Energy-Resolved Fragmentation Aiding the Structure Elucidation of Steroid Biomarkers,ACS Environmental Au

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Energy-Resolved Fragmentation Aiding the Structure Elucidation of Steroid Biomarkers
ACS Environmental Au ( IF 6.7 ) Pub Date : 2022-06-07 , DOI: 10.1021/jasms.2c00092
Christopher C. J. Fitzgerald ₁ , Christopher Bowen ₂ , Madysen Elbourne ₃ , Adam Cawley ₄ , Malcolm D. McLeod ₁

Affiliation

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.

中文翻译：

能量分辨碎片有助于类固醇生物标志物的结构阐明

生物样品中类固醇硫酸盐代谢物的鉴定和确认对于包括反兴奋剂分析和临床科学在内的各个领域都是必不可少的。超高效液相色谱和串联质谱 (UHPLC-MS/MS) 是检测生物体液中完整类固醇偶联物的主要方法，但由于生物样品固有的复杂性和许多目标目标的低浓度，仅基于质谱的代谢物鉴定仍然是一项重大挑战。新代谢物的确认通常取决于与合成衍生的参考材料的比较，这些参考材料包含一系列可能的结合位点和立体化学。在此处，能量分辨碰撞诱导解离 (CID) 用作 UHPLC-HRMS/MS 分析的一部分，以区分区域异构体和立体异构体硫酸酯化合物。这种完全基于 MS 的方法用于指导参考材料的合成，以明确确认丙酸睾酮给药的马类固醇硫酸盐生物标志物的身份。

更新日期：2022-06-07

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