title: Analysis of anabolic steroids in urine by gas chromatography-microchip atmospheric pressure photoionization-mass spectrometry with chlorobenzene as dopant.
abstract: A gas chromatography-microchip atmospheric pressure photoionization-tandem mass spectrometry (GC-μAPPI-MS/MS) method was developed for the analysis of anabolic androgenic steroids in urine as their trimethylsilyl derivatives. The method utilizes a heated nebulizer microchip in atmospheric pressure photoionization mode (μAPPI) with chlorobenzene as dopant, which provides high ionization efficiency by producing abundant radical cations with minimal fragmentation. The performance of GC-μAPPI-MS/MS was evaluated with respect to repeatability, linearity, linear range, and limit of detection (LOD). The results confirmed the potential of the method for doping control analysis of anabolic steroids. Repeatability (RSD<10%), linearity (R(2)≥0.996) and sensitivity (LODs 0.05-0.1ng/mL) were acceptable. Quantitative performance of the method was tested and compared with that of conventional GC-electron ionization-MS, and the results were in good agreement.
authors.affiliation: Division of Pharmaceutical Chemistry, Faculty of Pharmacy, P.O. Box 56, 00014 University of Helsinki, Finland.
authors.forename: Laura
authors.initials: L
authors.lastname: Hintikka
authors.forename: Markus
authors.initials: M
authors.lastname: Haapala
authors.forename: Tiia
authors.initials: T
authors.lastname: Kuuranne
authors.forename: Antti
authors.initials: A
authors.lastname: Leinonen
authors.forename: Risto
authors.initials: R
authors.lastname: Kostiainen
mesh_terms: D045930:Anabolic Agents / Q000737:chemistry / Q000652:urine*; D000728:Androgens / Q000737:chemistry / Q000652:urine; D002722:Chlorobenzenes / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D016014:Linear Models; D008777:Methyltestosterone / Q000737:chemistry / Q000652:urine; D008958:Models, Molecular; D009277:Nandrolone / Q000737:chemistry / Q000652:urine; D055668:Photochemical Processes; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D045930:Anabolic Agents; D000728:Androgens; D002722:Chlorobenzenes; D009277:Nandrolone; C031294:chlorobenzene; D008777:Methyltestosterone
keywords: Anabolic steroids; Atmospheric pressure photoionization; Doping control; Gas chromatography; Microchip; Tandem mass spectrometry