Journal
JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY
Volume -, Issue -, Pages -Publisher
AMER CHEMICAL SOC
DOI: 10.1021/jasms.2c00092
Keywords
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Funding
- Australian Research Council Linkage Project Scheme [LP180100421]
- Australian Research Council [LP180100421] Funding Source: Australian Research Council
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The identification and confirmation of steroid sulfate metabolites in biological samples are crucial in anti-doping analysis and clinical sciences. This study utilized energy-resolved collision-induced dissociation to distinguish isomeric steroid sulfate compounds and guide the synthesis of reference materials for unambiguous confirmation of a steroid sulfate biomarker.
The identification and confirmation of steroid sulfate metabolites in biological samples are essential to various fields, including anti-doping analysis and clinical sciences. Ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) is the leading method for the detection of intact steroid conjugates in biofluids, but because of the inherent complexity of biological samples and the low concentration of many targets of interest, metabolite identification based solely on mass spectrometry remains a major challenge. The confirmation of new metabolites typically depends on a comparison with synthetically derived reference materials that encompass a range of possible conjugation sites and stereochemistries. Herein, energy-resolved collision-induced dissociation (CID) is used as part of UHPLC-HRMS/MS analysis to distinguish between regio- and stereo-isomeric steroid sulfate compounds. This wholly MS-based approach was employed to guide the synthesis of reference materials to unambiguously confirm the identity of an equine steroid sulfate biomarker of testosterone propionate administration.
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