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...
| Autores: | , , , , , |
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| 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 |
| 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. |
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