title: Direct high-performance liquid chromatographic and high-performance liquid chromatographic-thermospray-mass spectrometric determination of enantiomers of methamphetamine and its main metabolites amphetamine and p-hydroxymethamphetamine in human urine.
abstract: For the identification of drug abuse, a simple and rapid method which allows us to distinguish enantiomers of methamphetamine (MA) and its metabolites amphetamine (AP) and p-hydroxymethamphetamine (p-OHMA) in human urine was explored by coupling direct HPLC and HPLC-thermospray-mass spectrometry (HPLC-TSP-MS) both of which employ a beta-cyclodextrin phenylcarbamate-bonded silica column. HPLC analysis was performed after the solid-phase extraction from the urine sample with Bond Elut SCX, and D- and L-enantiomers of MA, AP and p-OHMA could be separated well. The proposed conditions are as follows: eluent, acetonitrile-methanol-50 mM potassium phosphate buffer (pH 6.0) (10:30:60, v/v) flow-rate, 1.0 ml/min temperature, 25 degrees C. The linear calibration curves were obtained for D- and L- MA and AP in the concentration range from 0.2 to 20 micrograms/ml; the relative standard deviation for D- and L-AP and D- and, L-MA ranged from 1.67 to 2.35% at 2 micrograms/ml and the detection limits were 50 ng/ml for D- and L-AP and D-MA and 100 ng/ml for L-MA. For the verification of the direct HPLC identification, HPLC-TSP-MS was also carried out under the same conditions except that acetonitrile-methanol-100 mM ammonium acetate (pH 6.0) (10:30:60, v/v) was used as an eluent. Upon applying the scan mode, 10 ng/ml for D- and L-AP and D-MA and 20 ng/ml for L-MA were the detection limits. Using the selected ion monitoring mode, 0.5 ng/ml, 0.8 ng/ml and 1 ng/ml could be detected for D- and L-AP, D-MA and L-MA, respectively.
authors.affiliation: Forensic Science Laboratory, Osaka Prefectural Police, Japan.
authors.forename: M
authors.initials: M
authors.lastname: Katagi
authors.forename: H
authors.initials: H
authors.lastname: Nishioka
authors.forename: K
authors.initials: K
authors.lastname: Nakajima
authors.forename: H
authors.initials: H
authors.lastname: Tsuchihashi
authors.forename: H
authors.initials: H
authors.lastname: Fujima
authors.forename: H
authors.initials: H
authors.lastname: Wada
authors.forename: K
authors.initials: K
authors.lastname: Nakamura
authors.forename: K
authors.initials: K
authors.lastname: Makino
mesh_terms: D000661:Amphetamine / Q000652:urine*; D000697:Central Nervous System Stimulants / Q000652:urine*; D055598:Chemical Phenomena; D002627:Chemistry, Physical; D002851:Chromatography, High Pressure Liquid; D002852:Chromatography, Ion Exchange; D006801:Humans; D013058:Mass Spectrometry; D008694:Methamphetamine / Q000031:analogs & derivatives* / Q000652:urine; D012997:Solvents; D013237:Stereoisomerism; D015813:Substance Abuse Detection
chemical_list: D000697:Central Nervous System Stimulants; D012997:Solvents; D008694:Methamphetamine; C005877:pholedrine; D000661:Amphetamine