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Analytical characterization of gold nanoparticle primary particles, aggregates, agglomerates, and agglomerated aggregates

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Abstract

Gold nanoparticles have been studied for many biomedical applications. However, alterations in the gold nanoparticles’ environment frequently lead to the formation of aggregates and agglomerates, which have not been well characterized. These new structures could significantly change the biological impact of the nanoparticles, so the appropriate characterization of these structures prior to biological administration is vital for the correct interpretation of toxicology results. By varying the solvent or heating under pressure, four reproducible gold nanoparticles structures were created: 10 nm primary particles, aggregates of the primary particles that contain non-reversible bonds between the individual nanoparticles, agglomerates of primary particles that contain reversible interactions between the individual nanoparticles, and agglomerated aggregates that have reversible bonds linking individual aggregates. Ultraviolet–visible (UV–Vis) spectroscopy, thermal gravitational analysis, and neutron activation analysis were each found to accurately measure the concentration of the primary particles. The primary particles measured 10 nm by dynamic light scattering (DLS) and had a spherical morphology by transmission electron microscopy (TEM) while the aggregates measured 110 nm by DLS and had a distorted morphology by TEM. The agglomerate and aggregated agglomerate samples both measured >1,000 nm by DLS, but the individual particles had significantly different morphologies by TEM. Multiple other analytical techniques, including ultracentrifugation, gel electrophoresis, and X-ray diffraction, also showed unique traits for each structure. The structural differences did not change in the presence of cell culture media or rat serum. In addition, the primary particles, aggregates, and agglomerates each had a unique UV–Vis spectrum, allowing for an inexpensive, rapid method to differentiate between the structures.

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Acknowledgments

The authors acknowledge Dr. Rodney Rouse, FDA, for providing the rat serum samples, Dr. Beni Dair, FDA, for TEM assistance, Jeff Davis, National Institutes of Standards and Technology, for the use of his XRD and standards, and the Office of Science and Engineering Laboratories, FDA, for the use of their TEM and TGA. This project was supported in part by an appointment to the Research Participation Program at the Center for Drug Evaluation and Research administered by the Oak Ridge Institute for Science and Education through an interagency agreement between the U.S. Department of Energy and the U.S. Food and Drug Administration. The findings and conclusions in this article have not been formally disseminated by the Food and Drug Administration and should not be construed to represent any Agency determination or policy. The mention of commercial products, their sources, or their use in connection with material reported herein is not to be construed as either an actual or implied endorsement of such products by the Department of Health and Human Services.

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Authors and Affiliations

  1. Center for Drug Evaluation and Research, FDA, Bldg 64, Rm 2086, 10903 New Hampshire Ave., Silver Spring, MD, 20993, USA

    Athena M. Keene & Katherine M. Tyner

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  1. Athena M. Keene
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  2. Katherine M. Tyner
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Correspondence to Katherine M. Tyner.

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The findings and conclusions in this article have not been formally disseminated by the Food and Drug Administration and should not be construed to represent any Agency determination or policy. The mention of commercial products, their sources, or their use in connection with material reported herein is not to be construed as either an actual or implied endorsement of such products by the Department of Health and Human Services.

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Keene, A.M., Tyner, K.M. Analytical characterization of gold nanoparticle primary particles, aggregates, agglomerates, and agglomerated aggregates. J Nanopart Res 13, 3465–3481 (2011). https://doi.org/10.1007/s11051-011-0268-4

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  • DOI: https://doi.org/10.1007/s11051-011-0268-4

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