Determination of ring-substituted amphetamines through automated online hollow fiber liquid-phase microextraction-liquid chromatography

Autor(es)

Rodriguez Cabal, Luis Felipe ^[1] ; Vargas Medina, Deyber Arley ^[1] ; Costa, Jose Luiz ^[2] ; Lancas, Fernando Mauro ^[1] ; Santos-Neto, Alvaro Jose ^[1]

Afiliação do(s) autor(es)

^[1] Univ Sao Paulo, Sao Carlos Inst Chem, BR-13566590 Sao Carlos, SP - Brazil

^[2] Univ Estadual Campinas, Fac Pharmaceut Sci, BR-13083859 Campinas, SP - Brazil

• Tipo de documento: Artigo Científico
• Fonte: ANALYTICAL AND BIOANALYTICAL CHEMISTRY; v. 411, n. 29, p. 7889-7897, NOV 2019.
• Citações Web of Science: 0

Resumo

The present paper describes an original method for the online preconcentration and analysis of ring-substituted amphetamines in urine samples, used on the integration of robot-assisted hollow fiber liquid-phase microextraction (HF-LPME), high-performance liquid chromatography (HPLC), and fluorescence detection (FLD). A lab-made autosampler, actuating a 100-mu L syringe and equipped with a three-way solenoid microvalve, allowed the acceptor phase to flow through and be withdrawn from the lumen fiber, enabling the automated online transference of the enriched acceptor phase for chromatographic analysis, through a six-port switching valve. The developed online HF-LPME-LC/FLD method demonstrated high analytical throughput and confidence, facilitating the efficient extraction and determination of the target analytes, with minimal solvent consumption and sample manipulation, in a straightforward way. Sample cleanup, analyte uptake, and analysis were carried out in 14.5 min. Under optimal conditions, automated online HF-LPME showed excellent linearity, precision, and trueness, obtaining intraday RSDs between 2.9 and 9.2% (n = 6) and interday RSDs between 5.3 and 9.3% (n = 6). Enrichment factors (EFs) ranged between 14.2 and 15.7, extraction recoveries (ERs) ranged between 17.7 and 19.5%, and the limits of detection (S/N = 3) were 2.0, 3.0, and 3.0 mu g L-1 for MDA, MDMA, and MDEA, respectively. The method proved to be an effortless, rapid, reliable, and environment-friendly approach for the determination of drug abuse in urine samples. (AU)

• Processo FAPESP: 17/02147-0 - Cromatografia líquida em uma gota e seu acoplamento com espectrometria de massas: estratégias instrumentais, desenvolvimento de materiais, automatização e aplicações analíticas
• Beneficiário: Fernando Mauro Lanças
• Modalidade de apoio: Auxílio à Pesquisa - Temático
• Processo FAPESP: 18/00432-1 - A Toxicologia das Novas Substâncias Psicoativas (NSP): epidemiologia do consumo através da análise de amostras de cabelo e fluido oral
• Beneficiário: José Luiz da Costa
• Modalidade de apoio: Auxílio à Pesquisa - Regular
• Processo FAPESP: 16/21950-5 - Estratégias automatizadas para preparo de amostras miniaturizado: SDME com agitação na seringa e integração online com a cromatografia líquida
• Beneficiário: Deyber Arley Vargas Medina
• Modalidade de apoio: Bolsas no Exterior - Estágio de Pesquisa - Doutorado
• Processo FAPESP: 10/19910-9 - Desenvolvimento de estratégias de química verde em cromatografia e aplicação na avaliação da degradação de antibióticos em águas residuárias por biorreatores anaeróbios de leito fixo
• Beneficiário: Alvaro José dos Santos Neto
• Modalidade de apoio: Auxílio à Pesquisa - Regular