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

Author(s)

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

Affiliation

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

• Document type: Journal article
• Source: JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES; v. 1139, FEB 15 2020.
• Web of Science Citations: 0

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 (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)

• FAPESP's process: 16/20214-3 - Verification of drugs and medicines consume by professional drivers using toxicological analysis of oral fluid: development of new analytical methods and prevalence studies
• Grantee: Vilma Leyton
• Support Opportunities: Regular Research Grants
• FAPESP's process: 17/13882-2 - Illicit drugs in blood samples: new methodologies for toxicological analysis
• Grantee: Henrique Silva Bombana
• Support Opportunities: Scholarships in Brazil - Doctorate