Determination of alcohol sulfates and alcohol ethoxysulfates in wastewater samples by liquid chromatography tandem mass spectrometry

The work develops a liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for the identification and quantification of alkyl homologues of alcohol sulfates (AS) and ethoxymers of alcohol ethoxysulfates (AES) in wastewaters. The method involves isolation and preconcentration of the analytes from the samples using solid-phase extraction (SPE) with SAX cartridges prior to their quantification by LC–MS/MS with electrospray (ESI) interface in negative mode. The limits of detection (LOD) found were 0.1 Î¼g L− 1 for AS, and ranged from 0.2 to 0.5 Î¼g L− 1 for AES. The limits of quantification (LOQ) ranged from 0.3 to 0.4 Î¼g L− 1 for AS, and from 0.5 to 1.5 Î¼g L− 1 for AES. The accuracy of the method was studied in terms of trueness and precision. Trueness was evaluated by using a spike recovery assay with spiked blank samples. Recoveries ranged from 96.0 to 102.8% for AS and from 93.4 to 105.1% for AES. Precision (in terms of inter- and intra-day RSD) was lower than 5% for AS and AES. Finally, the method was satisfactorily applied to the quantification of compounds in wastewater samples collected from a wastewater treatment plant (WWTP) located in the city of Granada (Spain). Data obtained showed that AS are present in concentration levels from 0.7 to 39.4 Î¼g L− 1 in influent waters and from 1.1 to 8.1 Î¼g L− 1 in effluent waters. As for AES, the amounts (sum of ethoxymers) found ranged from 0.7 to 24.0 Î¼g L− 1 in influents and from 1.9 to 2.5 Î¼g L− 1 in effluents. ⺠Two methods to quantify alcohol sulfates and alcohol etoxysulfates in wastewaters. ⺠SPE allows for very low detection and quantification limits. ⺠Validation of the method: quality parameters, accuracy (trueness and precision). ⺠Application of the method to samples collected from influents and effluents wastewaters.