Determination of selected stimulants in urine for sports drug analysis by solid phase extraction via cation exchange and means of liquid chromatography-tandem mass spectrometry.
Stimulatory substances applied during competition possess a reasonable potential as performance enhancing agents and their misuse in elite sport has been frequently reported during the last few decades. An analytical method for the qualitative determination of selected stimulants containing a primary or secondary amine moiety in human urine for doping control purposes was developed. A rapid and highly specific procedure based on a sample preparation using weak cation exchange solid phase extraction (SPE-XCW) followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with a C6-Phenyl analytical column allowed the unambiguous identification of the target analytes down to low ng mL(-1) concentration levels. Validation provided recovery rates of better than 75%, precisions of less than 20% and a linear approximation in the required working range (10-750 ng mL(-1)) were obtained for 19 different target compounds. This method provides a rugged and highly specific alternative to the established method utilising gas or liquid chromatography after liquid-liquid extraction.
Thomas
Andreas
A
Center for Preventive Doping Research, Institute of Biochemistry, German Sport University Cologne, Am Sportpark Müngersdorf 6, 50933 Cologne, Germany. a.thomas@biochem.dshs-koeln.de
Sigmund
Gerd
G
Guddat
Sven
S
Schänzer
Wilhelm
W
Thevis
Mario
M
D000328:Adult; D002411:Cation Exchange Resins; D000697:Central Nervous System Stimulants / Q000652:urine*; D002851:Chromatography, High Pressure Liquid; D004300:Doping in Sports; D005260:Female; D006801:Humans; D008297:Male; D008875:Middle Aged; D052616:Solid Phase Extraction; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D015813:Substance Abuse Detection / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
D002411:Cation Exchange Resins; D000697:Central Nervous System Stimulants