Autor(es)

dos Santos, Natalia Gabrielly Pereira ; Medina, Deyber Arley Vargas ; Lancas, Fernando Mauro

• Tipo de documento: Artigo Científico
• Fonte: ANALYTICAL AND BIOANALYTICAL CHEMISTRY; v. N/A, p. 10-pg., 2024-08-10.

Resumo

Water, renowned for its sustainability and minimal toxicity, is an ideal candidate for environmentally friendly solvent-based microextraction. However, its potential as an extractant solvent in miniaturized sample preparation remains largely unexplored. This paper pioneers using water as the extraction solvent in headspace single-drop microextraction (HS-SDME) for N-nitrosamines from losartan tablets. Autonomous HS-SDME is executed by an Arduino-controlled, lab-made Cartesian robot, using water for the online preconcentration of enriched extracts through direct injection into a column-switching system. Critical experimental parameters influencing HS-SDME performance are systematically explored through univariate and multivariate experiments. While most previously reported methods for determining N-nitrosamines in pharmaceutical formulations rely on highly selective mass spectrometry detection techniques to handle the strong matrix effects typical of pharmaceutical samples, the water-based HS-SDME method efficiently eliminates the interfering effects of a large amount of the pharmaceutical active ingredient and tablet excipients, allowing straightforward analysis using high-performance liquid chromatography with ultraviolet detection (HPLC-UV-Vis). Under optimized conditions, the developed method exhibits linear responses from 100 to 2400 ng g-1, demonstrating appropriate detectability, precision, and accuracy for the proposed application. Additionally, the environmental sustainability of the method is assessed using the AGREEprep methodology, positioning it as an outstanding green alternative for determining hazardous contaminants in pharmaceutical products. (AU)

• Processo FAPESP: 19/22724-7 - Novas estratégias instrumentais no desenvolvimento de métodos analíticos automatizados e miniaturizados para a determinação de compostos orgânicos mediante cromatografia líquida acoplada a espectrometria de massas
• Beneficiário: Deyber Arley Vargas Medina
• Modalidade de apoio: Bolsas no Brasil - Pós-Doutorado
• 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: 15/15462-5 - Emprego do grafeno como material sorvente em técnicas miniaturizadas de preparo de amostra.
• Beneficiário: Bruno Henrique Fumes
• Modalidade de apoio: Bolsas no Brasil - Doutorado