Methods in endogenous steroid profiling – A comparison of gas chromatography mass spectrometry (GC–MS) with supercritical fluid chromatography tandem mass spectrometry (SFC-MS/MS)

Teubel, Juliane; Wüst, Bernhard; Schipke, Carola G.; Peters, Oliver; Parr, Maria Kristina

doi:10.1016/j.chroma.2018.04.035

Cited by 46 publications

(27 citation statements)

References 33 publications

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“…Due to the SL structural diversity, analysis of SL in complex biological samples is not straightforward limiting the exploitation of SL diagnostic and prognostic value. In addition to this, researchers employ a variety of solid-phase extraction (SPE) (Fong et al, 2013;Sánchez-Guijo et al, 2015;Wang et al, 2018) or liquid-liquid extraction approaches (LLE) (Kongmanas et al, 2010;Lam et al, 2014;Mirzaian et al, 2015b;Sion et al, 2001;Yao et al, 2016), with various solvent systems, and ESI and MALDI ionisation techniques (Serna et al, 2015;Teubel et al, 2018;Wang et al, 2018) which makes comparison of results difficult because of the potential sample losses, the differences in extraction performances and the ionization efficiencies associated with the different approaches (Lee et al, 2014;Pizarro et al, 2013;Reis et al, 2013;Sarafian et al, 2014).…”

Section: Introductionmentioning

confidence: 99%

Sulfate-based lipids: Analysis of healthy human fluids and cell extracts

Dias

Ferreira

Грубер

et al. 2019

Chemistry and Physics of Lipids

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Section: Introductionmentioning

confidence: 99%

Sulfate-based lipids: Analysis of healthy human fluids and cell extracts

Dias

Ferreira

Грубер

et al. 2019

Chemistry and Physics of Lipids

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“…With this procedure keto sterols (derived from sulfates 1-6) and sterols without keto groups (derived from 7, 8) can be analyzed likewise. [33]; for chromatographic and mass spectral characteristics see Supplementary Table S1.…”

Section: Methyloxime-trimethylsilyl (Mo-tms) Derivativesmentioning

confidence: 99%

“…For this purpose trimethyliodosilane can be used. This reactive reagent is generated in situ in a mixture [33]; for chromatographic and mass spectral characteristics see Supplementary Table S1. The problematic (and frequently inevitable) enol TMS ether formation of keto sterols can be avoided with a two-step derivatization protocol.…”

Section: Methyloxime-trimethylsilyl (Mo-tms) Derivativesmentioning

confidence: 99%

“…The observed total ion chromatogram (TIC) in Figure 3 shows one peak (I) for pregnenolone with only one TMS ether (silylated 3-OH) and three (II-IV) artifacts corresponding to pregnenolone derivatives with an additional enol TMS ether. The plausible structures of these derivatives are shown in Figure 3c [33].…”

Section: Introductionmentioning

confidence: 99%

“…This reactive reagent is generated in situ in a mixture of MSTFA and ammonium iodide. A reducing agent such as mercaptoethanol is further added in order to avoid undesired side reactions resulting from accidentally formed iodine [33][34][35][36][37][38]. This method requires much effort for optimization depending on the analytes of interest [36].…”

Section: Introductionmentioning

confidence: 99%

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Comparison of Strategies for the Determination of Sterol Sulfates via GC-MS Leading to a Novel Deconjugation-Derivatization Protocol

et al. 2019

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Sulfoconjugates of sterols play important roles as neurosteroids, neurotransmitters, and ion channel ligands in health and disease. In most cases, sterol conjugate analysis is performed with liquid chromatography-mass spectrometry. This is a valuable tool for routine analytics with the advantage of direct sterol sulfates analysis without previous cleavage and/or derivatization. The complementary technique gas chromatography-mass spectrometry (GC-MS) is a preeminent discovery tool in the field of sterolomics, but the analysis of sterol sulfates is hampered by mandatory deconjugation and derivatization. Despite the difficulties in sample workup, GC-MS is an indispensable tool for untargeted analysis and steroid profiling. There are no general sample preparation protocols for sterol sulfate analysis using GC-MS. In this study we present a reinvestigation and evaluation of different deconjugation and derivatization procedures with a set of representative sterol sulfates. The advantages and disadvantages of trimethylsilyl (TMS), methyloxime-trimethylsilyl (MO-TMS), and trifluoroacetyl (TFA) derivatives were examined. Different published procedures of sterol sulfate deconjugation, including enzymatic and chemical cleavage, were reinvestigated and examined for diverse sterol sulfates. Finally, we present a new protocol for the chemical cleavage of sterol sulfates, allowing for simultaneous deconjugation and derivatization, simplifying GC-MS based sterol sulfate analysis.

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Routine application of SFC‐MS in doping control: Analysis of 3 × 1000 urine samples using three different SFC‐MS instruments

Gavrilović,

Wüst,

Danaceau

et al. 2024

Drug Testing and Analysis

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Supercritical fluid chromatography‐mass spectrometry (SFC‐MS) has proved to be a beneficial tool for sample analysis for a wide variety of compounds and, as such, has recently gained the attention of the anti‐doping community. We have tested the applicability of SFC‐MS for routine doping control analysing approximately 3 × 1000 identical anti‐doping samples utilising SFC‐MS instruments from three different vendors: Agilent Technologies, Waters Corporation and Shimadzu Corporation. A ‘dilute and inject’ approach either without or after hydrolysis of glucuronide metabolites was applied. Most of the compounds included in our study demonstrated excellent chromatography, whereas some showed co‐elution with endogenous interferences requiring MS discrimination. Retention times typically were very stable within batches (%CV ≤ 0.5%), although this appeared to be analyte and column dependent. Chromatographic peak shape was good (symmetrical) and stable over the period of the testing without any change of column. Our results suggest that SFC‐MS is a sensitive, reproducible and robust analytical tool ready to be used in anti‐doping laboratories alongside the currently applied techniques such as gas and liquid chromatography coupled to mass spectrometry. Even if instruments are designed slightly differently, all three setups demonstrated their fitness for the purpose in anti‐doping testing.

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Methods in endogenous steroid profiling – A comparison of gas chromatography mass spectrometry (GC–MS) with supercritical fluid chromatography tandem mass spectrometry (SFC-MS/MS)

Cited by 46 publications

References 33 publications

Sulfate-based lipids: Analysis of healthy human fluids and cell extracts

Sulfate-based lipids: Analysis of healthy human fluids and cell extracts

Comparison of Strategies for the Determination of Sterol Sulfates via GC-MS Leading to a Novel Deconjugation-Derivatization Protocol

Routine application of SFC‐MS in doping control: Analysis of 3 × 1000 urine samples using three different SFC‐MS instruments

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