmacology
  • Limit of Detection
  • Spiro Compounds / blood*
  • Spiro Compounds / metabolism*
  • Spiro Compounds / pharmacology
  • Tandem Mass Spectrometry / methods*
  • Time Factors

Substances

  • Enzyme Inhibitors
  • Imidazoles
  • Spiro Compounds
  • Amyloid Precursor Protein Secretases
  • Aspartic Acid Endopeptidases
  • BACE1 protein, human
  • lanabecestat