Laboratorio de Control del Dopaje, Agencia Española de Protección de la Salud en el Deporte, Ministerio de Educación, Cultura y Deporte, Gobierno de España, c/ Pintor El Greco s/n, 28040, Madrid, Spain.
Drug Test Anal. 2014 Jun;6(6):516-27. doi: 10.1002/dta.1538. Epub 2013 Oct 25.
Automation of sample preparation procedures in a doping control laboratory is of great interest due to the large number of samples that have to be analyzed, especially in large events where a high throughput protocol is required to process samples over 24 h. The automation of such protocols requires specific equipment capable of carrying out the diverse mechanical tasks required for accomplishing these analytical methodologies, which include pipetting, shaking, heating, or crimping. An automated sample preparation procedure for the determination of doping-related substances by gas chromatography-mass spectrometry (GC-MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis, including enzymatic hydrolysis, liquid-phase extraction and derivatization steps, was developed by using an automated liquid handling system. This paper presents a description of the equipment, together with the validation data for 72 doping-related compounds including extraction efficiency, evaluation of carry-over, interferences, and robustness. Validation was approached as a comparison between the results obtained using the manual protocol and the transferred automated one. The described methodology can be applied for sample preparation in routine anti-doping analysis with high sample throughput and suitable performance.
由于需要分析的样品数量众多，特别是在需要处理 24 小时以上样品的大型活动中，兴奋剂检测实验室中的样品制备程序自动化具有重要意义。此类协议的自动化需要特定的设备，这些设备能够执行完成这些分析方法所需的各种机械任务，包括移液、摇晃、加热或压接。本研究采用自动化液体处理系统开发了一种用于气相色谱-质谱（GC-MS）和气相色谱-串联质谱（GC-MS/MS）分析测定与兴奋剂相关物质的自动化样品制备程序，包括酶解、液-液萃取和衍生化步骤。本文介绍了设备的描述，以及包括提取效率、携带污染评估、干扰和稳健性在内的 72 种与兴奋剂相关化合物的验证数据。验证方法是将手动方法和转移的自动方法的结果进行比较。所描述的方法可用于具有高通量和良好性能的常规反兴奋剂分析中的样品制备。
