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微采样和 LC-MS/MS 用于尿液中糖皮质激素的兴奋剂检测。

Microsampling and LC-MS/MS for antidoping testing of glucocorticoids in urine.

机构信息

Research Group of Pharmaco-Toxicological Analysis (PTA Lab), Department of Pharmacy & Biotechnology (FaBiT), Alma Mater Studiorum -University of Bologna, Via Belmeloro 6, Bologna 40126, Italy.

Department for Life Quality Studies (QuVi), Alma Mater Studiorum - University of Bologna, Corso d'Augusto 237, Rimini 47921, Italy.

出版信息

Bioanalysis. 2020 Jun;12(11):769-782. doi: 10.4155/bio-2020-0044. Epub 2020 Jun 12.

DOI:10.4155/bio-2020-0044
PMID:32530296
Abstract

Systemic glucocorticoids are prohibited in-competition by the World Anti-Doping Agency. Here, we describe an original microsampling workflow for the quantitation of three endogenous (cortisol, corticosterone and cortisone) and three exogenous (dexamethasone, methylprednisolone and fludrocortisone) corticosteroids in 30 μl of human urine. Microsampling was carried out by dried urine spot (DUS) sampling and volumetric absorptive microsampling (VAMS), followed by solvent extraction and LC-MS/MS analysis. Good linearity (r > 0.9989) was obtained for all analytes; extraction yields (>81%), precision (RSD < 8.6%) and matrix effect (<12%) were satisfactory. Microsample stability at room temperature was good (analyte loss <15% after 3 months). Data obtained from real urine microsample analysis were compared with those of fluid urine, providing very good agreement (r > 0.9991).

摘要

世界反兴奋剂机构禁止在比赛中使用全身性糖皮质激素。在这里,我们描述了一种原始的微采样工作流程,用于定量分析 30μl 人尿中的三种内源性(皮质醇、皮质酮和可的松)和三种外源性(地塞米松、甲泼尼龙和氟氢可的松)皮质类固醇。微采样通过干尿斑(DUS)采样和体积吸收微采样(VAMS)进行,然后进行溶剂提取和 LC-MS/MS 分析。所有分析物均获得良好的线性(r > 0.9989);萃取回收率(> 81%)、精密度(RSD < 8.6%)和基质效应(< 12%)均令人满意。室温下微样本的稳定性良好(3 个月后分析物损失 < 15%)。从真实尿微样本分析中获得的数据与尿样数据进行了比较,结果非常吻合(r > 0.9991)。

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