RT Journal Article T1 Enzymatic hydrolysis for pre-treating human serum before titanium dioxide nanoparticles assessment by spICP-MS A1 Justo Vega, Ana A1 Vázquez Pérez, Sara A1 Domínguez González, Raquel A1 Bermejo Barrera, Pilar A1 Moreda Piñeiro, Antonio K1 Titanium dioxide nanoparticles K1 Serum K1 Enzymatic hydrolysis K1 Ultra centrifugal filtration K1 spICP-MS AB The current use of inorganic nanoparticles (NPs) in many industrial sectors, particularly in the food industry, has led to growing concerns about the toxicity of these emerging materials to humans. Therefore, NPs assessment in foodstuff, environmental materials and biological fluids is becoming an important topic, and the development of reliable quantification/characterization analytical methods is needed. The presence of NPs in blood and urine can be expected because of the bioavailability/assimilation of these entities by the organism. However, the determination of NPs in biofluids is a challenge mainly due to the complexity of the sample and the low levels of NPs (basal levels). The research on new methodologies for sample treatment is therefore needed.The possibilities of enzymatic hydrolysis followed by centrifugal ultrafiltration for isolating titanium dioxide nanoparticles (TiO2 NPs) from serum samples have been explored in the current research. Hydrolysis of serum's matrix components was performed with a pancreatin-lipase mixture (0.1 %(w/v) each one) operating at pH 7.4 and 37 °C for 4.0 h under orbital - horizontal shaking at 150 rpm. In addition, centrifugal ultrafiltration (30 kDa molecular weight cutoff (MWCO) membrane) was optimised for removing enzymes residues and other matrix's components. The developed method showed a limit of detection of 6.89 × 103 NPs mL−1, and a limit of detection in size of 36 nm, whereas analytical recovery for spiking assays with 100 nm TiO2 NPs were within the 103–114 % range. PB Elsevier SN 0039-9140 YR 2025 FD 2025-08-15 LK https://hdl.handle.net/10347/43142 UL https://hdl.handle.net/10347/43142 LA eng NO Justo-Vega, A., Vázquez-Pérez, S., Domínguez-González, R., Bermejo-Barrera, P., & Moreda-Piñeiro, A. (2025). Enzymatic hydrolysis for pre-treating human serum before titanium dioxide nanoparticles assessment by spICP-MS. “Talanta”, 291, 127766. https://doi.org/10.1016/j.talanta.2025.127766 NO Grant FOODNANORISK (reference PID2021-125276NB-I00) funded by MICIU/AEI/ 10.13039/501100011033 Spain. and Grupo de Refer encia Competitiva (reference ED431C 2022/029) funded by Consellería de Educacion, ′ Ciencia, Universidades y Formacion ′ Profesional, Xunta de Galicia, Spain. A. J.-V. acknowledges Xunta de Galicia, Spain, for a pre doctoral grant. DS Minerva RD 24 abr 2026