title: Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.
abstract: A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.
authors.affiliation: Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825, Japan.
authors.forename: Akihiro
authors.initials: A
authors.lastname: Nakamoto
authors.forename: Manami
authors.initials: M
authors.lastname: Nishida
authors.forename: Takeshi
authors.initials: T
authors.lastname: Saito
authors.forename: Izumi
authors.initials: I
authors.lastname: Kishiyama
authors.forename: Shota
authors.initials: S
authors.lastname: Miyazaki
authors.forename: Katsunori
authors.initials: K
authors.lastname: Murakami
authors.forename: Masataka
authors.initials: M
authors.lastname: Nagao
authors.forename: Akira
authors.initials: A
authors.lastname: Namura
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000652:urine*; D000662:Amphetamines / Q000652:urine*; D053000:Analytic Sample Preparation Methods / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D057230:Limit of Detection; D015394:Molecular Structure; D012822:Silicon Dioxide / Q000737:chemistry*
chemical_list: D000662:Amphetamines; D015104:3,4-Methylenedioxyamphetamine; D012822:Silicon Dioxide