2026-09-18T10:43:44Zhttps://gredos.usal.es/oai/request

oai:gredos.usal.es:10366/1621692025-04-30T19:49:30Zcom_10366_4182com_10366_4055com_10366_3946com_10366_3823col_10366_4183

González Mariño, Iria Casas Ferreira, Ana María Nogal Sánchez, Miguel del Pérez Pavón, José Luis 2025-01-21T11:47:33Z 2025-01-21T11:47:33Z 2023 Iria González-Mariño, Ana María Casas-Ferreira, Miguel del Nogal Sánchez, José Luis Pérez Pavón, Use of a guard column coupled to mass spectrometry as a fast semi-quantitative methodology for the determination of plasticizer metabolites in urine, Journal of Chromatography A, Volume 1690, 2023, 463788, ISSN 0021-9673, https://doi.org/10.1016/j.chroma.2023.463788. (https://www.sciencedirect.com/science/article/pii/S002196732300016X) 0021-9673 http://hdl.handle.net/10366/162169 10.1016/j.chroma.2023.463788 [EN]or the first time, a very simple and fast method combining the use of a guard column coupled to tandem mass spectrometry (guard column-MS/MS) has been proposed for the determination of plasticizer metabolites in urine. Briefly, samples (1.0 mL) were submitted to enzymatic hydrolysis for 10 min, filtered, diluted 1/10 v/v with ultrapure water and directly injected into the system. A fast run of only 2 min (3 min including the injection cycle) allowed the determination of 19 analytes. Enzymatic hydrolysis, filtering material, and guard column-MS/MS conditions were optimized. Intra-day precision at the low-level concentration (expressed as relative standard deviation, %RSD) obtained from the analysis of synthetic urine samples varied between 11 and 20%. Limits of quantification ranged from 2.8 to 60 ng/mL. Trueness values, calculated as apparent recoveries, ranged from 70 to 135%. To correct for matrix effects, analyte concentrations in real urine were quantified by the standard addition method. To confirm the results obtained by guard column-MS/MS, an ultra(high)-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was also applied (total chromatographic run time 17 min, including column re-equilibration). Concentrations measured with both methods were in good agreement. Hence, we propose the use of guard column-MS/MS to analyse a large number samples in a very short time (semi-quantification), and apply the chromatographic analysis only to those samples with levels close to/higher than the concentrations equivalent to the safe maximum daily intakes of the parent compounds (confirmation). This double strategy (semi-quantification by guard column-MS/MS and confirmation-when needed-by UHPLC-MS/MS) implies important savings in time and money. eng http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess Attribution-NonCommercial-NoDerivatives 4.0 Internacional Phthalate metabolites Urine Guard column Tandem mass spectrometry Ultra(high)-performance liquid chromatography Use of a guard column coupled to mass spectrometry as a fast semi-quantitative methodology for the determination of plasticizer metabolites in urine info:eu-repo/semantics/article