Abstract
In this study, an intra-laboratory assessment was carried out to establish the effectiveness of a method for the detection of TiO2 engineered nanoparticles (ENPs) present in sunscreen containing nano-scale TiO2 and a higher nanometer-range (approx. 200–500 nm) TiO2, as well as iron oxide particles. Three replicate measurements were performed on five separate days to generate the measurement uncertainties associated with the quantitative asymmetrical flow field-flow fractionation (AF4) measurement of the hydrodynamic radius rh,mode1 (MALS), rh,mode1 (ICP-MS), rh,mode2 (ICP-MS), and calculated mass-based particle size distribution (d10, d50, d90). The validation study demonstrates that the analysis of TiO2 ENPs present in sunscreen by AF4 separation-multi detection produces quantitative data (mass-based particle size distribution) after applying the sample preparation method developed within the NanoDefine project with uncertainties based on the precision (uIP) of 3.9–8.8%. This method can, therefore, be considered as the method with a good precision. Finally, the bias data shows that the trueness of the method (ut = 5.5–52%) can only be taken as a proxy due to the lack of a sunscreen standard containing certified TiO2 ENPs.
Highlights
The current EU Cosmetic Products Regulation (EU Regulation (EC) No 1223/2009) requires the labeling of products containing engineered nanoparticles (ENPs) (EC, 2009)
This paper presents the results of an intra-laboratory assessment which examines the AF4-multi angle light scattering (MALS)-inductively coupled plasma–mass spectrometry (ICP-MS) method for the characterization of TiO2 ENPs
For the first time an intra-laboratory assessment of a sample preparation method followed by AF4-MALS-ICP-MS analysis for the detection and quantification of TiO2 ENPs present in sunscreen has been carried out
Summary
The current EU Cosmetic Products Regulation (EU Regulation (EC) No 1223/2009) requires the labeling of products containing engineered nanoparticles (ENPs) (EC, 2009). To our knowledge, most of the studies rely on time-consuming stepwise sample preparation procedures (Kammer et al, 2012) requiring the extraction of TiO2 ENPs from sunscreen and further characterization in terms of particle size distribution by separation techniques such as field-flow fractionation (FFF) (Contado and Pagnoni, 2008; Nischwitz and GoenagaInfante, 2012; López-Heras et al, 2014; Müller et al, 2016; Philippe et al, 2018; Bocca et al, 2018; de la Calle et al, 2018). No thorough standardization and validation of the methods with respect to both sample preparation and multi-detector asymmetrical flow field-flow fractionation has been reported up to date (Babick et al, 2016; Gao and Lowry, 2018)
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