title: Automated sample preparation and gas chromatographic-mass spectrometric analysis of urinary androgenic anabolic steroids.
abstract: This paper presents an automated method for extracting anabolic agents from urine samples for their GC-MS analysis by selected-ion monitoring. The sample preparation was carried out in a Hewlett-Packard 7686 SPE PrepStation system. Each 0.6-ml aliquot was hydrolyzed, extracted, dried and trimethylsilyl (TMS) derivatized in a 2-ml vial without any hands-on labor. When sample preparation was finished 2 microl of the extract was injected into the gas chromatograph by split (1:10) mode. Due to the small amount of free space in the 2-ml vials for handling the sample, parameters like time of hydrolysis, type of shaking, number of extractions and some TMS derivatization parameters had to be adjusted to achieve the best recovery for all of the compounds in the screening. Manual and automated sample preparation schemes were compared in terms of linearity, precision, accuracy, limit of detection and recovery data. When large concentrations were analyzed using the automated method no carry-over effect was observed.
authors.affiliation: Doping Control Laboratory, Higher Sports Council, Madrid, Spain.
authors.forename: E
authors.initials: E
authors.lastname: Haber
authors.forename: J A
authors.initials: JA
authors.lastname: Muñoz-Guerra
authors.forename: C
authors.initials: C
authors.lastname: Soriano
authors.forename: D
authors.initials: D
authors.lastname: Carreras
authors.forename: C
authors.initials: C
authors.lastname: Rodriguez
authors.forename: F A
authors.initials: FA
authors.lastname: Rodriguez
mesh_terms: D045930:Anabolic Agents / Q000032:analysis* / Q000302:isolation & purification / Q000652:urine; D001331:Automation; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D015203:Reproducibility of Results; D014297:Trimethylsilyl Compounds
chemical_list: D045930:Anabolic Agents; D014297:Trimethylsilyl Compounds