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The increasing use of titanium dioxide nanoparticles in daily use consumer products such as cosmetics, personal care products, food additives, and even medicine has led to growing concerns regarding human safety. It would be ideal to track exposure to this emerging nanopollutant, for example through bioassays, however, so far nanoparticle assessment in biological matrices such as urine remains challenging. The lack of data is mainly due to the limitations of the current metrology, but also to the low expected concentration in human samples. In this study, a quantification method for titanium dioxide nanoparticles in urine has been developed and validated following the ISO/CEI 17025:2017 guidelines. The detection limit for titanium dioxide nanoparticle mass concentration by single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS) was 0.05 ng mL−1. The particle size limit was determined using three different approaches, with the highest calculated limit value approaching 50 nm. Repeatability and reproducibility of 14% and 18% respectively were achieved for particle mass concentration, and 6% for both parameters for particle size determination. Method trueness and recovery were 98% and 84%, respectively. [ABSTRACT FROM AUTHOR]

Due to their omnipresence in consumer products, there is a growing concern about the potential effects of nanoparticles on human health. Toxicological assessment and NP end-product studies require proper quantification of these materials in biological fluids. However, their quantifications in these media require stable predispersed NP solutions in aqueous media to enable the fortification in the matrices of interest or the preparation of calibration standards. In this study, a sample preparation scheme was developed by studying various dispersion media (polyvinylpyrrolidone and polyethylene glycol) and sonication strategies (bath and ultrasonic probe) to ensure homogeneous dispersion of titanium dioxide nanoparticles. Optimization of the various parameters was performed using SRM NIST 1898 NP reference material, composed of rutile and anatase phases. Number-based size distribution for titanium dioxide NPs was determined by dynamic light scattering and single-particle inductively coupled plasma mass spectrometry to evaluate the procedure efficiency. Changes in mean size and most frequent size distribution were also studied to determine if the agglomeration of nanoparticles occurs at the various dispersion conditions tested. Among the different dispersion parameters tested herein, the use of polyvinylpyrrolidone combined with a sonication process generated by a probe leads to a significant improvement in terms of suspension efficiency and stability over 72 h. The dispersion efficiency of the proposed methodology was assessed by single-particle inductively coupled plasma mass spectrometry with spiked biological fluids such as urine and blood. [ABSTRACT FROM AUTHOR]

Biomonitoring for manganese (Mn) exposure is important due to its potential to cause adverse health effects. In this study, we investigate how different sample preparation methods (dilution, digestion), calibration protocols (aqueous, blood-based, standard additions), and instrumental techniques affect Mn method bias and analytical imprecision. The techniques used included graphite furnace atomic absorption spectrometry (GFAAS), dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS), and sector field (SF-) ICP-MS. We analyzed NIST SRM 1643e Trace Elements in Water and SRM 1598a Inorganic Constituents in Animal Serum (both certified for Mn), and SRM 955c Toxic Metals in Caprine Blood – Level 1 (not certified for Mn). Various matrix effects in ICP-MS produced inaccurate results for SRM 1643e and discrepant results for SRM 955c. In the absence of a certified value for Mn in SRM 955c, we assigned a “consensus” value by combining data from the New York State Department of Health (NYS), the Centers for Disease Control and Prevention (CDC) and the Centre de toxicologie du Québec (CTQ). With this interlaboratory approach, we established an “all-lab” consensus value of 16.3 ± 0.8 μg L−1 based on data from DRC-ICP-MS with dilution sample preparation and blood-based calibration. We also assigned an “all-method” consensus value of 16.3 ± 0.9 μg L−1 based on GFAAS and SF-ICP-MS data from the NYS lab and the DRC-ICP-MS all-lab consensus value. Although the expanded uncertainty (U) calculated for the consensus values may not fully account for all sources of uncertainty, it does show the relative variation that might be expected from one study to the next for the determination of Mn in blood. [ABSTRACT FROM AUTHOR]