Quantifying Citrate Surface Ligands on Iron Oxide Nanoparticles with TGA, CHN Analysis, NMR, and RP-HPLC with UV Detection
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| Názov: | Quantifying Citrate Surface Ligands on Iron Oxide Nanoparticles with TGA, CHN Analysis, NMR, and RP-HPLC with UV Detection |
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| Autori: | Anna Matiushkina, Sarah-Luise Abram, Isabella Tavernaro, Robert Richstein, Michael R. Reithofer, Elina Andresen, Matthias Michaelis, Matthias Koch, Ute Resch-Genger |
| Zdroj: | Analytical Chemistry. 97:19627-19634 |
| Informácie o vydavateľovi: | American Chemical Society (ACS), 2025. |
| Rok vydania: | 2025 |
| Predmety: | 104002 Analytische Chemie, 104002 Analytical chemistry, Iron, Ligands, High-performance liquid chromatography |
| Popis: | Although citrate is frequently used as a surface ligand for nanomaterials (NMs) such as metal, metal oxide, and lanthanide-based NMs in hydrophilic environments due to its biocompatibility and simple replacement by other more strongly binding ligands in postsynthetic surface modification reactions, its quantification on NM surfaces has rarely been addressed. Here, we present a multimethod approach for citrate quantification on iron oxide nanoparticles (IONPs) broadly applied in the life and material sciences. Methods explored include thermogravimetric (TGA) and elemental (CHN) analysis, providing citrate-nonspecific information on the IONP coating, simple photometry, and citrate-selective reversed-phase high-performance liquid chromatography (RP-HPLC) with absorption (UV) detection and quantitative nuclear magnetic resonance spectroscopy (qNMR). Challenges originating from the strongly absorbing magnetic NM and paramagnetic iron species interfering with optical and NMR methods were overcome by suitable sample preparation workflows. Our multimethod approach to citrate quantification highlights the advantages of combining specific and unspecific methods for characterizing NM surface chemistry and method cross-validation. It also demonstrates that chemically nonselective measurements can favor an overestimation of the amount of a specific surface ligand by signal contributions from molecules remaining on the NM surface, e.g., from particle synthesis, such as initially employed ligands and/or surfactants. Our results emphasize the potential of underexplored selective RP-HPLC for quantifying ligands on NMs, which does not require a multistep sample preparation workflow such as qNMR for many NMs and provides a higher sensitivity. These findings can pave the road to future applications of versatile HPLC methods in NM characterization. |
| Druh dokumentu: | Article |
| Jazyk: | English |
| ISSN: | 1520-6882 0003-2700 |
| DOI: | 10.1021/acs.analchem.5c03024 |
| DOI: | 10.17169/refubium-49631 |
| Prístupová URL adresa: | https://refubium.fu-berlin.de/handle/fub188/49906 https://doi.org/10.1021/acs.analchem.5c03024 https://doi.org/10.17169/refubium-49631 |
| Rights: | CC BY |
| Prístupové číslo: | edsair.doi.dedup.....8261093c7b5d0d4f40c451668d0515e6 |
| Databáza: | OpenAIRE |
Nájsť tento článok vo Web of Science | Abstrakt: | Although citrate is frequently used as a surface ligand for nanomaterials (NMs) such as metal, metal oxide, and lanthanide-based NMs in hydrophilic environments due to its biocompatibility and simple replacement by other more strongly binding ligands in postsynthetic surface modification reactions, its quantification on NM surfaces has rarely been addressed. Here, we present a multimethod approach for citrate quantification on iron oxide nanoparticles (IONPs) broadly applied in the life and material sciences. Methods explored include thermogravimetric (TGA) and elemental (CHN) analysis, providing citrate-nonspecific information on the IONP coating, simple photometry, and citrate-selective reversed-phase high-performance liquid chromatography (RP-HPLC) with absorption (UV) detection and quantitative nuclear magnetic resonance spectroscopy (qNMR). Challenges originating from the strongly absorbing magnetic NM and paramagnetic iron species interfering with optical and NMR methods were overcome by suitable sample preparation workflows. Our multimethod approach to citrate quantification highlights the advantages of combining specific and unspecific methods for characterizing NM surface chemistry and method cross-validation. It also demonstrates that chemically nonselective measurements can favor an overestimation of the amount of a specific surface ligand by signal contributions from molecules remaining on the NM surface, e.g., from particle synthesis, such as initially employed ligands and/or surfactants. Our results emphasize the potential of underexplored selective RP-HPLC for quantifying ligands on NMs, which does not require a multistep sample preparation workflow such as qNMR for many NMs and provides a higher sensitivity. These findings can pave the road to future applications of versatile HPLC methods in NM characterization. |
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| ISSN: | 15206882 00032700 |
| DOI: | 10.1021/acs.analchem.5c03024 |