Preventive doping control analysis: liquid and gas chromatography time-of-flight mass spectrometry for detection of designer steroids.
A new combined doping control screening method for the analysis of anabolic steroids in human urine using liquid chromatography/electrospray ionization orthogonal acceleration time-of-flight mass spectrometry (LCoaTOFMS) and gas chromatography/electron ionization orthogonal acceleration time-of-flight mass spectrometry (GCoaTOFMS) has been developed in order to acquire accurate full scan MS data to be used to detect designer steroids. The developed method allowed the detection of representative prohibited substances, in addition to steroids, at concentrations of 10 ng/mL for anabolic agents and metabolites, 30 ng/mL for corticosteroids, 500 ng/mL for stimulants and beta-blockers, 250 ng/mL for diuretics, and 200 ng/mL for narcotics. Sample preparation was based on liquid-liquid extraction of hydrolyzed human urine, and the final extract was analyzed as trimethylsilylated derivatives in GCoaTOFMS and underivatized in LCoaTOFMS in positive ion mode. The sensitivity, mass accuracy, advantages and limitations of the developed method are presented.
Georgakopoulos
Costas G
CG
Doping Control Laboratory of Athens, Olympic Athletic Center of Athens Spiros Louis, 37 Kifissias Ave., 151 23 Maroussi, Greece. oaka@ath.forthnet.gr
Vonaparti
Ariadni
A
Stamou
Marianna
M
Kiousi
Polyxeni
P
Lyris
Emmanouil
E
Angelis
Yiannis S
YS
Tsoupras
George
G
Wuest
Bernhard
B
Nielen
Michel W F
MW
Panderi
Irene
I
Koupparis
Michalis
M
D045930:Anabolic Agents / Q000652:urine*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D015198:Designer Drugs / Q000032:analysis*; D004300:Doping in Sports / Q000517:prevention & control*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013256:Steroids / Q000652:urine*
D045930:Anabolic Agents; D015198:Designer Drugs; D013256:Steroids