Abstract
A method for determining the size of silver nanoparticles and their quantification by asymmetric flow field-flow fractionation coupled with inductively coupled plasma mass spectrometry (ICP-MS) is proposed and was tested in consumer products. Experimental conditions were studied in detail to avoid aggregation processes or alteration of the original size distributions. Additionally, losses from sorption processes onto the channel membrane were minimized for correct quantification of the nanoparticles. Mobile phase composition, injection/focusing, and fractionation conditions were evaluated in terms of their influence on both separation resolution and recovery. The ionic strength, pH, and the presence of ionic and nonionic surfactants had a strong influence on both separation and recovery of the nanoparticles. In general, better results were obtained under those conditions that favored charge repulsions with the membrane. Recovery values of 83 ± 8% and 93 ± 4% with respect to the content of silver nanoparticles were achieved for the consumer products studied. Silver nanoparticle standards were used for size calibration of the channel. The results were compared with those obtained by photon correlation spectroscopy and images taken by transmission electron microscopy. The quantification of silver nanoparticles was performed by direct injection of ionic silver standard solutions into the ICP-MS system, integration of the corresponding peaks, and interpolation of the fractogram area. A limit of detection of 5.6 μg L-1 silver, which corresponds to a number concentration of 1×1012 L-1 for nanoparticles of 10 nm, was achieved for an injection volume of 20 μL.
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Acknowledgements
This work was sponsored by the Spanish Ministry of Science and Innovation (project CTQ2009-14237-C02-01). The authors also thank Laboratorios Argenol S.L. for providing the Collargol samples, Gemma Cepria for the differential pulse anodic stripping voltammetry measurements, and Yolanda Rodas from the Institute of Nanoscience of Aragon for the PCS and zeta potential measurements. ICP-MS measurements were performed in the facilities of the Analytical Central Laboratory of the University of Zaragoza.
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Published in the special issue Plasma Spectrochemistry with Guest Editors Juan Castillo and Martín Resano.
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Bolea, E., Jiménez-Lamana, J., Laborda, F. et al. Size characterization and quantification of silver nanoparticles by asymmetric flow field-flow fractionation coupled with inductively coupled plasma mass spectrometry. Anal Bioanal Chem 401, 2723–2732 (2011). https://doi.org/10.1007/s00216-011-5201-2
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DOI: https://doi.org/10.1007/s00216-011-5201-2