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Rapid analysis of amphetamine, methamphetamine, MDA, and MDMA in urine using solid-phase microextraction, direct on-fiber derivatization, and analysis by GC-MS.
J Anal Toxicol. 2000 Jan-Feb; 24(1):11-6.JA

Abstract

A rapid, sensitive, and solvent-free procedure for the simultaneous determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), and 3,4-methylenedioxymethamphetamine (MDMA) in urine was developed using solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode. A headspace vial containing the urine sample, NaOH, NaCl, and amphetamine-d3 as the internal standard was heated at 100 degrees C for 20 min. A polydimethylsiloxane fiber was maintained in the vial headspace for 10 min in order to adsorb the amphetaminic compounds, which were subsequently derivatized by exposing the fiber to trifluoroacetic anhydride for 20 min in the headspace of another vial maintained at 60 degrees C for 20 min. The trifluoroacetyl derivatives were desorbed in the GC injection port for 5 min. Several parameters were considered during the method optimization process. These included a comparison of SPME with or without headspace, the required derivatization procedure, and the influence of temperature on the headspace extraction and derivatization methods. The optimized method was validated for the four compounds tested. Calibration curves showed linearity in the range 50-1000 ng/mL (r = 0.9946-0.9999). Recovery data were 71.89-103.24%. The quantitation limits were 10 ng/mL for amphetamine and methamphetamine and 20 ng/mL for MDA and MDMA. All of these data recommend the applicability of the method for use in the analytical routine of a forensic laboratory.

Authors+Show Affiliations

Jurado C
Instituto Nacional de Toxicología, Sevilla, Spain. quim@sev.inaltox.es
Giménez MP
No affiliation info available
Soriano T
No affiliation info available
Menéndez M
No affiliation info available
Repetto M
No affiliation info available

MeSH

3,4-MethylenedioxyamphetamineAmphetamineDimethylpolysiloxanesGas Chromatography-Mass SpectrometryHumansMethamphetamineMicrochemistryN-Methyl-3,4-methylenedioxyamphetamineReproducibility of ResultsSensitivity and SpecificitySubstance Abuse DetectionSympathomimeticsTemperatureTime Factors

Pub Type(s)

Comparative Study
Journal Article

Language

eng

PubMed ID

10654563

Citation

Jurado, C, et al. "Rapid Analysis of Amphetamine, Methamphetamine, MDA, and MDMA in Urine Using Solid-phase Microextraction, Direct On-fiber Derivatization, and Analysis By GC-MS." Journal of Analytical Toxicology, vol. 24, no. 1, 2000, pp. 11-6.
Jurado C, Giménez MP, Soriano T, et al. Rapid analysis of amphetamine, methamphetamine, MDA, and MDMA in urine using solid-phase microextraction, direct on-fiber derivatization, and analysis by GC-MS. J Anal Toxicol. 2000;24(1):11-6.
Jurado, C., Giménez, M. P., Soriano, T., Menéndez, M., & Repetto, M. (2000). Rapid analysis of amphetamine, methamphetamine, MDA, and MDMA in urine using solid-phase microextraction, direct on-fiber derivatization, and analysis by GC-MS. Journal of Analytical Toxicology, 24(1), 11-6.
Jurado C, et al. Rapid Analysis of Amphetamine, Methamphetamine, MDA, and MDMA in Urine Using Solid-phase Microextraction, Direct On-fiber Derivatization, and Analysis By GC-MS. J Anal Toxicol. 2000 Jan-Feb;24(1):11-6. PubMed PMID: 10654563.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Rapid analysis of amphetamine, methamphetamine, MDA, and MDMA in urine using solid-phase microextraction, direct on-fiber derivatization, and analysis by GC-MS. AU - Jurado,C, AU - Giménez,M P, AU - Soriano,T, AU - Menéndez,M, AU - Repetto,M, PY - 2000/2/2/pubmed PY - 2000/3/11/medline PY - 2000/2/2/entrez SP - 11 EP - 6 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 24 IS - 1 N2 - A rapid, sensitive, and solvent-free procedure for the simultaneous determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), and 3,4-methylenedioxymethamphetamine (MDMA) in urine was developed using solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) in the selected ion monitoring mode. A headspace vial containing the urine sample, NaOH, NaCl, and amphetamine-d3 as the internal standard was heated at 100 degrees C for 20 min. A polydimethylsiloxane fiber was maintained in the vial headspace for 10 min in order to adsorb the amphetaminic compounds, which were subsequently derivatized by exposing the fiber to trifluoroacetic anhydride for 20 min in the headspace of another vial maintained at 60 degrees C for 20 min. The trifluoroacetyl derivatives were desorbed in the GC injection port for 5 min. Several parameters were considered during the method optimization process. These included a comparison of SPME with or without headspace, the required derivatization procedure, and the influence of temperature on the headspace extraction and derivatization methods. The optimized method was validated for the four compounds tested. Calibration curves showed linearity in the range 50-1000 ng/mL (r = 0.9946-0.9999). Recovery data were 71.89-103.24%. The quantitation limits were 10 ng/mL for amphetamine and methamphetamine and 20 ng/mL for MDA and MDMA. All of these data recommend the applicability of the method for use in the analytical routine of a forensic laboratory. SN - 0146-4760 UR - https://www.unboundmedicine.com/medline/citation/10654563/Rapid_analysis_of_amphetamine_methamphetamine_MDA_and_MDMA_in_urine_using_solid_phase_microextraction_direct_on_fiber_derivatization_and_analysis_by_GC_MS_ DB - PRIME DP - Unbound Medicine ER -
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