PMID- 31962207 OWN - NLM STAT- MEDLINE DCOM- 20200420 LR - 20200420 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 1139 DP - 2020 Feb 15 TI - Hollow-fibre liquid-phase microextraction and gas chromatography-mass spectrometric determination of amphetamines in whole blood. PG - 121973 LID - S1570-0232(19)31300-5 [pii] LID - 10.1016/j.jchromb.2020.121973 [doi] AB - 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 (r(2)) 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/x(2)), MDA (1/x), FEN (1/x(1/2)), MDMA (1/x(2)) 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. CI - Copyright (c) 2020 Elsevier B.V. All rights reserved. FAU - Bombana, Henrique Silva AU - Bombana HS AD - Faculty of Medicine, University of Sao Paulo, Av. Dr. Arnaldo, 455 Cerqueira Cesar, Sao Paulo 01246-903, Brazil. Electronic address: hbombana@usp.br. FAU - Dos Santos, Marcelo Filonzi AU - Dos Santos MF AD - Faculty of Medicine, University of Sao Paulo, Av. Dr. Arnaldo, 455 Cerqueira Cesar, Sao Paulo 01246-903, Brazil. FAU - Munoz, Daniel Romero AU - Munoz DR AD - Faculty of Medicine, University of Sao Paulo, Av. Dr. Arnaldo, 455 Cerqueira Cesar, Sao Paulo 01246-903, Brazil. FAU - Leyton, Vilma AU - Leyton V AD - Faculty of Medicine, University of Sao Paulo, Av. Dr. Arnaldo, 455 Cerqueira Cesar, Sao Paulo 01246-903, Brazil. LA - eng PT - Journal Article DEP - 20200113 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Amphetamines) SB - IM MH - Amphetamines/*blood/chemistry/isolation & purification MH - Forensic Toxicology MH - Gas Chromatography-Mass Spectrometry/*methods MH - Green Chemistry Technology MH - Humans MH - Limit of Detection MH - Linear Models MH - Liquid Phase Microextraction/*methods MH - Reproducibility of Results OTO - NOTNLM OT - Amphetamines OT - Green chemistry OT - Liquid-phase microextraction COIS- Declaration of Competing Interest The authors have no conflicts of interest to declare. EDAT- 2020/01/22 06:00 MHDA- 2020/04/21 06:00 CRDT- 2020/01/22 06:00 PHST- 2019/08/30 00:00 [received] PHST- 2020/01/08 00:00 [revised] PHST- 2020/01/09 00:00 [accepted] PHST- 2020/01/22 06:00 [pubmed] PHST- 2020/04/21 06:00 [medline] PHST- 2020/01/22 06:00 [entrez] AID - S1570-0232(19)31300-5 [pii] AID - 10.1016/j.jchromb.2020.121973 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2020 Feb 15;1139:121973. doi: 10.1016/j.jchromb.2020.121973. Epub 2020 Jan 13.