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首页> 外文OA文献 >The Development and Evaluation of Methods for the Screening of Steroids using Molecular Imprinted Polymers coupled with comprehensive Gas Chromatography/Mass Spectrometry and Aptamers coupled with Liquid Chromatography/Mass Spectrometry
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The Development and Evaluation of Methods for the Screening of Steroids using Molecular Imprinted Polymers coupled with comprehensive Gas Chromatography/Mass Spectrometry and Aptamers coupled with Liquid Chromatography/Mass Spectrometry

机译：分子印迹聚合物结合全面气相色谱/质谱联用液相色谱/质谱联用筛选类固醇方法的开发与评价

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The profiling of hormones is an important requirement in sports dope testing and it is increasingly being used for clinical applications. The screening of samples for the detection of steroids is usually undertaken in urine and these analyses present many challenges. Issues related to the complexity of the matrix, the separation of exogenous from endogenous species and the very low detection limits have placed increasing demands on clinical and International Olympic Commission accredited laboratories. Whilst liquid chromatography (LC) systems provide a highly sensitive detection method for targeted species, gas chromatography, especially when coupled to mass spectrometry, is considered preferable for the screening of a wider range of target and unknown species. Existing chromatography methods are not without their limitations, not least the difficulty in reproducibly derivatising the wide range of steroids that can be exogenously administered, in particular the so called ‘designer steroids’ which deliberately hinder this process.ududInitially, a pilot study was conducted to investigate whether aptamer-coated magnetic beads could provide a simple, low cost method for the extraction of estradiol from urine, prior to its detection and quantification with mass spectrometry. In reality, the process necessitated the use of additional solvent extraction steps to the standard method applied previously. These additional steps added complexity and were not without issue and the limit of detection was not found to be adequate for the proposed clinical purpose.ududThe project explored the application of comprehensive gas chromatography/mass spectrometry (GC x GC/MS) coupled to bespoke molecular imprinted polymers (MIPS) as an alternative solution to the problem of the screening of multiple steroids in urine. Twelve structurally similar and commercially relevant steroids were used to develop the chromatographic method. Once optimised, these compounds were then extracted from synthetic urine using a MIP templated with testosterone and developed during the project. Significant improvements compared to commercially available C-18 materials were found. All the steroids were identified and detected when spiked at the 10 ng/ml level, as required by World Anti-Doping Agency (WADA) at the time. The method was further validated and then successfully applied to the extraction of designer steroids from synthetic urine, in the presence of the original steroids. Epistane, which has a different structure to testosterone, was not detected indicating the efficacy of the templating process.
机译：激素分布图是运动涂料测试中的一项重要要求，并且越来越多地用于临床。通常在尿液中进行用于类固醇检测的样品筛选，这些分析提出了许多挑战。与基质的复杂性，外源性与内源性物种的分离以及极低的检出限有关的问题对临床和国际奥委会认可的实验室提出了越来越高的要求。尽管液相色谱（LC）系统为目标物种提供了一种高度灵敏的检测方法，但气相色谱法（尤其是与质谱法联用时）被认为对于筛选范围更广的目标物种和未知物种更为可取。现有的色谱方法并非没有局限性，尤其是难以重现性地衍生出可以外源施用的多种类固醇的困难，特别是故意阻碍该过程的所谓“设计类固醇”。 ud ud最初是一项试验研究进行了研究，以探讨在用质谱检测和定量之前，适体包被的磁珠能否从尿液中提取雌二醇提供简单，低成本的方法。实际上，该方法需要在以前应用的标准方法中使用其他溶剂提取步骤。这些额外的步骤增加了复杂性，并且并非没有问题，并且发现的检测极限不足以满足拟议的临床目的。 ud ud该项目探索了气相色谱/质谱（GC x GC / MS）耦合的应用定制分子印迹聚合物（MIPS）作为尿液中多种类固醇筛查问题的替代解决方案。使用十二种结构相似且与商业相关的类固醇来开发色谱方法。一旦优化后，这些化合物就可以使用以睾丸激素为模板的MIP从合成尿中提取出来，并在项目开发过程中进行开发。与市售的C-18材料相比，发现了重大改进。按照当时的世界反兴奋剂机构（WADA）的要求，当以10 ng / ml的水平加标时，所有类固醇均得到鉴定和检测。该方法经过进一步验证，然后在原始类固醇存在的情况下成功地应用于从合成尿中提取设计类固醇。未检测到具有与睾丸激素不同结构的环氧乙烷，表明模板过程的功效。

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    Zulfiqar Adnan;

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  • 年度 2016
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