2026-05-31T17:09:42Zhttps://riuma.uma.es/rest/oai/request

oai:riuma.uma.es:10630/273152026-02-03T11:21:32Zcom_10630_2254col_10630_37953

00925njm 22002777a 4500 dc Montoro-Leal, Pablo author García-Mesa, Juan Carlos author Morales-Benítez, Irene author Vázquez‑Palomo, Laura author López-Guerrero, María del Mar author Vereda-Alonso, Elisa Isabel author 2023 A new magnetic functionalized material based on graphene oxide magnetic nanoparticles named by us, M@GO-TS, was designed and characterized in order to develop a magnetic solid-phase extraction method (MSPE) to enrich inorganic and organic species of lead, mercury, and vanadium. A flow injection (FI) system was used to preconcentrate the metallic and organometallic species simultaneously, while the ultra-trace separation and determination of the selected species were achieved by high-performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC-ICP MS). Therefore, preconcentration and separation/determination processes were automated and conducted separately. To the best of our knowledge, this is the first method combining an online MSPE and HPLC-ICP MS for multielemental speciation. Under the optimized conditions, the enrichment factor obtained for PbII, trimethyllead (TML), HgII, methylmercury (MetHg), and VV was 27. The calculated LOD for all studied species were as follows: 5 ng L−1, 20 ng L−1, 2 ng L−1, 10 ng L−1, and 0.4 ng L−1, respectively. The RSD values calculated with a solution containing 0.5 μg L−1 of all species were between 2.5 and 4.5%. The developed method was validated by analyzing Certified Reference Materials TMDA 64.3 for total concentration and also by recovery analysis of the species in human urine from volunteers and a seawater sample collected in Málaga. The t statistical test showed no significant differences between the certified and found values for TMDA 64.3. All the recoveries obtained from spiked human urine and seawater samples were close to 100%. All samples were analyzed using external calibration. The developed method is sensitive and promising for routine monitoring of the selected species in environmental waters and biological samples. Montoro-Leal, P., García-Mesa, J.C., Morales-Benítez, I. et al. Synthesis of a novel magnetic nanomaterial for the development of a multielemental speciation method of lead, mercury, and vanadium via HPLC-ICP MS. Microchim Acta 190, 296 (2023). https://doi.org/10.1007/s00604-023-05877-x https://hdl.handle.net/10630/27315 10.1007/s00604-023-05877-x Materiales nanoestructurados - Propiedades magnéticas Minerales - Preparación Synthesis of a novel magnetic nanomaterial for the development of a multielemental speciation method of lead, mercury, and vanadium via HPLC‑ICP MS