Combined quantification of faecal sterols, stanols, stanones and bile acids in soils and terrestrial sediments by gas chromatography-mass spectrometry

Journal of Chromatography. a
Jago Jonathan BirkBruno Glaser

Abstract

Faeces incorporation can alter the concentration patterns of stanols, stanones, Δ(5)-sterols and bile acids in soils and terrestrial sediments. A joint quantification of these substances would give robust and specific information about the faecal input. Therefore, a method was developed for their purification and determination via gas chromatography-mass spectrometry (GC-MS) based on a total lipid extract (TLE) of soils and terrestrial sediments. Stanols, stanones, Δ(5)-steroles and bile acids were extracted by a single Soxhlet extraction yielding a TLE. The TLE was saponified with KOH in methanol. Sequential liquid-liquid extraction was applied to recover the biomarkers from the saponified extract and to separate the bile acids from the neutral stanoles, stanones and Δ(5)-steroles. The neutral fraction was directly purified using solid phase extraction (SPE) columns packed with 5% deactivated silica gel. The bile acids were methylated in dry HCl in methanol and purified on SPE columns packed with activated silica gel. A mixture of hexamethyldisilazane (HMDS), trimethylchlorosilane (TMCS) and pyridine was used to silylate the hydroxyl groups of the stanols and Δ(5)-sterols avoiding a silylation of the keto groups of the stanone...Continue Reading

Citations

Dec 6, 2012·Analytical Chemistry·Katherine E GregoryBruce S Kristal
Sep 8, 2015·Analytical and Bioanalytical Chemistry·Dario BattistelCarlo Barbante
Feb 13, 2014·Rapid Communications in Mass Spectrometry : RCM·Michaela A DippoldBruno Glaser
Jan 16, 2015·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Huiyong WangWeiming Li
Jul 14, 2016·Environmental Science & Technology·Wenhan ChengJules M Blais
Feb 6, 2019·Rapid Communications in Mass Spectrometry : RCM·Kyle Mason-JonesMichaela A Dippold
May 25, 2018·Lipids in Health and Disease·Yanan LiuDong Liu
Apr 27, 2018·Proceedings. Biological Sciences·Kathryn E HarganJules M Blais
Nov 13, 2013·Analytical Chemistry·Min LiHuwei Liu

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