Multiresidue methods for the analysis of pharmaceuticals, personal care products and illicit drugs in surface water and wastewater by solid-phase extraction and ultra performance liquid chromatography-electrospray tandem mass spectrometry

• Published in: Analytical and bioanalytical chemistry 2008-06, Vol.391 (4), p.1293-1308
• Main Authors: Kasprzyk-Hordern, Barbara, Dinsdale, Richard M, Guwy, Alan J
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Biochemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatography, Liquid - methods; drugs; Environmental Monitoring; Food Science; Illicit drugs; Ion suppression; Laboratory Medicine; Monitoring/Environmental Analysis; Multiresidue method; Original Paper; personal care products; Pharmaceutical Preparations - analysis; solid phase extraction; Solid Phase Extraction - methods; Spectrometry, Mass, Electrospray Ionization - methods; Tandem Mass Spectrometry - methods; Ultra performance liquid chromatography-tandem mass spectrometry; Water - analysis; Water Pollutants, Chemical - analysis
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-008-1854-x

The main aim of the presented research is to introduce a new technique, ultra performance liquid chromatography-positive/negative electrospray tandem mass spectrometry (UPLC-ESI/MS/MS), for the development of new simultaneous multiresidue methods (over 50 compounds). These methods were used for the determination of multiple classes of pharmaceuticals (acidic, basic and neutral compounds: analgesic/anti-inflammatory drugs, antibiotics, antiepileptics, beta-adrenoceptor blocking drugs, lipid regulating agents, etc.), personal care products (sunscreen agents, preservatives, disinfectant/antiseptics) and illicit drugs (amphetamine, cocaine and benzoylecgonine) in surface water and wastewater. The usage of the novel UPLC system with a 1.7 μm particle-packed column allowed for good resolution of analytes with the utilisation of low mobile phase flow rates (0.05-0.07 mL min⁻¹) and short retention times (method times of up to 25 min), delivering a fast and cost-effective method. SPE with the usage of Oasis MCX strong cation-exchange mixed-mode polymeric sorbent was chosen for sample clean-up and concentration. The influence of mobile phase composition, matrix-assisted ion suppression in ESI-MS and SPE recovery on the sensitivity of the method was extensively studied. The method limits of quantification were at low nanogram per litre levels and ranged from tenths of ng L⁻¹ to tens of ng L⁻¹ in surface water and from single ng L⁻¹ to a few hundreds of ng L⁻¹ in the case of wastewater. The instrumental and method intraday and interday repeatabilities were on average less than 5%. The method was successfully applied for the determination of pharmaceuticals in the River Taff (South Wales) and a wastewater treatment plant (WWTP Cilfynydd). Several pharmaceuticals and personal care products were determined in river water at levels ranging from single ng L⁻¹ to single μg L⁻¹.