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An LC-MS/MS methodological approach to the analysis of hair for amphetamine-type-stimulant (ATS) drugs, including selected synthetic cathinones and piperazines.
Drug Test Anal. 2017 Jan; 9(1):96-105.DT

Abstract

Amphetamine-type-stimulants (ATS) are the second most commonly used group of illicit drugs worldwide. However, in the last few years, new psychoactive substances (NPS) with stimulant effects have appeared on the illegal market, which are not detected with traditional analytical methods. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination in hair of classic ATS (amphetamine, methamphetamine, 3,4-methylenedioxymethamphetamine and 3,4-methylenedioxyamphetamine), synthetic cathinones (methylone, methedrone, mephedrone, 3,4-methylenedioxypyrovalerone, (±)-4-fluoromethamphetamine and 4-fluoromethcathinone), synthetic piperazines (1-(3-chlorophenyl)piperazine (mCPP) and 3-trifluoromethylphenylpiperazine), and medicines (trazodone and phenazone) that produce mCPP as a metabolite, was developed and fully validated. Hair samples (30 mg) were incubated in acid methanol (0.1% HCl) and extracted by a mixed-mode solid-phase extraction. Chromatographic separation was performed using an Atlantis T3 (3 µm; 2.1x50 mm) analytical column, and ammonium formate 2 mM pH 3 and acetonitrile as mobile phase. The method was validated, including selectivity (no endogenous or exogenous interferences); linearity (2-20 to 2000-4000 pg/mg); limits of detection (0.2 to 5 pg/mg) and quantification (2 to 20 pg/mg); accuracy (93.4-109.4% of target concentration); imprecision (%CV<11.6%); extraction recovery (40.5-92.1%); matrix effect (24.1-227.2%); process efficiency (9.8-165.7%) and stability in the autosampler (-14.5% of loss). The method was applied to the analysis of 16 hair samples. Amphetamine (n=7; 69.1-777.1 pg/mg), methamphetamine (n=3; 120.4-1,538.9 pg/mg), MDA (n=2; 27.8-135.4 pg/mg) and MDMA (n=8; 73.4-3,654.5 pg/mg) were found. Moreover, 10 positive results for mCPP were detected (341.7->4000 pg/mg); however, in all cases trazodone identification (2085.3->4000 pg/mg) probed a licit origin of mCPP. Copyright © 2016 John Wiley & Sons, Ltd.

Authors+Show Affiliations

Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.Servizo de Psiquiatría, Complexo Hospitalario Universitario de Santiago (CHUS), Servizo Galego de Saúde (SERGAS), Santiago de Compostela, Spain.Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.Servicio de Toxicología, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain.

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

26914712

Citation

Lendoiro, Elena, et al. "An LC-MS/MS Methodological Approach to the Analysis of Hair for Amphetamine-type-stimulant (ATS) Drugs, Including Selected Synthetic Cathinones and Piperazines." Drug Testing and Analysis, vol. 9, no. 1, 2017, pp. 96-105.
Lendoiro E, Jiménez-Morigosa C, Cruz A, et al. An LC-MS/MS methodological approach to the analysis of hair for amphetamine-type-stimulant (ATS) drugs, including selected synthetic cathinones and piperazines. Drug Test Anal. 2017;9(1):96-105.
Lendoiro, E., Jiménez-Morigosa, C., Cruz, A., Páramo, M., López-Rivadulla, M., & de Castro, A. (2017). An LC-MS/MS methodological approach to the analysis of hair for amphetamine-type-stimulant (ATS) drugs, including selected synthetic cathinones and piperazines. Drug Testing and Analysis, 9(1), 96-105. https://doi.org/10.1002/dta.1948
Lendoiro E, et al. An LC-MS/MS Methodological Approach to the Analysis of Hair for Amphetamine-type-stimulant (ATS) Drugs, Including Selected Synthetic Cathinones and Piperazines. Drug Test Anal. 2017;9(1):96-105. PubMed PMID: 26914712.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - An LC-MS/MS methodological approach to the analysis of hair for amphetamine-type-stimulant (ATS) drugs, including selected synthetic cathinones and piperazines. AU - Lendoiro,Elena, AU - Jiménez-Morigosa,Cristian, AU - Cruz,Angelines, AU - Páramo,Mario, AU - López-Rivadulla,Manuel, AU - de Castro,Ana, Y1 - 2016/02/24/ PY - 2015/06/08/received PY - 2015/12/04/revised PY - 2015/12/12/accepted PY - 2016/2/26/pubmed PY - 2017/5/17/medline PY - 2016/2/26/entrez KW - amphetamine-type-stimulants KW - hair KW - new psychoactive substances KW - synthetic cathinones KW - synthetic piperazines SP - 96 EP - 105 JF - Drug testing and analysis JO - Drug Test Anal VL - 9 IS - 1 N2 - Amphetamine-type-stimulants (ATS) are the second most commonly used group of illicit drugs worldwide. However, in the last few years, new psychoactive substances (NPS) with stimulant effects have appeared on the illegal market, which are not detected with traditional analytical methods. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination in hair of classic ATS (amphetamine, methamphetamine, 3,4-methylenedioxymethamphetamine and 3,4-methylenedioxyamphetamine), synthetic cathinones (methylone, methedrone, mephedrone, 3,4-methylenedioxypyrovalerone, (±)-4-fluoromethamphetamine and 4-fluoromethcathinone), synthetic piperazines (1-(3-chlorophenyl)piperazine (mCPP) and 3-trifluoromethylphenylpiperazine), and medicines (trazodone and phenazone) that produce mCPP as a metabolite, was developed and fully validated. Hair samples (30 mg) were incubated in acid methanol (0.1% HCl) and extracted by a mixed-mode solid-phase extraction. Chromatographic separation was performed using an Atlantis T3 (3 µm; 2.1x50 mm) analytical column, and ammonium formate 2 mM pH 3 and acetonitrile as mobile phase. The method was validated, including selectivity (no endogenous or exogenous interferences); linearity (2-20 to 2000-4000 pg/mg); limits of detection (0.2 to 5 pg/mg) and quantification (2 to 20 pg/mg); accuracy (93.4-109.4% of target concentration); imprecision (%CV<11.6%); extraction recovery (40.5-92.1%); matrix effect (24.1-227.2%); process efficiency (9.8-165.7%) and stability in the autosampler (-14.5% of loss). The method was applied to the analysis of 16 hair samples. Amphetamine (n=7; 69.1-777.1 pg/mg), methamphetamine (n=3; 120.4-1,538.9 pg/mg), MDA (n=2; 27.8-135.4 pg/mg) and MDMA (n=8; 73.4-3,654.5 pg/mg) were found. Moreover, 10 positive results for mCPP were detected (341.7->4000 pg/mg); however, in all cases trazodone identification (2085.3->4000 pg/mg) probed a licit origin of mCPP. Copyright © 2016 John Wiley & Sons, Ltd. SN - 1942-7611 UR - https://www.unboundmedicine.com/medline/citation/26914712/An_LC_MS/MS_methodological_approach_to_the_analysis_of_hair_for_amphetamine_type_stimulant__ATS__drugs_including_selected_synthetic_cathinones_and_piperazines_ L2 - https://doi.org/10.1002/dta.1948 DB - PRIME DP - Unbound Medicine ER -