Simultaneous Determination of PUFA-derived Pro-Resolving Metabolites and Pathway Markers Using Chiral Chromatography and Tandem Mass Spectrometry

Anal Chim Acta. 2018 Nov 15;1031:185-194. doi: 10.1016/j.aca.2018.05.020. Epub 2018 May 8.

Abstract

Lipid mediators play an important role as biological messengers involved in inflammatory processes. Deriving from different polyunsaturated fatty acids, endogenously built mediators featuring both pro- and anti-inflammatory properties as well as pro-resolving lipid mediators and their biological precursors have been investigated. A newly developed method using chiral chromatography-tandem mass spectrometry on human plasma has demonstrated its suitability for the simultaneous determination of prostaglandins, lipoxins, D-series derived resolvins as well as protectins, maresin 1, leukotriene B4 and several precursors of them in order to yield information about metabolic pathways. Due to the matrix complexity, a solid phase extraction method using an octadecyl-modified silica gel cartridge was carried out. The developed method allows the determination of 34 analytes in 25 min showing enough selectivity as well as precision and accuracy (≤15% relative standard deviation, ≤15% relative error) in the calibration range of 0.1-10 ng mL-1 or 0.2-20 ng mL-1 depending on the analytes. Stability of the analytes in plasma has been demonstrated for at least 3 h at room temperature, 72 h in the autosampler and 60 days in the freezer at -80 °C. This method has been validated and shown its suitability for the determination of all studied analytes in human plasma samples.

Keywords: Chiral chromatography; LC-MS/MS; Resolution; Sensitivity; Specialized pro-resolving lipid mediators.

MeSH terms

  • Biomarkers / blood
  • Chromatography, High Pressure Liquid*
  • Fatty Acids, Unsaturated / blood*
  • Fatty Acids, Unsaturated / isolation & purification
  • Fatty Acids, Unsaturated / metabolism
  • Humans
  • Leukotriene B4 / blood
  • Limit of Detection
  • Prostaglandins / blood
  • Solid Phase Extraction
  • Stereoisomerism
  • Tandem Mass Spectrometry*

Substances

  • Biomarkers
  • Fatty Acids, Unsaturated
  • Prostaglandins
  • Leukotriene B4