title: Selective determination of acidic pharmaceuticals in wastewater using molecularly imprinted solid-phase extraction.
abstract: The determination of acidic pharmaceuticals, such as non-steroidal anti-inflammatory drugs NSAIDs and clofibric acid (metabolite of clofibrate), at low ngL(-1) levels in wastewater requires highly selective and sensitive analytical procedures. The removal of matrix components during sample preparation results in significant benefits towards reducing the matrix effects during LC-MS analysis. Therefore this work describes a simple method to enrich and clean up NSAIDs and clofibric acid from sewage water using molecularly imprinted solid-phase extraction (MISPE). Final analysis was performed by liquid chromatography-tandem mass spectrometry. The performance of this method has been evaluated in fortified tap and sewage water in terms of recovery, precision, linearity, and method quantification limit. Recovery for all compounds ranged in all matrices between 84 and 116% with intra-day R.S.D. values below 11.5%. Matrix effect evaluation demonstrated that even complex sample matrixes, such as pond or sewage water did not showed significant ion suppression/enhancement compared to tap water. The performance of the method was further emphasized by the study of pond water, which receives treated water from a sewage treatment plant in south Sweden. Raw sewage and treated water were also tested. In those samples, all acidic pharmaceuticals were detected in concentration above method quantification limits ranging from 5.1 to 5153.0ngL(-1).
authors.affiliation: Division of Analytical Chemistry, Lund University, P.O. Box 124, SE-22100, Lund, Sweden. saioa.zorita@analykem.lu.se
authors.forename: Saioa
authors.initials: S
authors.lastname: Zorita
authors.forename: Brian
authors.initials: B
authors.lastname: Boyd
authors.forename: Stig
authors.initials: S
authors.lastname: Jönsson
authors.forename: Ecevit
authors.initials: E
authors.lastname: Yilmaz
authors.forename: Carin
authors.initials: C
authors.lastname: Svensson
authors.forename: Lennart
authors.initials: L
authors.lastname: Mathiasson
authors.forename: Staffan
authors.initials: S
authors.lastname: Bergström
mesh_terms: D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis* / Q000302:isolation & purification; D002853:Chromatography, Liquid; D002995:Clofibric Acid / Q000032:analysis* / Q000302:isolation & purification; D011108:Polymers / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012722:Sewage / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D000894:Anti-Inflammatory Agents, Non-Steroidal; D011108:Polymers; D012722:Sewage; D014874:Water Pollutants, Chemical; D002995:Clofibric Acid