UHPLC-MS/MS method for the determination of bisphenol A and its chlorinated derivatives, bisphenol S, parabens, and benzophenones in human urine samples.
In the present work, a new method based on a sample treatment by dispersive liquid-liquid microextraction (DLLME) for the extraction of six bisphenols (bisphenol A, bisphenol S, and monochloro-, dichloro-, trichloro-, and tetrachlorobisphenol A), four parabens (methyl-, ethyl-, propyl-, and butylparaben), and six benzophenones (benzophenone-1, benzophenone-2, benzophenone-3, benzophenone-6, benzophenone-8, and 4-hydroxybenzophenone) in human urine samples, followed by ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis, is validated. An enzymatic treatment allows determining the total content of the target EDCs. The extraction parameters were accurately optimized using multivariate optimization strategies. Ethylparaben ring-(13)C6, benzophenone-d10, and bisphenol A-d16 were used as surrogates. Limits of quantification ranging from 0.1 to 0.6 ng mL(-1) and interday variabilities (evaluated as relative standard deviations) from 2.0 to 13.8% were obtained. The method was validated using matrix-matched standard calibration followed by a recovery assay with spiked samples. Recovery rates ranged from 94 to 106%. A good linearity, for concentrations up to 300 ng mL(-1) for parabens and 40 ng mL(-1) for benzophenones and bisphenols, was also obtained. The method was satisfactorily applied for the determination of target compounds in human urine samples from 20 randomly selected individuals.
Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, 18071, Granada, Spain.
F
F
Vela-Soria
O
O
Ballesteros
A
A
Zafra-Gómez
L
L
Ballesteros
A
A
Navalón
D001559:Benzhydryl Compounds / Q000737:chemistry*; D001577:Benzophenones / Q000737:chemistry; D002713:Chlorine / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid; D005260:Female; D006801:Humans; D006863:Hydrogen-Ion Concentration; D059627:Liquid Phase Microextraction; D008297:Male; D010226:Parabens / Q000032:analysis* / Q000737:chemistry; D010636:Phenols / Q000737:chemistry*; D015203:Reproducibility of Results; D012492:Salts; D012997:Solvents; D053719:Tandem Mass Spectrometry; D016482:Urinalysis / Q000379:methods*; D000098826:Bisphenol A Compounds
D001559:Benzhydryl Compounds; D001577:Benzophenones; D002713:Chlorine; D010226:Parabens; D010636:Phenols; D012492:Salts; D012997:Solvents; C012313:ethyl-p-hydroxybenzoate; C047723:benzophenone; C006780:bisphenol A; D000098826:Bisphenol A Compounds