Development and Application of an In-Capillary CE-DAD Method for the Inhibitory Screening of Natural Extracts Towards Acetylcholinesterase Enzyme

<b>Background:</b> The enzymatic activity of acetylcholinesterase (AChE) has been a focal point in neurodegenerative diseases research, particularly in relation to Alzheimer’s disease. This is attributed to the significantly reduced levels of cholinergic neurons observed in Alzheimer’s p...

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Main Authors: Francesca Rinaldi, Sofia Salerno, Elena Frigoli, Giulia De Soricellis, Gloria Brusotti, Stefano Negri, Matteo Radice, Francesca Merlo, Andrea Speltini, Hellas Cena, Enrica Calleri
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Language:English
Published: MDPI AG 2025-04-01
Series:Metabolites
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Online Access:https://www.mdpi.com/2218-1989/15/4/283
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author Francesca Rinaldi
Sofia Salerno
Elena Frigoli
Giulia De Soricellis
Gloria Brusotti
Stefano Negri
Matteo Radice
Francesca Merlo
Andrea Speltini
Hellas Cena
Enrica Calleri
author_facet Francesca Rinaldi
Sofia Salerno
Elena Frigoli
Giulia De Soricellis
Gloria Brusotti
Stefano Negri
Matteo Radice
Francesca Merlo
Andrea Speltini
Hellas Cena
Enrica Calleri
author_sort Francesca Rinaldi
collection DOAJ
description <b>Background:</b> The enzymatic activity of acetylcholinesterase (AChE) has been a focal point in neurodegenerative diseases research, particularly in relation to Alzheimer’s disease. This is attributed to the significantly reduced levels of cholinergic neurons observed in Alzheimer’s patients compared to healthy individuals. The strategy to mitigate the onset of these diseases in patients lies in the exploration of new potential AChE inhibitors with a focus also on natural extracts. A rapid and specific capillary electrophoresis method with direct ultraviolet detection (CZE-UV/Vis) was developed to screen natural extracts by assessing their potential to inhibit AChE. <b>Materials and Methods:</b> To enhance the specificity when analysing complex matrixes such as natural extracts, a sequential analysis approach based on the “sandwich model” was implemented using Ellman’s reagent [5,5′-dithiobis-(2-nitrobenzoic acid)] (DTNB) as a colorimetric indicator. <b>Results:</b> A reference inhibitor, neostigmine, was used for system validation through IC<sub>50</sub> and K<sub>i</sub> values determination by subsequent injections of acetylthiocholine substrate in the presence of neostigmine at increasing concentrations, and the enzyme combined with DTNB in borate-phosphate buffer (30 mM, pH 8.0). The enzymatic product was selectively detected at 412 nm. The validated system was applied to the analysis of seven natural extracts. <b>Conclusions:</b> Results demonstrated promising outcomes for identifying phytotherapeutic agents with potential applications in the prevention of neurodegenerative diseases. This method provides high selectivity and automation, offering a streamlined and effective approach for screening natural matrices containing potential AChE inhibitors.
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spelling doaj-art-c44f40e203af44a18a744a6fc446471f2025-08-20T02:18:19ZengMDPI AGMetabolites2218-19892025-04-0115428310.3390/metabo15040283Development and Application of an In-Capillary CE-DAD Method for the Inhibitory Screening of Natural Extracts Towards Acetylcholinesterase EnzymeFrancesca Rinaldi0Sofia Salerno1Elena Frigoli2Giulia De Soricellis3Gloria Brusotti4Stefano Negri5Matteo Radice6Francesca Merlo7Andrea Speltini8Hellas Cena9Enrica Calleri10Department of Drug Sciences, University of Pavia, Viale Taramelli 12, 27100 Pavia, ItalyDepartment of Drug Sciences, University of Pavia, Viale Taramelli 12, 27100 Pavia, ItalyDepartment of Drug Sciences, University of Pavia, Viale Taramelli 12, 27100 Pavia, ItalyDepartment of Drug Sciences, University of Pavia, Viale Taramelli 12, 27100 Pavia, ItalyDepartment of Drug Sciences, University of Pavia, Viale Taramelli 12, 27100 Pavia, ItalyNational Biodiversity Future Center (NBFC), 90133 Palermo, ItalyCampus Puyo, Universidad Estatal Amazónica, Km 2, Via Puyo-Tena, Puyo 160150, EcuadorDepartment of Chemistry, University of Pavia, Via Taramelli 12, 27100 Pavia, ItalyDepartment of Chemistry, University of Pavia, Via Taramelli 12, 27100 Pavia, ItalyNational Biodiversity Future Center (NBFC), 90133 Palermo, ItalyDepartment of Drug Sciences, University of Pavia, Viale Taramelli 12, 27100 Pavia, Italy<b>Background:</b> The enzymatic activity of acetylcholinesterase (AChE) has been a focal point in neurodegenerative diseases research, particularly in relation to Alzheimer’s disease. This is attributed to the significantly reduced levels of cholinergic neurons observed in Alzheimer’s patients compared to healthy individuals. The strategy to mitigate the onset of these diseases in patients lies in the exploration of new potential AChE inhibitors with a focus also on natural extracts. A rapid and specific capillary electrophoresis method with direct ultraviolet detection (CZE-UV/Vis) was developed to screen natural extracts by assessing their potential to inhibit AChE. <b>Materials and Methods:</b> To enhance the specificity when analysing complex matrixes such as natural extracts, a sequential analysis approach based on the “sandwich model” was implemented using Ellman’s reagent [5,5′-dithiobis-(2-nitrobenzoic acid)] (DTNB) as a colorimetric indicator. <b>Results:</b> A reference inhibitor, neostigmine, was used for system validation through IC<sub>50</sub> and K<sub>i</sub> values determination by subsequent injections of acetylthiocholine substrate in the presence of neostigmine at increasing concentrations, and the enzyme combined with DTNB in borate-phosphate buffer (30 mM, pH 8.0). The enzymatic product was selectively detected at 412 nm. The validated system was applied to the analysis of seven natural extracts. <b>Conclusions:</b> Results demonstrated promising outcomes for identifying phytotherapeutic agents with potential applications in the prevention of neurodegenerative diseases. This method provides high selectivity and automation, offering a streamlined and effective approach for screening natural matrices containing potential AChE inhibitors.https://www.mdpi.com/2218-1989/15/4/283Alzheimer’s diseaseplant extractscapillary electrophoresis
spellingShingle Francesca Rinaldi
Sofia Salerno
Elena Frigoli
Giulia De Soricellis
Gloria Brusotti
Stefano Negri
Matteo Radice
Francesca Merlo
Andrea Speltini
Hellas Cena
Enrica Calleri
Development and Application of an In-Capillary CE-DAD Method for the Inhibitory Screening of Natural Extracts Towards Acetylcholinesterase Enzyme
Metabolites
Alzheimer’s disease
plant extracts
capillary electrophoresis
title Development and Application of an In-Capillary CE-DAD Method for the Inhibitory Screening of Natural Extracts Towards Acetylcholinesterase Enzyme
title_full Development and Application of an In-Capillary CE-DAD Method for the Inhibitory Screening of Natural Extracts Towards Acetylcholinesterase Enzyme
title_fullStr Development and Application of an In-Capillary CE-DAD Method for the Inhibitory Screening of Natural Extracts Towards Acetylcholinesterase Enzyme
title_full_unstemmed Development and Application of an In-Capillary CE-DAD Method for the Inhibitory Screening of Natural Extracts Towards Acetylcholinesterase Enzyme
title_short Development and Application of an In-Capillary CE-DAD Method for the Inhibitory Screening of Natural Extracts Towards Acetylcholinesterase Enzyme
title_sort development and application of an in capillary ce dad method for the inhibitory screening of natural extracts towards acetylcholinesterase enzyme
topic Alzheimer’s disease
plant extracts
capillary electrophoresis
url https://www.mdpi.com/2218-1989/15/4/283
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