Cleanup strategies and advantages in the determination of several therapeutic classes of pharmaceuticals in wastewater samples by SPE-LC-MS/MS

• Published in: Analytical and bioanalytical chemistry 2011-01, Vol.399 (2), p.807-822
• Main Authors: Sousa, M. A, Gonçalves, C, Cunha, E, Hajšlová, J, Alpendurada, M. F
• Format: Article
• Language: English
• Subjects: Adsorbents; Analysis; Analysis methods; Analytical Chemistry; Applied sciences; Biochemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatographic methods and physical methods associated with chromatography; Chromatography, Liquid - methods; Cleanup; Contamination; Drugs; Environmental Monitoring - methods; Exact sciences and technology; Extraction (Chemistry); Food Science; Global environmental pollution; Ion exchange chromatography; Ionization; Laboratory Medicine; Liquid chromatography; Liquid chromatography-tandem mass spectrometry (LC-MS/MS); Mass spectrometry; MAX cartridges; Methods; Monitoring/Environmental Analysis; Natural water pollution; Original Paper; Other chromatographic methods; Pharmaceutical Preparations - analysis; Pharmaceutical Preparations - isolation & purification; Pollution; Portugal; Purification; Rivers - chemistry; Sewage; Solid Phase Extraction - methods; Spectrometric and optical methods; Spectrometry, Mass, Electrospray Ionization - methods; surface water; Tandem Mass Spectrometry - methods; Waste Disposal, Fluid - methods; Waste management; Wastewater; Water - analysis; Water Pollutants, Chemical - analysis; Water Pollutants, Chemical - isolation & purification; Water treatment and pollution
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-010-4297-0

This work describes the development and validation of an offline solid-phase extraction with simultaneous cleanup capability, followed by liquid chromatography-(electrospray ionisation)-ion trap mass spectrometry, enabling the concurrent determination of 23 pharmaceuticals of diverse chemical nature, among the most consumed in Portugal, in wastewater samples. Several cleanup strategies, exploiting the physical and chemical properties of the analytes vs. interferences, alongside with the use of internal standards, were assayed in order to minimise the influence of matrix components in the ionisation efficiency of target analytes. After testing all combinations of adsorbents (normal-phase, ion exchange and mixed composition) and elution solvents, the best results were achieved with the mixed-anion exchange Oasis MAX cartridges. They provided recovery rates generally higher than 60%. The precision of the method ranged from 2% to 18% and 4% to 19% (except for diclofenac (22%) and simvastatin (26%)) for intra- and inter-day analysis, respectively. Method detection limits varied between 1 and 20 ng L⁻¹, while method quantification limits were