Development of a novel methodology for determination of dialkyl phosphates in human urine using liquid chromatography-tandem mass spectrometry
Por:
Fernández SF, Pastor A, Yusà V, Montesinos L and Pardo O
Publicada:
1 nov 2019
Ahead of Print:
4 oct 2019
Resumen:
In this study a fast and sensitive method was developed for the quantitative determination of six dialkyl phosphates (DAPs) in human urine using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The proposed methodology was based on liquid-liquid extraction (LLE) with diethyl ether and ethyl acetate using MgSO4 and NaCl, followed by liquid chromatography and mass spectrometry detection in the selected reaction mode (SRM) with negative electrospray ionization (ESI-). Detection settings were optimized by design of experiments (DoE). Dibutyl phosphate (DBP) was used as internal standard. Several criteria established in the SANTE/11813/2017 guidance document for pesticide residues and analysis in food and feed were used to validate the suggested method: recoveries (R %) between 70 and 120% and coefficients of variation (CV %) <= 20%. The procedural limit of quantification (LoQ) was 0.50 ng mL(-1) for the six DAPs. The R% and CV% ranges were 82-117% and 3-20%, respectively. In total, 20 spot urine samples from lactating mothers were satisfactorily analyzed by the proposed analytical strategy.
Filiaciones:
:
Foundation for the Promotion of Health and Biomedical Research in the Valencian Region, FISABIO-Public Health, Av. Catalunya, 21, 46020 Valencia, Spain
Public Health Laboratory of Valencia, 21, Avenida Cataluña, 46020 Valencia, Spain
Pastor A:
Department of Analytical Chemistry, University of Valencia, Doctor Moliner 50, 46100 Burjassot, Spain
:
Foundation for the Promotion of Health and Biomedical Research in the Valencian Region, FISABIO-Public Health, Av. Catalunya, 21, 46020 Valencia, Spain
Public Health Laboratory of Valencia, 21, Avenida Cataluña, 46020 Valencia, Spain
Department of Analytical Chemistry, University of Valencia, Doctor Moliner 50, 46100 Burjassot, Spain
:
Public Health Laboratory of Valencia, 21, Avenida Cataluña, 46020 Valencia, Spain
:
Foundation for the Promotion of Health and Biomedical Research in the Valencian Region, FISABIO-Public Health, Av. Catalunya, 21, 46020 Valencia, Spain
Public Health Laboratory of Valencia, 21, Avenida Cataluña, 46020 Valencia, Spain
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