Determination of globotriaosylceramide in plasma and urine by mass spectrometry

Clin Chem Lab Med. 2010 Feb;48(2):189-98. doi: 10.1515/CCLM.2010.048.

Abstract

Background: Fabry disease is an X-chromosomally inherited lysosomal storage disorder leading to accumulation of glycosphingolipids, mainly globotriaosylceramide (ceramide-trihexoside, Gb3). Concentrations of Gb3 in plasma and urine have been used to diagnose Fabry disease and to monitor enzyme replacement therapy with recombinant alpha-galactosidase.

Methods: Gb3 was purified from plasma or urine by combined liquid extraction/protein precipitation and solid-phase extraction, and was detected by flow-injection analysis electrospray mass spectrometry (MS) using multi-reaction-monitoring. Calibration was performed via standard addition using C17-Gb3 as internal standard. The most abundant isoforms were monitored for calculation of total Gb3.

Results: A MS-based assay for quantification of Gb3 in plasma and urine was established and validated. Intra- and inter-assay coefficient of variation (CV) of the method were <or=12%. However, at low concentrations the CV was 16%. The linear range covers roughly two orders of magnitude, down to 0.54 mg/L in plasma and 0.07 mg/L in urine. Careful adjustment of tuning parameters was necessary to obtain identical isoform intensities and quantitative results on different mass spectrometers. Gb3 concentrations in healthy controls were <4 mg/L in EDTA-plasma and <10 microg/mmol creatinine in urine. Significantly increased Gb3 concentrations were found in plasma and urine from male and female patients with Fabry disease.

Conclusions: An improved MS protocol for Gb3 quantification has been developed, validated, and shown to be suitable for diagnosis and monitoring of Fabry patients.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Calibration
  • Chromatography, Liquid
  • Enzyme Replacement Therapy
  • Fabry Disease / blood
  • Fabry Disease / diagnosis
  • Fabry Disease / therapy
  • Fabry Disease / urine
  • Female
  • Humans
  • Lysosomal Storage Diseases / enzymology
  • Lysosomal Storage Diseases / genetics
  • Lysosomal Storage Diseases / metabolism
  • Lysosomal Storage Diseases / pathology
  • Male
  • Reference Standards
  • Solid Phase Extraction
  • Tandem Mass Spectrometry
  • Trihexosylceramides / blood*
  • Trihexosylceramides / urine*
  • alpha-Galactosidase / metabolism

Substances

  • Trihexosylceramides
  • globotriaosylceramide
  • alpha-Galactosidase