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

Autor(es)

Bombana, Henrique Silva ^[1] ; dos Santos, Marcelo Filonzi ^[1] ; Munoz, Daniel Romero ^[1] ; Leyton, Vilma ^[1]

Afiliação do(s) autor(es)

^[1] Univ Sao Paulo, Fac Med, Av Dr Arnaldo, 455 Cerqueira Cesar, BR-01246903 Sao Paulo - Brazil

• Tipo de documento: Artigo Científico
• Fonte: JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES; v. 1139, FEB 15 2020.
• Citações Web of Science: 0

Resumo

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. (AU)

• Processo FAPESP: 16/20214-3 - Verificação do uso de drogas e medicamentos por motoristas profissionais através da análise toxicológica de fluido oral: desenvolvimento de novos métodos analíticos e estudos de prevalência
• Beneficiário: Vilma Leyton
• Modalidade de apoio: Auxílio à Pesquisa - Regular
• Processo FAPESP: 17/13882-2 - Drogas ilícitas em sangue: novas metodologias de análises toxicológicas
• Beneficiário: Henrique Silva Bombana
• Modalidade de apoio: Bolsas no Brasil - Doutorado