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

Author(s)

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

• Document type: Journal article
• Source: SEPARATION SCIENCE PLUS; v. N/A, p. 12-pg., 2023-08-07.

Abstract

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)

• FAPESP's process: 17/02147-0 - Single drop chromatography and its coupling to mass spectrometry: instrumental strategies, development of materials, automation and analytical applications
• Grantee: Fernando Mauro Lanças
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 20/00126-8 - Development of the methods of the microextraction hyphenated with LC-MS/MS or directly to MS/MS for the determination of biomarkers in biological samples of patient or rats with neurodegenerative diseases
• Grantee: Maria Eugênia Queiroz Nassur
• Support Opportunities: Regular Research Grants
• FAPESP's process: 19/04386-7 - Development of an organic monolithic phase for the determination of b-amyloid peptides AB40 and AB42 in plasma samples from patients with Alzheimer's Disease by UHPLC-MS/MS in column switching mode
• Grantee: Caroline Fernandes Grecco
• Support Opportunities: Scholarships in Brazil - Doctorate