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Simultaneous determination of methamphetamine, 3,4-methylenedioxy-N-methylamphetamine, 3,4-methylenedioxy-N-ethylamphetamine, N,N-dimethylamphetamine, and their metabolites in urine by liquid chromatography-electrospray ionization-tandem mass spectrometry.
Arch Pharm Res. 2008 Dec; 31(12):1644-51.AP

Abstract

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 x 2.0 mm I.D., 5 microm) 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 microL/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.

Authors+Show Affiliations

Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office, Seoul, 137-730, Korea. paxus@spo.go.krNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

19099236

Citation

Kim, Jin Young, et al. "Simultaneous Determination of Methamphetamine, 3,4-methylenedioxy-N-methylamphetamine, 3,4-methylenedioxy-N-ethylamphetamine, N,N-dimethylamphetamine, and Their Metabolites in Urine By Liquid Chromatography-electrospray Ionization-tandem Mass Spectrometry." Archives of Pharmacal Research, vol. 31, no. 12, 2008, pp. 1644-51.
Kim JY, Cheong JC, Ko BJ, et al. Simultaneous determination of methamphetamine, 3,4-methylenedioxy-N-methylamphetamine, 3,4-methylenedioxy-N-ethylamphetamine, N,N-dimethylamphetamine, and their metabolites in urine by liquid chromatography-electrospray ionization-tandem mass spectrometry. Arch Pharm Res. 2008;31(12):1644-51.
Kim, J. Y., Cheong, J. C., Ko, B. J., Lee, S. K., Yoo, H. H., Jin, C., & In, M. K. (2008). Simultaneous determination of methamphetamine, 3,4-methylenedioxy-N-methylamphetamine, 3,4-methylenedioxy-N-ethylamphetamine, N,N-dimethylamphetamine, and their metabolites in urine by liquid chromatography-electrospray ionization-tandem mass spectrometry. Archives of Pharmacal Research, 31(12), 1644-51. https://doi.org/10.1007/s12272-001-2163-5
Kim JY, et al. Simultaneous Determination of Methamphetamine, 3,4-methylenedioxy-N-methylamphetamine, 3,4-methylenedioxy-N-ethylamphetamine, N,N-dimethylamphetamine, and Their Metabolites in Urine By Liquid Chromatography-electrospray Ionization-tandem Mass Spectrometry. Arch Pharm Res. 2008;31(12):1644-51. PubMed PMID: 19099236.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous determination of methamphetamine, 3,4-methylenedioxy-N-methylamphetamine, 3,4-methylenedioxy-N-ethylamphetamine, N,N-dimethylamphetamine, and their metabolites in urine by liquid chromatography-electrospray ionization-tandem mass spectrometry. AU - Kim,Jin Young, AU - Cheong,Jae Chul, AU - Ko,Beom Jun, AU - Lee,Sang Kyu, AU - Yoo,Hye Hyun, AU - Jin,Changbae, AU - In,Moon Kyo, Y1 - 2008/12/20/ PY - 2008/09/19/received PY - 2008/11/14/accepted PY - 2008/11/07/revised PY - 2008/12/23/entrez PY - 2008/12/23/pubmed PY - 2009/2/4/medline SP - 1644 EP - 51 JF - Archives of pharmacal research JO - Arch. Pharm. Res. VL - 31 IS - 12 N2 - 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 x 2.0 mm I.D., 5 microm) 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 microL/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. SN - 0253-6269 UR - https://www.unboundmedicine.com/medline/citation/19099236/Simultaneous_determination_of_methamphetamine_34_methylenedioxy_N_methylamphetamine_34_methylenedioxy_N_ethylamphetamine_NN_dimethylamphetamine_and_their_metabolites_in_urine_by_liquid_chromatography_electrospray_ionization_tandem_mass_spectrometry_ L2 - https://dx.doi.org/10.1007/s12272-001-2163-5 DB - PRIME DP - Unbound Medicine ER -