title: Sensitive determination of parabens in human urine and serum using methacrylate monoliths and reversed-phase capillary liquid chromatography-mass spectrometry.
abstract: A method for the determination of parabens in human urine and serum by capillary liquid chromatography (cLC) with UV-Vis and mass spectrometry (MS) detection using methacrylate ester-based monolithic columns has been developed. The influence of composition of polymerization mixture was studied. The optimum monolith was obtained with butyl methacrylate monomer at 60/40% (wt/wt) butyl methacrylate/ethylene dimethacrylate ratio and 50wt% porogens (composed of 36wt% of 1,4-butanediol, 54wt% 1-propanol and 10wt% water). Baseline resolution of analytes was achieved through a mobile phase of acetonitrile/water in gradient elution mode. Additionally, dispersive liquid-liquid microextraction (DLLME) was combined with both cLC-UV-Vis and cLC-MS to achieve the determination of parabens in human urine and serum samples with very low limits of detection. Satisfactory intra- and inter-day repeatabilities were obtained in UV-Vis and MS detection, although the latter provided lower detection limits (up to 300-fold) than the UV-Vis detection. Recoveries for the target analytes from spiked biological samples ranged from 95.2% to 106.7%. The proposed methodology for the ultra-low determination of parabens in human urine and serum samples is simple and fast, the consumption of reagents is very low, and very small samples can be analyzed.
authors.affiliation: Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100 Burjassot, Valencia, Spain.
authors.forename: Enrique Javier
authors.initials: EJ
authors.lastname: Carrasco-Correa
authors.affiliation: Department of Analytical Chemistry, University of Granada, 18071 Granada, Spain.
authors.forename: Fernando
authors.initials: F
authors.lastname: Vela-Soria
authors.affiliation: Department of Analytical Chemistry, University of Granada, 18071 Granada, Spain.
authors.forename: Oscar
authors.initials: O
authors.lastname: Ballesteros
authors.affiliation: Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100 Burjassot, Valencia, Spain.
authors.forename: Guillermo
authors.initials: G
authors.lastname: Ramis-Ramos
authors.affiliation: Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100 Burjassot, Valencia, Spain. Electronic address: jmherrer@uv.es.
authors.forename: José Manuel
authors.initials: JM
authors.lastname: Herrero-Martínez
mesh_terms: D001774:Blood Chemical Analysis / Q000379:methods*; D056148:Chromatography, Reverse-Phase; D006801:Humans; D057230:Limit of Detection; D013058:Mass Spectrometry; D008689:Methacrylates / Q000737:chemistry*; D010226:Parabens / Q000032:analysis*; D016482:Urinalysis / Q000379:methods*
chemical_list: D008689:Methacrylates; D010226:Parabens
keywords: Capillary-LC–MS; DLLME; Human serum; Human urine; Methacrylate monolithic columns; Parabens