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Routine application of SFC-MS in doping control: Analysis of 3 × 1000 urine samples using three different SFC-MS instruments
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2024-02-15 , DOI: 10.1002/dta.3652
Ivana Gavrilović 1 , Bernhard Wüst 2 , Jonathan Danaceau 3 , Emmanuelle Braidman 4 , Xavier de la Torre 5 , Francesco Botrè 5, 6 , Maria Kristina Parr 7 , David Cowan 8
Affiliation  

Supercritical fluid chromatography-mass spectrometry (SFC-MS) has proved to be a beneficial tool for sample analysis for a wide variety of compounds and, as such, has recently gained the attention of the anti-doping community. We have tested the applicability of SFC-MS for routine doping control analysing approximately 3 × 1000 identical anti-doping samples utilising SFC-MS instruments from three different vendors: Agilent Technologies, Waters Corporation and Shimadzu Corporation. A ‘dilute and inject’ approach either without or after hydrolysis of glucuronide metabolites was applied. Most of the compounds included in our study demonstrated excellent chromatography, whereas some showed co-elution with endogenous interferences requiring MS discrimination. Retention times typically were very stable within batches (%CV ≤ 0.5%), although this appeared to be analyte and column dependent. Chromatographic peak shape was good (symmetrical) and stable over the period of the testing without any change of column. Our results suggest that SFC-MS is a sensitive, reproducible and robust analytical tool ready to be used in anti-doping laboratories alongside the currently applied techniques such as gas and liquid chromatography coupled to mass spectrometry. Even if instruments are designed slightly differently, all three setups demonstrated their fitness for the purpose in anti-doping testing.

中文翻译:


SFC-MS 在兴奋剂控制中的常规应用:使用三种不同的 SFC-MS 仪器分析 3 × 1000 份尿液样本



超临界流体色谱-质谱 (SFC-MS) 已被证明是对多种化合物进行样品分析的有用工具,因此最近引起了反兴奋剂界的关注。我们使用来自三个不同供应商(安捷伦科技公司、沃特世公司和岛津公司)的 SFC-MS 仪器,测试了 SFC-MS 在常规兴奋剂控制中的适用性,分析了大约 3 × 1000 个相同的反兴奋剂样品。应用不水解或水解葡萄糖醛酸代谢物后的“稀释并注射”方法。我们研究中包含的大多数化合物均表现出出色的色谱性能,而某些化合物则表现出与内源性干扰物共洗脱的情况,需要 MS 进行区分。批次内的保留时间通常非常稳定 (%CV ≤ 0.5%),尽管这似乎取决于分析物和色谱柱。色谱峰形状良好(对称)且在测试期间稳定,没有任何色谱柱变化。我们的结果表明,SFC-MS 是一种灵敏、可重复且稳定的分析工具,可与当前应用的技术(例如气相色谱和液相色谱与质谱联用)一起用于反兴奋剂实验室。即使仪器的设计略有不同,所有三种设置都证明了它们适合反兴奋剂测试的目的。
更新日期:2024-02-20
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