Influence of Sample Preparation on SERS Signal

Carbendazim (MBC), a commonly used fungicide from the benzimidazole group, was applied in this study as a probe molecule to understand the influence of sample preparation on the SERS (surface-enhanced Raman scattering) signal. We applied the external standard method (ESM), preparing fresh Ag colloid...

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Main Authors: Isabela Bianchi-Carvalho, Marcelo José dos Santos Oliveira, Cibely Silva Martin, Santiago Sánchez-Cortés, Carlos José Leopoldo Constantino
Format: Article
Language:English
Published: MDPI AG 2025-01-01
Series:Chemosensors
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Online Access:https://www.mdpi.com/2227-9040/13/1/22
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author Isabela Bianchi-Carvalho
Marcelo José dos Santos Oliveira
Cibely Silva Martin
Santiago Sánchez-Cortés
Carlos José Leopoldo Constantino
author_facet Isabela Bianchi-Carvalho
Marcelo José dos Santos Oliveira
Cibely Silva Martin
Santiago Sánchez-Cortés
Carlos José Leopoldo Constantino
author_sort Isabela Bianchi-Carvalho
collection DOAJ
description Carbendazim (MBC), a commonly used fungicide from the benzimidazole group, was applied in this study as a probe molecule to understand the influence of sample preparation on the SERS (surface-enhanced Raman scattering) signal. We applied the external standard method (ESM), preparing fresh Ag colloid samples (reduced by hydroxylamine) for each concentration and measuring with and without potassium nitrate (KNO₃) as an aggregation-inducing salt. The impact of sample dilution before or after the addition of the salt to the Ag colloid was also explored. SERS signals were correlated with Ag colloid aggregation observed via transmission electron microscopy (TEM), UV-Vis extinction, dynamic light scattering (DLS), and zeta potential, examining diffusion-limited cluster aggregation (DLCA) and reaction-limited cluster aggregation (RLCA) mechanisms. The optimal results were achieved without KNO₃, with more compact aggregates at lower concentrations and more branched ones at higher concentrations. Dilution of the Ag colloid before salt addition enabled lower detection limits than without any dilution. No SERS signal was observed when the salt was added before dilution. These findings emphasize that a consistent relationship between aggregate morphology and the SERS signal cannot be generalized across analytes. Analyte-specific properties play a crucial role in determining optimal aggregation conditions for SERS analysis.
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spelling doaj-art-9a67378978ad4934b91cf1a9c7bc9bb32025-01-24T13:26:55ZengMDPI AGChemosensors2227-90402025-01-011312210.3390/chemosensors13010022Influence of Sample Preparation on SERS SignalIsabela Bianchi-Carvalho0Marcelo José dos Santos Oliveira1Cibely Silva Martin2Santiago Sánchez-Cortés3Carlos José Leopoldo Constantino4School of Technology and Sciences, São Paulo State University (UNESP), Presidente Prudente 19060-900, SP, BrazilSchool of Technology and Sciences, São Paulo State University (UNESP), Presidente Prudente 19060-900, SP, BrazilSchool of Engineering, São Paulo State University (UNESP), Ilha Solteira 15385-007, SP, BrazilInstituto de Estructura de la Materia, Instituto de Estructura de la Materia-Consejo Superior de Investigaciones Científicas (IEM-CSIC), 28006 Madrid, SpainSchool of Technology and Sciences, São Paulo State University (UNESP), Presidente Prudente 19060-900, SP, BrazilCarbendazim (MBC), a commonly used fungicide from the benzimidazole group, was applied in this study as a probe molecule to understand the influence of sample preparation on the SERS (surface-enhanced Raman scattering) signal. We applied the external standard method (ESM), preparing fresh Ag colloid samples (reduced by hydroxylamine) for each concentration and measuring with and without potassium nitrate (KNO₃) as an aggregation-inducing salt. The impact of sample dilution before or after the addition of the salt to the Ag colloid was also explored. SERS signals were correlated with Ag colloid aggregation observed via transmission electron microscopy (TEM), UV-Vis extinction, dynamic light scattering (DLS), and zeta potential, examining diffusion-limited cluster aggregation (DLCA) and reaction-limited cluster aggregation (RLCA) mechanisms. The optimal results were achieved without KNO₃, with more compact aggregates at lower concentrations and more branched ones at higher concentrations. Dilution of the Ag colloid before salt addition enabled lower detection limits than without any dilution. No SERS signal was observed when the salt was added before dilution. These findings emphasize that a consistent relationship between aggregate morphology and the SERS signal cannot be generalized across analytes. Analyte-specific properties play a crucial role in determining optimal aggregation conditions for SERS analysis.https://www.mdpi.com/2227-9040/13/1/22aggregation mechanismcarbendazimSERSdetection
spellingShingle Isabela Bianchi-Carvalho
Marcelo José dos Santos Oliveira
Cibely Silva Martin
Santiago Sánchez-Cortés
Carlos José Leopoldo Constantino
Influence of Sample Preparation on SERS Signal
Chemosensors
aggregation mechanism
carbendazim
SERS
detection
title Influence of Sample Preparation on SERS Signal
title_full Influence of Sample Preparation on SERS Signal
title_fullStr Influence of Sample Preparation on SERS Signal
title_full_unstemmed Influence of Sample Preparation on SERS Signal
title_short Influence of Sample Preparation on SERS Signal
title_sort influence of sample preparation on sers signal
topic aggregation mechanism
carbendazim
SERS
detection
url https://www.mdpi.com/2227-9040/13/1/22
work_keys_str_mv AT isabelabianchicarvalho influenceofsamplepreparationonserssignal
AT marcelojosedossantosoliveira influenceofsamplepreparationonserssignal
AT cibelysilvamartin influenceofsamplepreparationonserssignal
AT santiagosanchezcortes influenceofsamplepreparationonserssignal
AT carlosjoseleopoldoconstantino influenceofsamplepreparationonserssignal