title: Feasibility of capillary liquid chromatography/microchip atmospheric pressure photoionization mass spectrometry in analyzing anabolic steroids in urine samples.
abstract: We examined the feasibility of capillary liquid chromatography/microchip atmospheric pressure photoionization tandem mass spectrometry (capLC/microAPPI-MS/MS) for the analysis of anabolic steroids in human urine. The urine samples were pretreated by enzymatic hydrolysis (with beta-glucuronidase from Helix pomatia), and the compounds were liquid-liquid extracted with diethyl ether. After separation the compounds were vaporized by microchip APPI, photoionized by a 10 eV krypton discharge lamp, and detected by selected reaction monitoring. The capLC/microAPPI-MS/MS method showed good sensitivity with detection limits at the level of 1.0 ng mL(-1), good linearity with correlation coefficients between 0.9954 and 0.9990, and good repeatability with relative standard deviations below 10%. These results demonstrate that microchip APPI combined with capLC/MS/MS provides a new potential method for analyzing non-polar and neutral compounds in biological samples.
authors.affiliation: Division of Pharmaceutical Chemistry, Faculty of Pharmacy, University of Helsinki, Helsinki, Finland.
authors.forename: Linda L
authors.initials: LL
authors.lastname: Ahonen
authors.forename: Markus
authors.initials: M
authors.lastname: Haapala
authors.forename: Ville
authors.initials: V
authors.lastname: Saarela
authors.forename: Sami
authors.initials: S
authors.lastname: Franssila
authors.forename: Tapio
authors.initials: T
authors.lastname: Kotiaho
authors.forename: Risto
authors.initials: R
authors.lastname: Kostiainen
mesh_terms: D045930:Anabolic Agents / Q000652:urine*; D053801:Capillary Electrochromatography / Q000379:methods*; D006801:Humans; D016014:Linear Models; D013058:Mass Spectrometry / Q000379:methods*; D008696:Methandrostenolone / Q000652:urine; D008777:Methyltestosterone / Q000652:urine; D046208:Microchip Analytical Procedures / Q000379:methods*; D009277:Nandrolone / Q000652:urine; D009330:Nebulizers and Vaporizers; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013256:Steroids / Q000652:urine*; D001617:beta-Glucosidase / Q000737:chemistry / Q000378:metabolism
chemical_list: D045930:Anabolic Agents; D013256:Steroids; D009277:Nandrolone; D008696:Methandrostenolone; D001617:beta-Glucosidase; D008777:Methyltestosterone