Tags

Type your tag names separated by a space and hit enter

Determination of amphetamine-type stimulants in urine samples using microextraction by packed sorbent and gas chromatography-mass spectrometry.

Abstract

The aim of this work was the development, optimization and full validation of a method applying microextraction by packed sorbent (MEPS) coupled to gas chromatography-mass spectrometry (GC-MS) to determine amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxyethylmethamphetamine (MDMA), 3,4-methylenedioxy-N-methyl-α-ethylfenilethylamine (MBDB), and 3,4-methylenedioxy-N-ethylamphetamine (MDE) in urine samples. Using 200 μL of sample, the MEPS procedure was optimized concerning type of sorbent, sample dilution, number of strokes, activation of the ion exchange mechanism and composition of both washing and elution solvents. The method was fully validated according to the Food and Drug Administration and the Scientific Working Group of Forensic Toxicology guidelines for the validation of bioanalytical methods. The studied parameters included selectivity, calibration model and linearity, limits of detection and quantification, precision, accuracy, stability, dilution integrity and recoveries. Linearity was obtained in the range of 25-1000 ng/mL for MAMP, MBDB and MDE, 35-1000 ng/mL for AMP and MDMA, and 50-1000 ng/mL for MDA, with coefficients of determination (R2) >0.99 for all analytes. Both intra- and inter-day precision and accuracy were adequate, and coefficients of variation lower than 15% and mean relative errors (RE) within a range of ±15% of the theoretical concentrations were obtained for all compounds under study. Analyte recoveries ranged from 19 to 71%, allowing LLOQs ≤50 ng/mL.

Authors+Show Affiliations

Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Covilhã, Portugal; Laboratório de Fármaco-Toxicologia - UBIMedical, Universidade da Beira Interior, Covilhã, Portugal.Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Covilhã, Portugal; Laboratório de Fármaco-Toxicologia - UBIMedical, Universidade da Beira Interior, Covilhã, Portugal.Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Covilhã, Portugal; Nal von Minden, GmbH, Regensburg, Germany.Materiais Fibrosos e Tecnologias Ambientais - FibEnTech, Departamento de Química, Universidade da Beira Interior, Covilhã, Portugal; Departamento de Química, Universidade da Beira Interior, Covilhã, Portugal.Departamento de Química, Universidade da Beira Interior, Covilhã, Portugal.Materiais Fibrosos e Tecnologias Ambientais - FibEnTech, Departamento de Química, Universidade da Beira Interior, Covilhã, Portugal; Departamento de Química, Universidade da Beira Interior, Covilhã, Portugal.Serviço de Química e Toxicologia Forenses, Instituto de Medicina Legal e Ciências Forenses - Delegação do Centro, Coimbra, Portugal.Serviço de Química e Toxicologia Forenses, Instituto de Medicina Legal e Ciências Forenses - Delegação do Sul, Lisboa, Portugal.Centro de Investigação em Ciências da Saúde, Universidade da Beira Interior (CICS-UBI), Covilhã, Portugal; Laboratório de Fármaco-Toxicologia - UBIMedical, Universidade da Beira Interior, Covilhã, Portugal. Electronic address: egallardo@fcsaude.ubi.pt.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

31063954

Citation

Malaca, Sara, et al. "Determination of Amphetamine-type Stimulants in Urine Samples Using Microextraction By Packed Sorbent and Gas Chromatography-mass Spectrometry." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1120, 2019, pp. 41-50.
Malaca S, Rosado T, Restolho J, et al. Determination of amphetamine-type stimulants in urine samples using microextraction by packed sorbent and gas chromatography-mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2019;1120:41-50.
Malaca, S., Rosado, T., Restolho, J., Rodilla, J. M., Rocha, P. M. M., Silva, L., Margalho, C., Barroso, M., & Gallardo, E. (2019). Determination of amphetamine-type stimulants in urine samples using microextraction by packed sorbent and gas chromatography-mass spectrometry. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1120, 41-50. https://doi.org/10.1016/j.jchromb.2019.04.052
Malaca S, et al. Determination of Amphetamine-type Stimulants in Urine Samples Using Microextraction By Packed Sorbent and Gas Chromatography-mass Spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Jul 1;1120:41-50. PubMed PMID: 31063954.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of amphetamine-type stimulants in urine samples using microextraction by packed sorbent and gas chromatography-mass spectrometry. AU - Malaca,Sara, AU - Rosado,Tiago, AU - Restolho,José, AU - Rodilla,Jesus M, AU - Rocha,Pedro M M, AU - Silva,Lúcia, AU - Margalho,Cláudia, AU - Barroso,Mário, AU - Gallardo,Eugenia, Y1 - 2019/04/29/ PY - 2019/01/03/received PY - 2019/04/23/revised PY - 2019/04/28/accepted PY - 2019/5/8/pubmed PY - 2019/6/14/medline PY - 2019/5/8/entrez KW - Amphetamines KW - GC–MS KW - Microextraction by packed sorbent KW - Urine SP - 41 EP - 50 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 1120 N2 - The aim of this work was the development, optimization and full validation of a method applying microextraction by packed sorbent (MEPS) coupled to gas chromatography-mass spectrometry (GC-MS) to determine amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxyethylmethamphetamine (MDMA), 3,4-methylenedioxy-N-methyl-α-ethylfenilethylamine (MBDB), and 3,4-methylenedioxy-N-ethylamphetamine (MDE) in urine samples. Using 200 μL of sample, the MEPS procedure was optimized concerning type of sorbent, sample dilution, number of strokes, activation of the ion exchange mechanism and composition of both washing and elution solvents. The method was fully validated according to the Food and Drug Administration and the Scientific Working Group of Forensic Toxicology guidelines for the validation of bioanalytical methods. The studied parameters included selectivity, calibration model and linearity, limits of detection and quantification, precision, accuracy, stability, dilution integrity and recoveries. Linearity was obtained in the range of 25-1000 ng/mL for MAMP, MBDB and MDE, 35-1000 ng/mL for AMP and MDMA, and 50-1000 ng/mL for MDA, with coefficients of determination (R2) >0.99 for all analytes. Both intra- and inter-day precision and accuracy were adequate, and coefficients of variation lower than 15% and mean relative errors (RE) within a range of ±15% of the theoretical concentrations were obtained for all compounds under study. Analyte recoveries ranged from 19 to 71%, allowing LLOQs ≤50 ng/mL. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/31063954/Determination_of_amphetamine_type_stimulants_in_urine_samples_using_microextraction_by_packed_sorbent_and_gas_chromatography_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(19)30010-8 DB - PRIME DP - Unbound Medicine ER -