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%.
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