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Open AccessArticle
Optimisation of a Microwave Synthesis of Silver Nanoparticles by a Quality by Design Approach to Improve SERS Analytical Performances
by
Julie Horne
Julie Horne 1,*,
Pierre Beckers
Pierre Beckers 1,
Pierre-Yves Sacré
Pierre-Yves Sacré
Dr. Pierre-Yves Sacré is a Senior Scientist at the Department of Pharmaceutical Sciences, of He his [...]
Dr. Pierre-Yves Sacré is a Senior Scientist at the Department of Pharmaceutical Sciences, University of Liège. He completed his PhD studies in Pharmaceuticals (Analytical Chemistry) at the University of Liège in 2011. He is the author or coauthor of more than 75 paper with an H index of 25. His interests include Pharmaceutical Analysis, Vibrational Spectroscopy, Hyperspectral Imaging; Chemometrics, Substandard and Falsified Medicines Detection, and Analytical Chemistry Instrumentation.
2,*,
Charlotte De Bleye
Charlotte De Bleye 1,
Pierre Francotte
Pierre Francotte
Dr. Pierre Francotte is currently an Associate Professor in the Medicinal Chemistry Laboratory, of a [...]
Dr. Pierre Francotte is currently an Associate Professor in the Medicinal Chemistry Laboratory, Department of Pharmaceutical Sciences, University of Liège. He is a pharmacist by training, and obtained his Master’s degree in Pharmaceutical Sciences at the University of Liège in 2003, his Master’s degree in Drug Design at the École nationale supérieure de chimie de Lille in 2006, and his PhD degree in Biomedical and Pharmaceutical Sciences at the University of Liège in 2008. His research interests include the design/synthesis of AMPA/KA positive allosteric modulators and the structure diversification/optimization of natural products using a total synthesis approach.
3,
Nicolas Thelen
Nicolas Thelen 4,
Philippe Hubert
Philippe Hubert 1,
Eric Ziemons
Eric Ziemons
Dr. Eric Ziemons is a Professor of Green Analytical Chemistry and Vice-Director of the Center for on [...]
Dr. Eric Ziemons is a Professor of Green Analytical Chemistry and Vice-Director of the Center for Interdisciplinary Research on Medicines (CIRM) at the University of Liège (ULiege). He received his Ph.D. in Pharmaceutical Sciences in 2006 under the supervision of Professor Philippe Hubert. He is the author or co-author of more than 120 peer-reviewed articles. His research interests cover both vibrational spectroscopy and hyperspectral imaging applied to the pharmaceutical and biomedical fields, with a particular focus on data processing and surface-enhanced Raman scattering for trace determination in complex media.
1,† and
Cédric Hubert
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
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.
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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