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Hollow-fibre liquid-phase microextraction and gas chromatography-mass spectrometric determination of amphetamines in whole blood.

Abstract

Here, we present a fully validated method using a hollow-fibre liquid-phase microextraction technique for the determination by gas chromatography-mass spectrometry (GC-MS) of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxyethylamphetamine (MDEA) in whole blood. The validation parameters presented successful values within those recommended by the Scientific Working Group for Forensic Toxicology (SWGTox) in the Standard Practices for Method Validation in Forensic Toxicology. The limits of detection ranged from 1 to 3 ng/mL, and the limits of quantification ranged from 2 to 5 ng/mL. The determination coefficients (r2) ranged from 0.990 to 0.997, and the method presented good intraday and interday accuracy (from 90.4% to 97.2%) and satisfactory recovery (from 68% to 110%). No carryover was observed. The heteroscedasticity was tested, and only AMP presented homoscedasticity. Weighting factors were applied to correct the linearity of MET (1/x2), MDA (1/x), FEN (1/x1/2), MDMA (1/x2) and MDEA (1/y). Dilution integrity was tested at ratios of 1:2, 1:5 and 1:10, and all maintained intraday precision (from 94.9% to 99.3%) and interday precision (from 89.4% to 94.9%). The validated method was applied to six real whole blood samples from individuals suspected of consuming ecstasy, and MDMA, MDA and amphetamine were successfully identified and quantified.

Authors+Show Affiliations

Faculty of Medicine, University of Sao Paulo, Av. Dr. Arnaldo, 455 Cerqueira Cesar, Sao Paulo 01246-903, Brazil. Electronic address: hbombana@usp.br.Faculty of Medicine, University of Sao Paulo, Av. Dr. Arnaldo, 455 Cerqueira Cesar, Sao Paulo 01246-903, Brazil.Faculty of Medicine, University of Sao Paulo, Av. Dr. Arnaldo, 455 Cerqueira Cesar, Sao Paulo 01246-903, Brazil.Faculty of Medicine, University of Sao Paulo, Av. Dr. Arnaldo, 455 Cerqueira Cesar, Sao Paulo 01246-903, Brazil.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

31962207

Citation

Bombana, Henrique Silva, et al. "Hollow-fibre Liquid-phase Microextraction and Gas Chromatography-mass Spectrometric Determination of Amphetamines in Whole Blood." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1139, 2020, p. 121973.
Bombana HS, Dos Santos MF, Muñoz DR, et al. Hollow-fibre liquid-phase microextraction and gas chromatography-mass spectrometric determination of amphetamines in whole blood. J Chromatogr B Analyt Technol Biomed Life Sci. 2020;1139:121973.
Bombana, H. S., Dos Santos, M. F., Muñoz, D. R., & Leyton, V. (2020). Hollow-fibre liquid-phase microextraction and gas chromatography-mass spectrometric determination of amphetamines in whole blood. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1139, 121973. https://doi.org/10.1016/j.jchromb.2020.121973
Bombana HS, et al. Hollow-fibre Liquid-phase Microextraction and Gas Chromatography-mass Spectrometric Determination of Amphetamines in Whole Blood. J Chromatogr B Analyt Technol Biomed Life Sci. 2020 Feb 15;1139:121973. PubMed PMID: 31962207.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Hollow-fibre liquid-phase microextraction and gas chromatography-mass spectrometric determination of amphetamines in whole blood. AU - Bombana,Henrique Silva, AU - Dos Santos,Marcelo Filonzi, AU - Muñoz,Daniel Romero, AU - Leyton,Vilma, Y1 - 2020/01/13/ PY - 2019/08/30/received PY - 2020/01/08/revised PY - 2020/01/09/accepted PY - 2020/1/22/pubmed PY - 2020/4/21/medline PY - 2020/1/22/entrez KW - Amphetamines KW - Green chemistry KW - Liquid-phase microextraction SP - 121973 EP - 121973 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 1139 N2 - Here, we present a fully validated method using a hollow-fibre liquid-phase microextraction technique for the determination by gas chromatography-mass spectrometry (GC-MS) of amphetamine (AMP), methamphetamine (MET), fenproporex (FEN), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxyethylamphetamine (MDEA) in whole blood. The validation parameters presented successful values within those recommended by the Scientific Working Group for Forensic Toxicology (SWGTox) in the Standard Practices for Method Validation in Forensic Toxicology. The limits of detection ranged from 1 to 3 ng/mL, and the limits of quantification ranged from 2 to 5 ng/mL. The determination coefficients (r2) ranged from 0.990 to 0.997, and the method presented good intraday and interday accuracy (from 90.4% to 97.2%) and satisfactory recovery (from 68% to 110%). No carryover was observed. The heteroscedasticity was tested, and only AMP presented homoscedasticity. Weighting factors were applied to correct the linearity of MET (1/x2), MDA (1/x), FEN (1/x1/2), MDMA (1/x2) and MDEA (1/y). Dilution integrity was tested at ratios of 1:2, 1:5 and 1:10, and all maintained intraday precision (from 94.9% to 99.3%) and interday precision (from 89.4% to 94.9%). The validated method was applied to six real whole blood samples from individuals suspected of consuming ecstasy, and MDMA, MDA and amphetamine were successfully identified and quantified. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/31962207/Hollow_fibre_liquid_phase_microextraction_and_gas_chromatography_mass_spectrometric_determination_of_amphetamines_in_whole_blood_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(19)31300-5 DB - PRIME DP - Unbound Medicine ER -