In-tube solid-phase microextraction (sulfopropyl methacrylate-co-ethylene glycol dimethacrylate monolithic capillary) coupled to LC-MS/MS to determine beta amyloid peptides in Alzheimer's cerebrospinal fluid samples

Autor(es)

Grecco, Caroline Fernandes ; Tumas, Vitor ; Hallak, Jaime Eduardo Cecilio ; Queiroz, Maria Eugenia Costa

• Tipo de documento: Artigo Científico
• Fonte: SEPARATION SCIENCE PLUS; v. N/A, p. 12-pg., 2023-08-07.

Resumo

Alzheimer's disease (AD) is a neurodegenerative disorder characterized by an extracellular accumulation of amyloid beta peptides in the brain. The concentration of the amyloid beta peptides in cerebrospinal fluid (CSF) have been evaluated as potential biomarkers of AD for early diagnostic. In this work, an in-tube solid-phase microextraction (in-tube SPME) coupled to UHPLC-MS/MS method was established to determine amyloid beta peptides in CSF samples from AD patients. A strong cation-exchange (sulfopropyl methacrylate-co-ethylene glycol dimethacrylate) monolithic capillary was synthesized on the inner surface of a fused silica capillary and used as an extractive phase for in-tube SPME. The morphology and chemical structure of the monolithic phase were characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The proposed method presented linear range from the lower limits of quantification 0.6 and 0.8 to 10 ng mL(-1). Excluding the lower limits of quantification values, the analytical validation showed precision with the coefficient of variation values lower than 13.1%, and accuracy with relative standard deviation lower than 13.5%. The in-tube SPME coupled to UHPLC-MS/MS method was successfully applied to determine amyloid beta peptides in CSF samples from AD patients. (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: 20/00126-8 - Desenvolvimento de métodos de microextração hifenados à LC-MS/MS ou diretamente à MS/MS para a determinação de biomarcadores em amostras biológicas de pacientes ou de ratos com doenças neurodegenerativas
• Beneficiário: Maria Eugênia Queiroz Nassur
• Modalidade de apoio: Auxílio à Pesquisa - Regular
• Processo FAPESP: 19/04386-7 - Desenvolvimento de fase monolítica orgânica para determinação de peptídeos b-amilóide AB40 e AB42 em amostras de plasma de pacientes com a Doença de Alzheimer por UHPLC-MS/MS no modo column switching
• Beneficiário: Caroline Fernandes Grecco
• Modalidade de apoio: Bolsas no Brasil - Doutorado