Cite #1

Simultaneous determination of selegiline-N-oxide, a new indicator for selegiline administration, and other metabolites in urine by high-performance liquid chromatography-electrospray ionization mbutt spectrometry by Katagi M, Tatsuno M, Miki A, Nishikawa M, Nakajima K, Tsuchihashi H. Forensic Science Laboratory, Osaka Prefectural Police Headquarters, Japan. J Chromatogr B Biomed Sci Appl 2001 Aug 5;759(1):125-33

ABSTRACT In order to discriminate selegiline (SG) use from methamphetamine (MA) use, the urinary metabolites of SG users have been investigated using high-performance liquid chromatography (HPLC)-electrospray ionization mbutt spectrometry (HPLC-ESI-MS). Selegiline-N-oxide (SGO), a specific metabolite of SG, was for the first time detected in the urine, in addition to other metabolites MA, amphetamine (AP) and desmethylselegiline (DM-SG). A combination of a Sep-pak C18 cartridge for the solid-phase extraction, a semi-micro SCX column (1.5 mm I.D.x 150 mm) for HPLC separation and ESI-MS for detection provided a simple and sensitive procedure for the simultaneous determination of these analytes. Acetonitrile-10 mM ammonium formate buffer adjusted to pH 3.0 (70:30, v-v) at a flow-rate of 0.1 ml-min was found to be the most effective mobile phase. Linear calibration curves were obtained over the concentration range from 0.5 to 100 ng-ml for all the analytes by monitoring each protonated molecular ion in the selected ion monitoring (SIM) mode. The detection limits ranged from 0.1 to 0.5 ng-ml. Upon applying the scan mode, 10-20 ng-ml were the detection limits. Quanbreastative investigation utilizing this revealed that SGO was about three times more abundant (47 ng-ml, 79 ng-ml) than DM-SG in two SG users' urine samples tested here. This newly-detected, specific metabolite SGO was found to be an effective indicator for SG administration.