title: Determination of amphetamine and related compounds in urine using on-line derivatization in octadecyl silica columns with 9-fluorenylmethyl chloroformate and liquid chromatography.
abstract: A method for the determination of amphetamine and related compounds in urine based on on-line derivatization with 9-fluorenylmethyl chloroformate (FMOC) and high-performance liquid chromatography is described. Derivatization is performed in a 20 x 2.1 mm I.D. column packed with a Hypersil ODS C18, 30 micron stationary phase, which is also used for sample clean-up and enrichment of the analytes. Next, the derivatized analytes are transferred to a LiChrospher 100 RP-C18 (5 micron, 125 x 4 mm I.D.) analytical column for their separation and quantification, using reversed-phase conditions and fluorescence detection. The described assay was applied to the determination of norephedrine, ephedrine, pseudoephedrine, amphetamine, phenylpropylamine and methamphetamine at concentrations of 0.5-10.0 micrograms/ml. Analyte conversions were about 55-96% of those obtained by the off-line derivatization mode under similar conditions, resulting in limits of detection in the 5-25 ng/ml range.
authors.affiliation: Department of Analytical Chemistry, University of València, Spain.
authors.forename: R
authors.initials: R
authors.lastname: Herráez-Hernández
authors.forename: P
authors.initials: P
authors.lastname: Campíns-Falcó
authors.forename: A
authors.initials: A
authors.lastname: Sevillano-Cabeza
mesh_terms: D000662:Amphetamines / Q000737:chemistry / Q000302:isolation & purification* / Q000652:urine; D001067:Appetite Depressants / Q000737:chemistry / Q000302:isolation & purification; D000697:Central Nervous System Stimulants / Q000737:chemistry / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004809:Ephedrine / Q000737:chemistry / Q000302:isolation & purification* / Q000652:urine; D005449:Fluorenes / Q000737:chemistry*; D008694:Methamphetamine / Q000737:chemistry / Q000302:isolation & purification / Q000652:urine; D009862:Online Systems; D011437:Propylamines / Q000737:chemistry / Q000302:isolation & purification* / Q000652:urine; D012822:Silicon Dioxide / Q000737:chemistry; D013050:Spectrometry, Fluorescence
chemical_list: D000662:Amphetamines; D001067:Appetite Depressants; D000697:Central Nervous System Stimulants; D005449:Fluorenes; D011437:Propylamines; C026679:octadecylsilica; D008694:Methamphetamine; D012822:Silicon Dioxide; C054007:1-(9-fluorenyl)methyl chloroformate; D004809:Ephedrine; C048861:3-phenylpropylamine