Urine and saliva biomonitoring by HF-LPME-LC/MS to assess dinitrophenols exposure

In this work, the determination of 2,4-, 2,5- and 2,6-dinitrophenols and the identification of some of their metabolites in human urine and saliva is proposed. A three phase hollow fiber based liquid phase microextraction prior to ultra-high performance liquid chromatography coupled to quadrupole ti...

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Detalles Bibliográficos
Autores: Kazakova, Julia, Villar Navarro, Mercedes, Pérez Bernal, Juan Luis, Ramos Payán, María Dolores, Bello López, Miguel Ángel, Fernández Torres, Rut
Tipo de recurso: artículo
Estado:Versión aceptada para publicación
Fecha de publicación:2021
País:España
Institución:Universidad de Sevilla (US)
Repositorio:idUS. Depósito de Investigación de la Universidad de Sevilla
OAI Identifier:oai:idus.us.es:11441/153302
Acceso en línea:https://hdl.handle.net/11441/153302
https://doi.org/10.1016/j.microc.2021.106193
Access Level:acceso abierto
Palabra clave:Hollow fiber liquid phase microextraction
HF-LPME
Liquid chromatography quadrupole time-of-flight
Dinitrophenols
Human urine
Human saliva
Descripción
Sumario:In this work, the determination of 2,4-, 2,5- and 2,6-dinitrophenols and the identification of some of their metabolites in human urine and saliva is proposed. A three phase hollow fiber based liquid phase microextraction prior to ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry allowed low detection and quantitation limits of the target analytes, as well as the investigation and tentatively identification of some metabolites by accurate mass full-spectrum measurements. The chromatographic separation was accomplished on an Acquity BEH C18 column (50 mm × 2.1 mm i.d., 1.7 μm particle size) at 25 ºC using water and acetonitrile (with 0.1 % (v/v) formic acid) 20:80 v/v as mobile phase, at a flow rate of 0.5 mL/min in isocratic elution mode for 5 min. Hollow fiber liquid phase microextraction was achieved at donor phase pH 2, acceptor phase pH 13 and dihexylether as supported liquid membrane. Under the optimal conditions, detection limits for 2,4-, 2,5- and 2,6-dinitrophenol, respectively, were 0.18 μg·L-1, 0.38 μg·L-1 and 0.14 μg·L-1 in urine samples and 0.32 μg·L-1, 0.67 μg·L-1 and 0.24 μg·L-1 in saliva samples. The proposed methodology was applied on urine and saliva samples from laboratory staff likely to be or not occupationally exposed to dinitrophenols, finding quantitative levels of 2,4- and 2,6-dinitrophenol and identifying some metabolites previously reported in literature.