title: Determination of artificial sweeteners in sewage sludge samples using pressurised liquid extraction and liquid chromatography-tandem mass spectrometry.
abstract: An analytical method for the determination of six artificial sweeteners in sewage sludge has been developed. The procedure is based on pressurised liquid extraction (PLE) with water followed by solid-phase extraction (SPE) and subsequent liquid chromatography-tandem mass spectrometry analysis. After optimisation of the different PLE parameters, extraction with aqueous 500mM formate buffer (pH 3.5) at 80°C during a single static cycle of 21min proved to be best conditions. After a subsequent SPE, quantification limits, referred to dry weight (dw) of sewage sludge, ranged from 0.3ng/g for acesulfame (ACE) to 16ng/g for saccharin (SAC) and neohespiridine dihydrochalcone. The trueness, expressed as recovery, ranged between 72% and 105% and the precision, expressed as relative standard deviation, was lower than 16%. Moreover, the method proved its linearity up to the 2μg/g range. Finally, the described method was applied to the determination of the artificial sweeteners in primary and secondary sewage sludge from urban wastewater treatment plants. Four of the six studied artificial sweeteners (ACE, cyclamate, SAC and sucralose) were found in the samples at concentrations ranging from 17 to 628ng/g dw.
authors.affiliation: Department of Analytical Chemistry, Nutrition and Food Sciences, IIAA - Institute for Food Analysis and Research, University of Santiago de Compostela, 15782 Santiago de Compostela, Spain.
authors.forename: Edgar Y
authors.initials: EY
authors.lastname: Ordoñez
authors.forename: José Benito
authors.initials: JB
authors.lastname: Quintana
authors.forename: Rosario
authors.initials: R
authors.lastname: Rodil
authors.forename: Rafael
authors.initials: R
authors.lastname: Cela
mesh_terms: D002021:Buffers; D002853:Chromatography, Liquid / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D011312:Pressure; D015203:Reproducibility of Results; D012722:Sewage / Q000737:chemistry*; D052616:Solid Phase Extraction; D013549:Sweetening Agents / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013696:Temperature
chemical_list: D002021:Buffers; D012722:Sewage; D013549:Sweetening Agents
keywords: Artificial sweeteners; Liquid chromatography–mass spectrometry; Pressurised liquid extraction; Sludge; Solid-phase extraction; Sucralose