title: Determination of chlorophenols in human urine based on the integration of on-line automated clean-up and preconcentration unit with micellar electrokinetic chromatography.
abstract: A new method was developed and validated for the determination of chlorophenols in human urine by using micellar electrokinetic chromatography (MEKC) coupled via a mechanic arm to an on-line automatic clean-up and preconcentration unit for urine samples. Separation is accomplished by using a selective buffer consisting of 15 mM borate, 25 mM phosphate and 100 mM sodium dodecyl sulfate (SDS) at pH 9.1 in addition to a positive power supply of 25 kV at 18 degrees C. The proposed capillary electrophoresis (CE) method allows the separation of 11 chlorophenols within 7 min with a reproducibility as relative standard deviation (RSD) between 2.6% and 7.2%, and limits of detection (LODs) between 0.08 and 0.46 microg/mL for all chlorophenols. Urine samples were previously hydrolyzed with 37% HCl at 80 degrees C for 60 min and then cleaned on a C-18 mini-column. Recoveries ranged from 58% to 103%. The preconcentration treatment affords limits of determination between 4 and 12 ng/mL for all chlorophenols except pentachlorophenol and 4-chlorophenol, which could not be determined. The overall analysis time, including on-line clean-up, preconcentration and electrophoretic separation is 20 min per sample.
authors.affiliation: Analytical Chemistry Division, Faculty of Sciences, University of Cordoba, Spain.
authors.forename: C
authors.initials: C
authors.lastname: Mardones
authors.forename: A
authors.initials: A
authors.lastname: Ríos
authors.forename: M
authors.initials: M
authors.lastname: Valcárcel
mesh_terms: D002733:Chlorophenols / Q000737:chemistry / Q000652:urine*; D020374:Chromatography, Micellar Electrokinetic Capillary / Q000379:methods*; D006801:Humans
chemical_list: D002733:Chlorophenols