Doping Control Laboratory Madrid, State Anti-Doping Agency, El Greco s/n, ES-28040, Madrid, Spain.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Jul 15;901:98-106. doi: 10.1016/j.jchromb.2012.06.007. Epub 2012 Jun 15.
Matrix effects (ion suppression/enhancement) are a well-observed phenomenon in analyses of biological matrices by high-performance liquid chromatography-mass spectrometry (LC-MS). However, few simple solutions for detecting and minimizing these adverse effects have been described so far in multianalyte analysis, especially in the field of doping control. This study describes an exhaustive characterization of matrix effects in one hundred urine samples fortified with 41 analytes (glucocorticoids and diuretics). It introduces a novel marker to identify samples in which the reliability of the results is compromised because of acute ion suppression. This new strategy strengthens the rigor of the analysis for screening purposes. Once the matrix effect is identified, a selective sample preparation is introduced to minimize the adverse ion suppression effect. That selective extraction together with the use of a deuterated internal standard permits enhancing the ruggedness of the estimation of glucocorticoid concentration in urine.
在高效液相色谱-质谱（LC-MS）分析生物基质时，基质效应（离子抑制/增强）是一种常见的现象。然而，到目前为止，在多分析物分析中，特别是在兴奋剂控制领域，还很少有简单的方法来检测和最小化这些不利影响。本研究对 100 个尿液样品进行了全面的基质效应特征描述，这些样品中添加了 41 种分析物（糖皮质激素和利尿剂）。它引入了一种新的标记物来识别由于急性离子抑制而导致结果可靠性受损的样品。这种新策略为筛选目的加强了分析的严格性。一旦确定了基质效应，就引入了一种选择性的样品制备方法来最小化不利的离子抑制效应。这种选择性提取以及使用氘代内标可以提高尿液中糖皮质激素浓度估计的坚固性。
