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A liquid chromatography-electrospray ionization-tandem mass spectrometric (LC-ESI-MS/MS) method was developed and validated for the simultaneous detection and quantification of seven amphetamine derivatives (amphetamine (AP), methamphetamine (MA), 3,4-methylenedioxy-N-amphetamine (MDA), 3,4-methylenedioxy-N-methamphetamine (MDMA), 3,4-methylenedioxy-N-ethylamphetamine (MDEA), N,N-dimethylamphetamine (DMA), and N,N-dimethylamphetamine-N-oxide (DMANO)) in human urine. Seven deuterium-labeled compounds were prepared for use as internal standards to quantify the analytes. One milliliter of urine was combined with 1 mL of 0.2 M sodium carbonate buffer solution (pH 9.0) before solid phase extraction (SPE). An Oasis HLB SPE column followed by chromatographic separation on a Capcell Pak C18 MG-II column (150 × 2.0 mm I.D., 5 μm) and electrospray mass spectrometry with multiple reaction monitoring were used for selective and sensitive detection. The use of ammonium formate (5 mM, pH adjusted to 4.0 with formic acid, Solvent A) and acetonitrile (Solvent B) as the mobile phase at a flow rate of 230 μL/min was found to be the most effective for the separation. The linear ranges were 5.0-1000 ng/mL for AP, MDA, MDMA, MDEA, DMA, and DMANO and 10.0- 1000 ng/mL for MA, with good correlation coefficients (r² > 0.996). The intra-day, inter-day, and interperson precisions were within 14.6%, 12.1% and 15.5%, respectively. The intra-day, inter-day, and interperson accuracies were between -11.6 and 9.0%, -7.9 and 2.3%, and -13.2 and 4.3%, respectively. The limits of detection (LODs) for each analytical compound were lower than 1.95 ng/mL. The recovery ranged from 72.3 to 103.3%. The applicability of the developed method was examined by analyzing several urine samples from confirmed drug abusers.

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참고문헌 (17건) : 자료제공( 네이버학술정보 )

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번호 참고문헌 국회도서관 소장유무
1 Chromatographia and Its Scientific Future 네이버 미소장
2 Chromatographia’s new layout and website 네이버 미소장
3 Caldwell, J., The metabolism of amphetamines in mammals. Drug Metab. Rev., 5, 219-280 (1976). 미소장
4 Cheng, W. C., Mok, V. K., Chan, K. K., and Li, A. F., A rapid and convenient LC/MS method for routine identification of methamphetamine/dimethylamphetamine and their metabolites in urine. Forensic Sci. Int., 166, 1-7 (2007). 미소장
5 Cho, B. I., Methamphetamine abuse: epidemiologic issues and implications. In Miller, M. A. and Kozel, N. J. (Eds.). NIDA Research Monograph 115. US Department of Health and Human Services, Rockville, pp. 99-106 (1991). 미소장
6 Cody, J. T., Metabolic precursors to amphetamine and methamphetamine. Forensic Sci. Rev., 5, 109-127 (1993). 미소장
7 Determination of amphetamine and methamphetamine in urine by solid phase extraction and ion-pair liquid chromatography-electrospray-tandem mass spectrometry. 네이버 미소장
8 Pharmacology and toxicology of amphetamine and related designer drugs. 네이버 미소장
9 Simultaneous chiral determination of methamphetamine and its metabolites in urine by capillary electrophoresis-mass spectrometry. 네이버 미소장
10 The metabolism of dimethylamphetamine in rat and man. 네이버 미소장
11 The role of nitrogen oxidation in the excretion of drugs and foreign compounds. 네이버 미소장
12 Discrimination of Dimethylamphetamine and Methamphetamine Use: Simultaneous Determination of Dimethylamphetamine-N-Oxide and Other Metabolites in Urine by High-Performance Liquid Chromatography-Electrospray Ionization Mass Spectrometry 네이버 미소장
13 Simultaneous determination of psychotropic phenylalkylamine derivatives in human hair by gas chromatography/mass spectrometry 네이버 미소장
14 Sato, M., Hida, M., and Nagase, H., Analysis of dimethylamphetamine and its metabolites in human urine by liquid chromatography-electrospray ionization-mass spectrometry with direct sample injection. Forensic Sci. Int., 128, 146- 154 (2002). 미소장
15 Supreme Prosecutors' Office, Drug Trend Report. vol. 12, Seoul, (2007). 미소장
16 Supreme Prosecutors' Office, White Paper on Drug-Related Crimes. Seoul, pp. 95-122, (2004). 미소장
17 Behavioral effects of N-methylamphetamine and N,N-dimethylamphetamine in rats and squirrel monkeys. 네이버 미소장