title: Determination of alkylphenols in water samples using liquid chromatography-tandem mass spectrometry after pre-column derivatization with dansyl chloride.
abstract: The present study describes an effect of reaction condition of pre-column derivatization of alkylphenols (APs): bisphenol A (BPA), 4-tert-octylphenol (4-t-OP), 4-octylphenol (4-OP), 4-n-nonylphenol (4-n-NP), and isomers of 4-nonylphenol (iso-NP) with 5-(dimethylamino) naphthalene-1-sulfonyl chloride (dansyl chloride, DNSC) on their LC-ESI-MS/MS determination in water samples. Chemical derivatization improves the sensitivity and selectivity of LC-MS/MS analysis. In principle, alkylphenols can be analyzed by LC-MS/MS without derivatization. However, pre-column derivatization of APs increases the sensitivity up to 1000 times in comparison with the analysis of underivatized alkylphenols. Reaction conditions affecting formation of the DNSC-derivatives, such as various solvent, reaction temperature, reaction time, DNSC concentration and pH values were tested. The most suitable conditions, in terms of achieving a high sensitivity, resulting from this study are: acetonitrile as reaction solvent, 60 min as reaction time, 60 °C as reaction temperature, pH values 10.5, 0.5 mg mL(-1) as DNSC concentration. Calibration curves are linear at least in the range of 1-1000 ng mL(-1), limits of detection (LOD) and limits of quantification (LOQ) ranging from 0.02 to 0.25 pg/injection and from 0.08 to 0.83 pg/injection, respectively. The improved procedure was successfully applied for the analysis of APs and BPA in real water samples. The median concentration of BPA and iso-NP obtained in bottled waters was 4.7 ng L(-1) and 33.5 ng L(-1), respectively. The median concentration of 4-t-OP was 1.3 ng L(-1.)
authors.affiliation: Masaryk University, Faculty of Science, Research Centre for Toxic Compounds in the Environment RECETOX, Kamenice 753/5, 625 00 Brno, Czech Republic.
authors.forename: Marek
authors.initials: M
authors.lastname: Pernica
authors.affiliation: Masaryk University, Faculty of Science, Research Centre for Toxic Compounds in the Environment RECETOX, Kamenice 753/5, 625 00 Brno, Czech Republic.
authors.forename: Petra
authors.initials: P
authors.lastname: Poloucká
authors.affiliation: Masaryk University, Faculty of Science, Research Centre for Toxic Compounds in the Environment RECETOX, Kamenice 753/5, 625 00 Brno, Czech Republic.
authors.forename: Marta
authors.initials: M
authors.lastname: Seifertová
authors.affiliation: Masaryk University, Faculty of Science, Research Centre for Toxic Compounds in the Environment RECETOX, Kamenice 753/5, 625 00 Brno, Czech Republic. Electronic address: simek@recetox.muni.cz.
authors.forename: Zdeněk
authors.initials: Z
authors.lastname: Šimek
mesh_terms: D001559:Benzhydryl Compounds / Q000032:analysis; D002853:Chromatography, Liquid / Q000379:methods; D003619:Dansyl Compounds / Q000737:chemistry*; D060766:Drinking Water / Q000032:analysis; D007202:Indicators and Reagents; D057230:Limit of Detection; D010636:Phenols / Q000032:analysis; D053719:Tandem Mass Spectrometry / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis*; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D003619:Dansyl Compounds; D060766:Drinking Water; D007202:Indicators and Reagents; D010636:Phenols; D014874:Water Pollutants, Chemical; C025256:nonylphenol; C080417:4-octylphenol; C041594:4-nonylphenol; C105260:4-tert-octylphenol; C006780:bisphenol A; D000098826:Bisphenol A Compounds; C029038:dansyl chloride
keywords: Alkylphenols; Chemical derivatization of alkylphenols; Electrospray ionization; Liquid chromatography; Tandem mass spectrometry