Mass spectrometric profiling of saturated fatty acid esters of steroids separated by high-temperature gas chromatography

J Chromatogr A. 2009 Feb 27;1216(9):1463-8. doi: 10.1016/j.chroma.2008.12.059. Epub 2008 Dec 27.

Abstract

An efficient analytical method for simultaneous determination of 12 SFEs in serum is described. The method involves solid-phase extraction to isolate of SFEs from interfering species, especially cholesteryl esters, conversion to trimethylsilyl (TMS) ether derivatives for the direct analysis by gas chromatography-mass spectrometry (GC-MS) using a high temperature MXT-1 (Silcosteel-treated stainless steel) capillary column. All SFEs as their TMS derivatives were well separated with excellent peak shapes within 12 min. Overall recoveries ranged from 88% to 119%, with a detection limits for SFEs ranged from 2 to 30 microg L(-1). The linearity as correlation coefficient was higher than 0.99 except for pregnenolone-3-arachidate (r(2)=0.98) in the concentration range of 5-3000 microg L(-1). Ten serum samples obtained from volunteers were also analyzed and quantitatively determined of DHEA-3-palmitate and pregnenolone-3-stearate in 1.8-1195.8 microg L(-1) concentration. The devised high temperature GC-MS method could be useful for identification of SFEs in biological specimens including serum.

MeSH terms

  • Esters / analysis*
  • Esters / blood
  • Esters / chemical synthesis
  • Fatty Acids / analysis*
  • Gas Chromatography-Mass Spectrometry / methods*
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Solid Phase Extraction / methods
  • Steroids / analysis*
  • Temperature

Substances

  • Esters
  • Fatty Acids
  • Steroids