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dc.contributor.authorBijlsma, Lubertus
dc.contributor.authorBeltrán Iturat, Eduardo
dc.contributor.authorBoix Sales, Clara
dc.contributor.authorSancho Llopis, Juan Vicente
dc.contributor.authorHernández Hernández, Félix
dc.identifier.citationBIJLSMA, L...[et al.]. Improvements in analytical methodology for the determination of frequently consumed illicit drugs in urban wastewater. Analytical and Bioanalytical Chemistry (July 2014), v. 406, Issue 17, pp. 4261-4272ca_CA
dc.description.abstractRapid and sensitive analytical methodology based on ultra high-performance liquid chromatography-tandem mass spectrometry has been developed for the determination of widely consumed drugs of abuse (amphetamines, MDMA, cocaine, opioids, cannabis and ketamine) and their major metabolites in urban wastewaters. Sample clean-up and pre-concentration was performed by a generic off-line SPE procedure using Oasis HLB. Special effort was made to incorporate amphetamine, which was found highly problematic in the wastewater samples tested, including an additional clean-up with Oasis MCX SPE and dispersive primary secondary amine. Correction for possible SPE losses or degradation during storage was made by the use of isotope-labelled internal standards (ILIS), available for all compounds, which were added to the samples as surrogates. Although ILIS were also efficient for matrix effects correction, the strong ionization suppression observed was not eliminated; therefore, a four-fold dilution prior to SPE was applied to influent wastewaters and a low injection volume was selected (3 μL), in order to reach a compromise between matrix effects, chromatographic performance and sensitivity. The method was validated at 25 and 200 ng L−1 (effluent), and 100 and 800 ng L−1 (influent), obtaining limits of quantification (i.e. the lowest level that the compound can be quantified and also confirmed with at least two MS/MS transitions) between 0.4–25 ng L−1 (effluent) and 2–100 ng L−1 (influent). The applicability of the method was demonstrated by analysis of 14 influent and 14 effluent wastewater samples collected over 2 weeks in Castellón (Spain) within a European collaborative study.ca_CA
dc.format.extent12 p.ca_CA
dc.relation.isPartOfAnalytical and Bioanalytical Chemistry (July 2014), v. 406, Issue 17ca_CA
dc.subjectDrugs of abuseca_CA
dc.subjectTriple quadrupoleca_CA
dc.subjectUltra high-performance liquidchromatographyca_CA
dc.subjectSample dilutionca_CA
dc.subjectUrban wastewaterca_CA
dc.titleImprovements in analytical methodology for the determination of frequently consumed illicit drugs in urban wastewaterca_CA

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