Separation and quantification of silver nanoparticles and silver ions using reversed phase high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry in combination with isotope dilution analysis.
A reversed phase high performance liquid chromatography coupled to an inductively coupled plasma mass spectrometer (HPLC-ICP-MS) approach in combination with isotope dilution analysis (IDA) for the separation and parallel quantification of nanostructured and ionic silver (Ag) is presented. The main focus of this work was the determination of the ionic Ag concentration. For a sufficient stabilization of the ions without dissolving the nanoparticles (NPs), the eluent had to be initially optimized. The determined Ag ion concentration was in a good agreement with results obtained using ultrafiltration. Further, the mechanism of the NP separation in the HPLC column was investigated. Typical size exclusion effects were found by comparing results from columns with different pore sizes. Since the recovery rates decreased with increasing Ag NP size and large Ag NPs did not elute from the column, additional interactions of the particles with the stationary phase were assumed. Our results reveal that the presented method is not only applicable to Ag NPs, but also to gold and polystyrene NPs. Finally, IDA-HPLC-ICP-MS experiments in single particle mode were performed to determine the particle cut-off size. The comparison with conventional spICP-MS experiments resulted in a similar diameter and particle size distribution.
Bundesanstalt für Materialforschung und - prüfung (BAM), Richard-Willstätter-Str. 11, D-12489 Berlin, Germany.
Carina A
CA
Sötebier
Bundesanstalt für Materialforschung und - prüfung (BAM), Richard-Willstätter-Str. 11, D-12489 Berlin, Germany. Electronic address: steffen.weidner@bam.de.
Steffen M
SM
Weidner
Bundesanstalt für Materialforschung und - prüfung (BAM), Richard-Willstätter-Str. 11, D-12489 Berlin, Germany.
Norbert
N
Jakubowski
Bundesanstalt für Materialforschung und - prüfung (BAM), Richard-Willstätter-Str. 11, D-12489 Berlin, Germany; Humboldt-Universität zu Berlin, Department of Chemistry, Brook-Taylor-Str. 2, D-12489 Berlin, Germany.
Ulrich
U
Panne
University of Oviedo, Department of Physical and Analytical Chemistry, C/Julián Clavería 8, E-33006 Oviedo, Spain. Electronic address: bettmerjorg@uniovi.es.
Jörg
J
Bettmer
D002623:Chemistry Techniques, Analytical / Q000295:instrumentation / Q000379:methods*; D056148:Chromatography, Reverse-Phase; D006046:Gold / Q000032:analysis / Q000302:isolation & purification; D007477:Ions / Q000032:analysis / Q000302:isolation & purification; D007554:Isotopes / Q000737:chemistry; D013058:Mass Spectrometry; D053768:Metal Nanoparticles / Q000032:analysis*; D010316:Particle Size; D012834:Silver / Q000032:analysis*; D013057:Spectrum Analysis
D007477:Ions; D007554:Isotopes; D012834:Silver; D006046:Gold
High performance liquid chromatography; ICP-MS; Isotope dilution analysis; Separation mechanism; Silver nanoparticles; Speciation