title: Determination of selected pharmaceutical compounds in biosolids by supported liquid extraction and gas chromatography-tandem mass spectrometry.
abstract: In this work, an analytical method was developed for the determination of pharmaceutical drugs in biosolids. Samples were extracted with an acidic mixture of water and acetone (1:2, v/v) and supported liquid extraction was used for the clean-up of extracts, eluting with ethyl acetate:methanol (90:10, v/v). The compounds were determined by gas chromatography-tandem mass spectrometry using matrix-match calibration after silylation to form their t-butyldimethylsilyl derivatives. This method presents various advantages, such as a fairly simple operation for the analysis of complex matrices, the use of inexpensive glassware and low solvent volumes. Satisfactory mean recoveries were obtained with the developed method ranging from 70 to 120% with relative standard deviations (RSDs) ≤ 13%, and limits of detection between 0.5 and 3.6 ng g(-1). The method was then successfully applied to biosolids samples collected in Madrid and Catalonia (Spain). Eleven of the sixteen target compounds were detected in the studied samples, at levels up to 1.1 μg g(-1) (salicylic acid). Ibuprofen, caffeine, paracetamol and fenofibrate were detected in all of the samples analyzed.
authors.affiliation: Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Ctra. de La Coruña Km 7.5, 28040 Madrid, Spain.
authors.forename: Beatriz
authors.initials: B
authors.lastname: Albero
authors.affiliation: Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Ctra. de La Coruña Km 7.5, 28040 Madrid, Spain.
authors.forename: Consuelo
authors.initials: C
authors.lastname: Sánchez-Brunete
authors.affiliation: Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Ctra. de La Coruña Km 7.5, 28040 Madrid, Spain.
authors.forename: Esther
authors.initials: E
authors.lastname: Miguel
authors.affiliation: Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Ctra. de La Coruña Km 7.5, 28040 Madrid, Spain.
authors.forename: Ramón
authors.initials: R
authors.lastname: Aznar
authors.affiliation: Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Ctra. de La Coruña Km 7.5, 28040 Madrid, Spain. Electronic address: tadeo@inia.es.
authors.forename: José L
authors.initials: JL
authors.lastname: Tadeo
mesh_terms: D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis / Q000302:isolation & purification; D005591:Chemical Fractionation; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000302:isolation & purification; D012722:Sewage / Q000737:chemistry; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000894:Anti-Inflammatory Agents, Non-Steroidal; D004364:Pharmaceutical Preparations; D012722:Sewage
keywords: Biosolids; Gas chromatography–tandem mass spectrometry; Pharmaceuticals; Sludge; Supported liquid extraction