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Article

Optimisation of a Microwave Synthesis of Silver Nanoparticles by a Quality by Design Approach to Improve SERS Analytical Performances

by
Julie Horne
1,*,
Pierre Beckers
1,
Pierre-Yves Sacré
2,*,
Charlotte De Bleye
1,
Pierre Francotte
3,
Nicolas Thelen
4,
Philippe Hubert
1,
Eric Ziemons
1,† and
Cédric Hubert
1,†
1
Laboratory of Pharmaceutical Analytical Chemistry, Department of Pharmacy, CIRM, ViBra-Sante Hub, University of Liege (ULiege), 4000 Liege, Belgium
2
Research Support Unit in Chemometrics, Department of Pharmacy, CIRM, University of Liege (ULiege), 4000 Liege, Belgium
3
Laboratory of Medicinal Chemistry, Department of Pharmacy, CIRM, University of Liege (ULiege), 4000 Liege, Belgium
4
GIGA-Neurosciences, Cell Biology, University of Liege (ULiege), 4000 Liege, Belgium
*
Authors to whom correspondence should be addressed.
These authors contributed equally to this work.
Molecules 2024, 29(14), 3442; https://doi.org/10.3390/molecules29143442 (registering DOI)
Submission received: 17 May 2024 / Revised: 19 July 2024 / Accepted: 19 July 2024 / Published: 22 July 2024
(This article belongs to the Section Green Chemistry)

Abstract

A major limitation preventing the use of surface-enhanced Raman scattering (SERS) in routine analyses is the signal variability due to the heterogeneity of metallic nanoparticles used as SERS substrates. This study aimed to robustly optimise a synthesis process of silver nanoparticles to improve the measured SERS signal repeatability and the protocol synthesis repeatability. The process is inspired by a chemical reduction method associated with microwave irradiation to guarantee better controlled and uniform heating. The innovative Quality by Design strategy was implemented to optimise the different parameters of the process. A preliminary investigation design was firstly carried out to evaluate the influence of four parameters selected by means of an Ishikawa diagram. The critical quality attributes were to maximise the intensity of the SERS response and minimise its variance. The reaction time, temperature and stirring speed are critical process parameters. These were optimised using an I-optimal design. A robust operating zone covering the optimal reaction conditions (3.36 min–130 °C–600 rpm) associated with a probability of success was modelled. Validation of this point confirmed the prediction with intra- and inter-batch variabilities of less than 15%. In conclusion, this study successfully optimised silver nanoparticles by a rapid, low cost and simple technique enhancing the quantitative perspectives of SERS.
Keywords: surface enhanced Raman scattering (SERS); silver nanoparticle synthesis; process optimisation; Quality by Design (QbD); microwave surface enhanced Raman scattering (SERS); silver nanoparticle synthesis; process optimisation; Quality by Design (QbD); microwave

Share and Cite

MDPI and ACS Style

Horne, J.; Beckers, P.; Sacré, P.-Y.; De Bleye, C.; Francotte, P.; Thelen, N.; Hubert, P.; Ziemons, E.; Hubert, C. Optimisation of a Microwave Synthesis of Silver Nanoparticles by a Quality by Design Approach to Improve SERS Analytical Performances. Molecules 2024, 29, 3442. https://doi.org/10.3390/molecules29143442

AMA Style

Horne J, Beckers P, Sacré P-Y, De Bleye C, Francotte P, Thelen N, Hubert P, Ziemons E, Hubert C. Optimisation of a Microwave Synthesis of Silver Nanoparticles by a Quality by Design Approach to Improve SERS Analytical Performances. Molecules. 2024; 29(14):3442. https://doi.org/10.3390/molecules29143442

Chicago/Turabian Style

Horne, Julie, Pierre Beckers, Pierre-Yves Sacré, Charlotte De Bleye, Pierre Francotte, Nicolas Thelen, Philippe Hubert, Eric Ziemons, and Cédric Hubert. 2024. "Optimisation of a Microwave Synthesis of Silver Nanoparticles by a Quality by Design Approach to Improve SERS Analytical Performances" Molecules 29, no. 14: 3442. https://doi.org/10.3390/molecules29143442

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