title: An automated sample preparation for detection of 72 doping-related substances.
abstract: 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.
authors.affiliation: 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.
authors.forename: Darío
authors.initials: D
authors.lastname: Cuervo
authors.forename: Pablo
authors.initials: P
authors.lastname: Díaz-Rodríguez
authors.forename: Jesús
authors.initials: J
authors.lastname: Muñoz-Guerra
mesh_terms: D001331:Automation; D004300:Doping in Sports; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D059625:Liquid-Liquid Extraction; D015813:Substance Abuse Detection / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods*
keywords: automated sample preparation; doping control analysis; liquid-liquid extraction; urine analysis