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1.
Anal Bioanal Chem ; 2024 May 10.
Artigo em Inglês | MEDLINE | ID: mdl-38724776

RESUMO

A multimodal approach combining inductively coupled plasma mass spectrometry (ICP-MS), single-particle ICP-MS (spICP-MS), scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDS) and Raman spectroscopy enabled a deeper insight into the balance between total titanium (Ti), the soluble titanium fraction and titanium dioxide based particle fraction levels in periprosthetic tissues collected from patients undergoing revision surgery. Hydrofluoric acid usage in the sample digestion allowed for complete digestion of TiO2 particles, thus enabling accurate estimation of total Ti levels. The TiO2 fraction represents 38-94% of the titanium load in the six samples where particles were detected, and the fraction is present mainly in samples from patients with aseptically loosened total hip arthroplasty. Further attention was given to this fraction determining the elemental composition, particle count, particle size and modification of TiO2. The spICP-MS analysis confirmed the presence of the TiO2-derived (nano)particles (NPs) with a 39- to 187-nm median size and particle count up to 2.3 × 1011 particles per gram of tissue. On top of that, the SEM-EDS confirmed the presence of the TiO2 nanoparticles with 230-nm median size and an anatase crystal phase was determined by Raman spectroscopy. This study presents a novel multimodal approach for TiO2 particle determination and characterization in tissue samples and is the first in vivo study of this character.

2.
Food Chem ; 447: 139010, 2024 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-38513487

RESUMO

Assessment of trace metal concentrations in plant oils has been considered a crucial quality control marker for potential health risks, oil flavour, and oxidative stability. A straightforward inductively coupled plasma mass spectrometry (ICP-MS) methodology was developed and validated through introduction of argon:oxygen gas mixture into plasma, allowing for a direct elemental analysis of organic matrices. This approach offers the advantage of a simple one-step preparation of plant oil samples with negligible contamination risks. The complete solubilization of the oil matrix enables the determination of total metal content from a single test tube with low dilution factor of 5. The modified plasma conditions resulted in the development of a robust and accurate ICP-MS method providing limits of detection at sub ng·g-1 levels. The ICP-MS method allowed the determination of trace levels of Ba, Cd, Cu, Fe, Mn, Pb, Sn, V, and Zn in olive, sunflower and rapeseed oils.


Assuntos
Oxigênio , Oligoelementos , Oxigênio/análise , Oligoelementos/análise , Metais , Óleos de Plantas/química , Espectrometria de Massas/métodos
3.
Talanta ; 222: 121512, 2021 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-33167223

RESUMO

In this work we discuss how sample surface topography can significantly influence the laser ablation (LA) process and, in turn, the analytical response of the LA Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) method. Six different surface topographies were prepared on a certified aluminium alloy sample BAM 311 and SRM NIST 610 to investigate the phenomenon. All the samples were repetitively measured by LA-ICP-MS using a spot by spot analysis. The effect of laser fluence in the range of 1-13 J/cm2 was studied. For majority of measured isotopes, the ICP-MS signal was amplified with roughening of the sample surface. A stronger effect was observed on the Al alloy sample, where the more than sixty-time enhancement was achieved in comparison to the polished surface of the sample. Since the effect of surface topography is different for each analyte, it can be stated that surface properties affect not only the ICP-MS response, but also elemental fractionation in LA. The presented results show that different surface topographies may lead to misleading data interpretation because even when applying ablation preshots, the signal of individual elements changes. The utmost care must be taken when preparing the surface for single shot analysis or chemical mapping. On the other hand, by roughening the sample surface, it is possible to significantly increase the sensitivity of the method for individual analytes and supress a matrix effect.

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