The present study investigates the applicability of the chemical analysis of wastewater to assess the use of doping substances by the general population and amateur athletes. To this end, an analytical methodology that can identify and quantify a list of 15 substances from the groups of anabolic steroids, weight loss products, and masking agents in wastewater has been developed. The method uses solid phase extraction to increase the detection sensitivity of the target analytes, expected to be present at very low concentrations (ng L⁻¹ range), and decrease possible matrix interferences. Instrumental analysis is performed by liquid chromatography coupled to high-resolution mass spectrometry, allowing data acquisition in both full scan and tandem MS mode. The method has been successfully validated at two concentration levels (50 and 200 ng L⁻¹) with limits of quantification ranging between 0.7 and 60 ng L⁻¹, intra- and inter-day precision expressed as relative standard deviation below 15%, procedural recoveries between 60 and 160% and matrix effects ranging from 45 to 121%. The stability of the analytes in wastewater was evaluated at different storage temperatures illustrating the importance of freezing the samples immediately after collection. The application of the method to 24-h composite wastewater samples collected at the entrance of three wastewater treatment plants and one pumping station while different sport events were taking place revealed the presence in wastewater, and hence the use, of the weight loss substances ephedrine, norephedrine, methylhexanamine, and 2,4-dinitrophenol. The use of these stimulants was visible just prior and during the event days and in greater amounts than anabolic steroids or masking agents.

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本研究调查了废水的化学分析方法的适用性，以评估普通人群和业余运动员对掺杂物质的使用。为此，已经开发了一种分析方法，可以识别和量化废水中的合成代谢类固醇，减肥产品和掩蔽剂中的15种物质。该方法使用固相萃取来提高目标分析物的检测灵敏度，目标分析物预期以非常低的浓度（ng L ^-1范围），并减少可能的矩阵干扰。通过液相色谱与高分辨率质谱联用进行仪器分析，从而可以全扫描和串联MS模式采集数据。该方法已在两个浓度水平（50和200 ng L ^-1）下成功验证，定量限在0.7到60 ng L ^-1之间，日内和日间精度表示为相对标准偏差低于15％，程序回收率在60％至160％之间以及矩阵效应在45％至121％之间。在不同的存储温度下评估了废水中分析物的稳定性，说明了收集后立即冷冻样品的重要性。该方法对在不同体育赛事中从三个废水处理厂和一个泵站入口处收集的24小时复合废水样品的应用表明，废水中存在麻黄素，因此使用了减肥物质麻黄碱，去甲麻黄碱，甲基己胺和2,4-二硝基苯酚。这些刺激物的使用在事件发生之前和发生期间是可见的，并且其含量高于合成代谢类固醇或掩蔽剂。

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