Plasma Lysosphingolipid Biomarker Measurement by Liquid Chromatography Tandem Mass Spectrometry

Methods Mol Biol. 2022:2546:271-284. doi: 10.1007/978-1-0716-2565-1_25.

Abstract

Plasma lysosphingolipids are highly elevated in patients with Gaucher, Krabbe, Fabry, and Niemann-Pick diseases and tend to accumulate to a greater extent than their respective primary sphingolipids in the plasma of affected patients. In this chapter, we describe two liquid chromatography tandem mass spectrometry (LC-MS/MS) methods to measure plasma concentrations of four lysosphingolipids species. The first method described measures glucosylsphingosine (lyso-GL1) and galactosylsphingosine (psychosine), biomarkers that accumulate in Gaucher and Krabbe diseases, respectively. The second method measures globotriaosylsphingosine (lyso-Gb3) and sphingosylphosphorylcholine (lyso-SPM), biomarkers for Fabry and Niemann-Pick diseases, respectively. Each method utilizes isotope-labeled internal standards and multipoint calibration curves to quantify the analytes of interest. Briefly, plasma samples are mixed with five volumes of LC-MS grade methanol containing internal standard, and protein is removed via centrifugation. Supernatant is dried and resuspended in initial mobile phase. Samples are separated by liquid chromatography using either a BEH amide column (lyso-GL1 + psychosine) or a C18 column (lyso-Gb3 + lyso-SPM). Protonated analytes are measured by selected reaction monitoring (SRM) in positive electrospray ionization mode. Using these methods, we have observed elevations of these lyso- species in Gaucher, Fabry, and Niemann-Pick and successfully distinguished different subtypes reflecting the disease severity.

Keywords: Fabry disease; Galactosylsphingosine (psychosine); Gaucher disease; Globotriaosylsphingosine (lyso-Gb3); Glucosylsphingosine (lyso-GL1); Krabbe disease; Liquid chromatography; Mass spectrometry; Niemann–Pick disease; Sphingosylphosphorylcholine (lyso-SPM).

MeSH terms

  • Amides
  • Biomarkers
  • Chromatography, Liquid / methods
  • Fabry Disease*
  • Humans
  • Methanol
  • Niemann-Pick Diseases*
  • Psychosine
  • Sphingolipids / chemistry
  • Tandem Mass Spectrometry / methods

Substances

  • Amides
  • Biomarkers
  • Sphingolipids
  • Psychosine
  • Methanol