Mathieu Galmiche, Marie-Anaïs Monat, Diego A. Lopez, Cyrille Lamboley, Paul Connolly, Sergey Girel, Davy Guillarme, Isabel Meister, Serge Rudaz
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引用次数: 0
摘要
类固醇可用作临床代谢组学和其他人体毒理学相关领域的生物标记物。考虑到其等压化合物的数量以及母体化合物可能经历的 I 期和 II 期代谢途径的多样性,该化学组以其复杂性而著称。要成功分析生物样本中的类固醇,必须对液相色谱分离技术进行微调。对于具有极性头并可能受非特异性吸附影响的葡萄糖醛酸化和硫酸化类固醇衍生物来说,这尤其具有挑战性。我们研究了联苯固定相化学在分离类固醇及其第二阶段代谢物的选择性方面的优势,以及非特异性吸附现象在多大程度上会降低色谱性能。用钝化硬件取代传统硬件可大大降低硫酸盐类物质的峰宽和不对称性。在流动相中添加弱离子配对剂也有助于减少非特异性吸附,但不利于质谱检测。血浆中 52 种类固醇的成功检测证实,使用联苯固定相并辅以钝化色谱柱硬件,对类固醇及其第二阶段代谢物的成功生物医学分析大有帮助。
Substantial benefits of an inert biphenyl column for the analysis of steroids and their phase II metabolites in biological samples
Steroids can be used as biomarkers in clinical metabolomics and other fields related to human toxicology. This chemical group is known for its complexity, considering its number of isobaric compounds and the wide variety of phases I and II metabolic pathways that parent compounds can undergo. For a successful analysis of steroids in biological samples, liquid chromatography separation must be finely tuned. It is especially challenging for glucuronidated and sulfated steroids derivatives that bear polar heads and can be affected by non-specific adsorption. The benefits of a biphenyl stationary phase chemistry for the selectivity of the separation of steroids and their phase II metabolites and the extent to which nonspecific adsorption phenomena could degrade chromatographic performance were investigated. Replacing a conventional hardware by a passivated hardware allowed to considerably reduce peaks width and asymmetry of sulfated species. The addition of weak ion pairing agents in the mobile phase could also help to reduce non-specific adsorption but are detrimental to mass spectrometry detection. As confirmed by the successful detection of 52 steroids in plasma, the use of a biphenyl stationary phase complemented by a passivated column hardware is of great help for a successful biomedical analysis of steroids and their phase II metabolites.
期刊介绍:
The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.