Systematic analysis of diuretic doping agents by HPLC screening and GC/MS confirmation.
The simultaneous analysis of diuretic agents by reversed-phase liquid chromatography with a diode-array detector (DAD) was performed by using a gradient elution with acetonitrile and phosphate buffer on a Hypersil-ODS column. For the spiked urine the extraction recovery of solid-phase extraction (SPE) using Sep-Pak C18 cartridge was compared with that of liquid-liquid extraction (LLE) with diethyl ether at various pH. The standard calibration curves were linear from 0.20-20.0 micrograms/mL for all diuretic agents except amiloride, 1.0-20.0 micrograms/mL, and the detection limit was about 0.2 micrograms/mL for 3 mL of urine, except that of amiloride, which was 1.0 micrograms/mL. The confirmation analysis was performed by gas chromatography/mass spectrometry (GC/MS) following methylation. The characteristic mass fragment ions obtained by electron-impact (EI) ionization (70 eV) provided identification of each diuretic agent.
Park
S J
SJ
Doping Control Center, Korea Institute of Science and Technology, Cheongryang, Seoul.
Pyo
H S
HS
Kim
Y J
YJ
Kim
M S
MS
Park
J
J
D000328:Adult; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D004232:Diuretics / Q000652:urine*; D004300:Doping in Sports; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D008297:Male; D015813:Substance Abuse Detection / Q000379:methods*
D004232:Diuretics