Comprehensive GC–MS analysis of fatty acids and sterols using sequential one-pot silylation: quantification and isotopologue analysis

D. Kloos, E Gay, H. Lingeman, F. Bracher, C. Müller, O.A. Mayboroda, A.M. Deelder, W.M.A. Niessen, M. Giera

Research output: Contribution to JournalArticleAcademicpeer-review

Abstract

RATIONALEFatty acids and sterol lipids play crucial roles in several biological processes and several biological facts underline the interconnection between these lipid classes. Therefore, it is of interest to develop a comprehensive method analysing both classes in the form of their most favourable derivatives suitable for quantification and isotopologue analysis. METHODSLipids were derivatised by a sequential one-pot procedure using N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide (MtBSTFA) and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA). No clean-up or concentration steps were necessary. The prepared samples were directly available for gas chromatography-electron ionisation mass spectrometric (GC-EI-MS) analysis on a standard column. For quantification, the SIM mode was used and for isotopologue analysis scheduled scan mode was applied. RESULTSDevelopment of a sequential one-pot derivatisation for GC-EI-MS allowing comprehensive analysis of fatty acids and sterols as their most favourable derivatives. Validation carried out using human plasma, comparison with certified NIST plasma. LLOQ of usually 3.3 ng/mL achieved. Isotopologue analysis of 2-[
Original languageEnglish
Pages (from-to)1507-1504
JournalRCM. Rapid Communications in Mass Spectrometry
Volume28
DOIs
Publication statusPublished - 2014

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