Disposable Pipette Extraction Followed by Direct MS/MS Analysis of Beta Amyloid Peptides (Aß38, Aß40, and Aβ42) in Cerebrospinal Fluid Samples

Author(s)

Caroline F. Grecco ^[1] ; Eduardo José Crevelin ^[2] ; Vitor Tumas ^[3] ; Jaime Eduardo C. Hallak ^[4] ; Maria Eugênia C. Queiroz ^[5]

Affiliation

^[1] Universidade de São Paulo. Departamento de Química de Ribeirão Preto. Faculdade de Filosofia - Brasil

^[2] Universidade de São Paulo. Departamento de Química de Ribeirão Preto. Faculdade de Filosofia - Brasil

^[3] Universidade de São Paulo. Departamento de Neurociências e Ciências do Comportamento. Faculdade de Medicina de Ribeirão Preto - Brasil

^[4] Universidade de São Paulo. Departamento de Neurociências e Ciências do Comportamento. Faculdade de Medicina de Ribeirão Preto - Brasil

^[5] Universidade de São Paulo. Departamento de Química de Ribeirão Preto. Faculdade de Filosofia - Brasil

• Document type: Journal article
• Source: Journal of the Brazilian Chemical Society; v. 36, n. 1 2024-06-17.

Abstract

Alzheimer’s disease (AD) is a neurodegenerative disorder characterized by extracellular accumulation of amyloid-β (Aβ) peptides in the brain. This study demonstrates the direct association of the disposable pipette extraction (DPX) with tandem mass spectrometry (MS/MS) for the analysis of Aβ peptides in cerebrospinal fluid (CSF) samples. Different parameters were optimized in order to improve detectability in the MS/MS including mobile phase percentage of ammonium hydroxide, mobile phase flow rate and acquisition mode. Also, this method used an electrospray ionization (ESI) low-flow probe and direct infusion of an organic solution in the MS/MS. The DPX-MS/MS method showed adequate linearity for determining Aβ peptides in CSF-linearity ranged from 0.1 to 1.5 ng mL 1. The coefficients of determination were higher than 0.99; the precision coefficient of variation (CV) ranged from 0.3 to 12.7%; and the accuracy relative standard deviation (RSD) ranged from -13.6 to 13.2%. (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: 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
• 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