title: A new procedure of determination of alcohol sulfates and alcohol ethoxysulfates in agricultural soils.
abstract: The number of analytical methodologies that focus in the determination of alcohol sulfates (AS) and alcohol ethoxysulfates (AES) in terrestrial environment is very limited. In the present work, a new methodology to improve the extraction and determination of AS and AES in agricultural soil samples has been developed. Prior to instrumental analysis, an extraction procedure using pressurized liquid extraction with methanol (PLE) was carried out in order to obtain the highest recoveries and improve sensitivity. The most influential variables affecting the PLE procedure were optimized. Then, the separation and quantification of analytes were performed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The limits of detection (LOD) ranged from 0.03 to 0.08μgg(-1) for AS homologues and in the case of AES ethoxymers from 0.03 to 0.09μgg(-1) for AES-C12Ex and from 0.03 to 0.08μgg(-1) for AES-C14Ex. Matrix-matched calibration was used. Trueness was evaluated by using a spike recovery assay with spiked blank samples, and the recoveries ranged from 98.3% to 101.0% for AS and from 99.9% to 100.1% for AES. The method was satisfactorily applied in a field study designed to evaluate the environmental behavior of these compounds in agricultural soil.
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Granada, Spain.
authors.forename: C
authors.initials: C
authors.lastname: Fernández-Ramos
authors.forename: O
authors.initials: O
authors.lastname: Ballesteros
authors.forename: A
authors.initials: A
authors.lastname: Zafra-Gómez
authors.forename: R
authors.initials: R
authors.lastname: Blanc
authors.forename: A
authors.initials: A
authors.lastname: Navalón
authors.forename: G
authors.initials: G
authors.lastname: Crovetto
authors.forename: S
authors.initials: S
authors.lastname: Cantarero
authors.forename: B
authors.initials: B
authors.lastname: Oliver-Rodríguez
authors.forename: J L
authors.initials: JL
authors.lastname: Vílchez
mesh_terms: D000383:Agriculture; D005591:Chemical Fractionation / Q000379:methods*; D002853:Chromatography, Liquid; D004785:Environmental Pollutants / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification*; D011312:Pressure; D015203:Reproducibility of Results; D012987:Soil / Q000737:chemistry*; D013431:Sulfates / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification*; D053719:Tandem Mass Spectrometry
chemical_list: D004785:Environmental Pollutants; D012987:Soil; D013431:Sulfates
keywords: Agricultural soil; Alcohol ethoxysulfates; Alcohol sulfates; Liquid chromatography–mass spectrometry; Pressurized liquid extraction