title: Simultaneous determination of estrogenic short ethoxy chain nonylphenols and their acidic metabolites in water by an in-sample derivatization/solid-phase microextraction method.
abstract: An in-sample derivatization headspace solid-phase microextraction method has been developed for the simultaneous determination of nonylphenol, nonylphenol mono- and diethoxylates (NP, NP1EO, NP2EO), and their acidic metabolites (NPlEC, NP2EC) in water. The analytical procedure involves derivatization of NPEOs and NPECs to their methyl ethers--esters with dimethyl sulfate/NaOH and further headspace (HS) solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS) determination. Parameters affecting both derivatization efficiency and headspace SPME procedure, such as the selection of the SPME coating, derivatizationextraction time, temperature and ionic strength were optimized. The commercially available Carbowax-divinylbenzene (CW-DVB) fiber appears to be the most suitable for the simultaneous determination of both NPEOs-NPECs. Run-to-run precision of the in-sample derivatization/HS-SPME-GC/MS method gave relative standard deviations between 8 and 18%. The method was linear for NP over 2 orders of magnitude, and detection limits were compound dependent but ranged from 20 to 1500 ng/L. The SPME procedure was compared with a solid-phase extraction SPE-GC/MS method for the analysis of NPEOs-NPECs in water samples and good agreement was obtained. Therefore, in-sample derivatization HS-SPME-GC/MS can be used as a method for the simultaneous determination of short ethoxy chain nonylphenols and their acidic metabolites in water.
authors.affiliation: AGBAR, Aigües de Barcelona, Spain.
authors.forename: Alfredo
authors.initials: A
authors.lastname: Díaz
authors.forename: Francesc
authors.initials: F
authors.lastname: Ventura
authors.forename: Maria Teresa
authors.initials: MT
authors.lastname: Galceran
mesh_terms: D002264:Carboxylic Acids; D008401:Gas Chromatography-Mass Spectrometry / Q000592:standards; D007220:Industrial Waste / Q000032:analysis; D010636:Phenols / Q000032:analysis*; D012680:Sensitivity and Specificity; D013501:Surface-Active Agents / Q000032:analysis*; D014873:Water Pollutants / Q000032:analysis* / Q000592:standards
chemical_list: D002264:Carboxylic Acids; D007220:Industrial Waste; D010636:Phenols; D013501:Surface-Active Agents; D014873:Water Pollutants; C025256:nonylphenol