Analysis of non‐derivatised bacteriohopanepolyols by ultrahigh‐performance liquid chromatography/tandem mass spectrometry

Abstract

UPLC/MS/MS analysis using an ACE Excel C18 column produced superior separation for amine-containing BHPs and reduced run times from 60 to 9 min compared with previous methods. Unexpected variations in fragmentation pathways between structural subgroups must be taken into account when optimising MRM transitions for future quantitative studies. Copyright © 2016 John Wiley & Sons, Ltd.

Biomarker evidence for the occurrence of anaerobic ammonium oxidation in the eastern Mediterranean Sea during Quaternary and Pliocene sapropel formation

“…BHT isomer can possibly be used to explore the role anammox may have played in these basin anoxic events. The residence time of BHT isomer in marine sediment records likely does not extend beyond the Early Cretaceous (van Dongen et al, 2006;Talbot et al, 2016a). However, BHT isomer can be applied to the Paleocene-Eocene Thermal Maximum (PETM; 55 Ma).…”

“…BHT and BHT isomer were baseline separated, and the MS 2 spectra of BHT and its isomer (Fig. S1) were comparable to spectra of non-derivatised BHT published by Talbot et al (2016b). MS performance was continuously monitored, and matrix effects were assessed using the PAF standard.…”

“…Samples were dissolved in MeOH : propan-2-ol (3 : 2; v : v) and filtered on 0.2 µm PTFE filters. BHT isomer was analysed by high-performance liquid chromatography coupled to positive ion atmospheric pressure chemical ionisation mass spectrometry (HPLC/APCI-MS), using a data-dependent (3 events) scan mode on a system equipped with an ion trap MS (Talbot et al, 2007;van Winden et al, 2012). Semi-quantification of BHT isomer was achieved at Newcastle University using a BHT standard gifted by Michel Rohmer.…”

“…in roughly equal amounts (Rush et al, 2014b). Notably, the synthesis of BHT isomer has also been seen in a few other non-anammox, nonmarine bacteria (van Winden et al, 2012;Rosa-Putra et al, 2001;Peiseler and Rohmer, 1992), and, therefore, some care should be taken when applying this lipid as a biomarker for anammox. However, anammox is the only known marine source of BHT isomer, and BHT isomer has been shown to correlate with ladderanes (Rush et al, 2014b) and metagenomic evidence for anammox bacteria (Matys et al, 2017) in modern oxygen-deficient marine settings.…”

Analytical and Computational Advances, Opportunities, and Challenges in Marine Organic Biogeochemistry in an Era of “Omics”

“…Core and intact archaeal isoprenoidal GDGTs can be now analyzed in a single run using reversed-phase chromatography (Zhu et al, 2013), while the analysis of core bacterial and archaeal GDGTs has been improved by the use of ethylene bridged hybrid (BEH) HILIC columns (Hopmans et al, 2016). The detection of BHPs has been improved by the analysis of non-derivatized compounds using either atmospheric pressure chemical ionization (APCI) (Talbot et al, 2016) or electrospray ionization (ESI) (Rush et al, 2019).…”