Chromatographic–mass spectrometric analysis of peptidic analytes (2–10 kDa) in doping control urine samples

IF 1.9 3区 化学 Q3 BIOCHEMICAL RESEARCH METHODS
Andreas Thomas, Katja Walpurgis, Mario Thevis
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引用次数: 0

Abstract

Peptides with a molecular mass between 2 and 10 kDa that are prohibited in elite sports usually require dedicated sample preparation and mass spectrometric detection that commonly cannot be combined with other (lower molecular mass) substances. In most instances, the physicochemical differences are too significant to allow for a generic analytical procedure. A simplification of established and comparably complex analytical approaches is therefore desirable and has been accomplished in the context of this study. With urine samples representing still the most frequently collected doping control specimens, efficient extraction of peptidic analytes from this matrix was a major goal of this method, as demonstrated for the included compounds such as insulins (human, lispro, aspart, glulisine, tresiba, glargine metabolite, bovine insulin, porcine insulin), growth hormone-releasing hormones (sermorelin, CJC-1295, tesamorelin) incl. their respective metabolites, insulin-like-growth factors (long-R3-IGF-I, R3-IGF-I, des1–3-IGF-I), synacthen, gonadorelin and mechano growth factors (human MGF, MGF-Goldspink). Sample preparation and detection are controlled by five internal standards, covering all five included peptide drug categories. Nearly all requirements of the recent technical documents from the World Anti-Doping Agency (WADA) considering their minimum required performance levels (MRPL) are fulfilled, and the method was validated for its utilisation as initial testing procedure in doping controls. Finally, the approach was applied to authentic post-administration study urine samples (for insulins and gonadorelin) in order to provide proof of principle.

Abstract Image

兴奋剂检测尿样中肽类分析物(2-10 kDa)的色谱-质谱分析。
精英运动中禁用的分子质量在 2 到 10 kDa 之间的肽通常需要专门的样品制备和质谱检测,通常不能与其他(低分子质量)物质结合使用。在大多数情况下,理化差异太大,无法采用通用的分析程序。因此,简化既有的、复杂程度相当的分析方法是可取的,而本研究已实现了这一点。由于尿样仍是最常采集的兴奋剂检测标本,因此从这种基质中高效提取肽类分析物是本方法的主要目标。胰岛素样生长因子(long-R3 -IGF-I、R3 -IGF-I、des1-3 -IGF-I)、synacthen、促性腺激素和机械生长因子(人 MGF、MGF-Goldspink)。样品制备和检测由五种内部标准品控制,涵盖了所有五种肽类药物。该方法几乎满足了世界反兴奋剂机构(WADA)最新技术文件对最低性能要求(MRPL)的所有要求,并通过了在兴奋剂控制中用作初始检测程序的验证。最后,将该方法应用于真实的给药后研究尿样(胰岛素和促性腺激素),以提供原理证明。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
Journal of Mass Spectrometry
Journal of Mass Spectrometry 化学-光谱学
CiteScore
5.10
自引率
0.00%
发文量
84
审稿时长
1.5 months
期刊介绍: The Journal of Mass Spectrometry publishes papers on a broad range of topics of interest to scientists working in both fundamental and applied areas involving the study of gaseous ions. The aim of JMS is to serve the scientific community with information provided and arranged to help senior investigators to better stay abreast of new discoveries and studies in their own field, to make them aware of events and developments in associated fields, and to provide students and newcomers the basic tools with which to learn fundamental and applied aspects of mass spectrometry.
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