Table 1: HPLC gradient.
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Recent years have seen an increase in the monitoring of pharmaceutical residues in environmental water samples. A significant
number of contaminants from common drug classes with analytes at very low concentrations have been reported to be present
in rivers, streams and drinking water in both Europe and the US. Common classes including cholesterol-lowering drugs, antibiotics,
analgesics, antiseptics and beta-blockers have been detected.
A suite of pharmaceutical compounds were identified as potential environmental contaminants by the UK Environment Agency.
These compounds exhibit a wide range of functionality and polarity (logP).
This Application Note describes the extraction of 19 pharmaceuticals from river water using EVOLUTE ABN SPE Columns followed
by LC–MS–MS analysis.
EVOLUTE ABN is a resin-based non-polar SPE column developed for the extraction a wide range of compounds from aqueous sample
matrices.
Experimental Procedure
Sample Preparation
Water samples (500 mL) were spiked at 100 ng/L concentration of the compounds listed above.
Generic SPE method:
SPE column: EVOLUTE ABN 50 μm, 200 mg/6 mL
Sample pre-treatment: None
Column solvation: Methanol (6 mL)
Column equilibration: Water (6 mL)
Sample load: 500 mL at a flow-rate of approx 15 mL/min (–10" Hg)
Interference elution: Water (6 mL)
Elution: Methanol containing 5% (v/v) NH4OH (6 mL)
Evaporate to dryness. Reconstitute in 500 μL methanol, add 500 μL water prior to injection.
HPLC Conditions
Instrument: Waters Alliance 2795 Separations Module.
Column: Zorbax Eclipse XDB-C18. (100 × 2.1 mm, 3.5 μm) Agilent
Guard column: Zorbax Eclipse XDB-C8. (12.5 × 2.1 mm, 5 μm) Agilent
Injection volume: 10 μL
Flow-rate: 0.25 mL/min
MS Conditions
Instrument: Waters Quattro Ultima Pt triple quadrupole MS equipped with an electrospray source.
Source temperature: 100 °C
Desolvation temperature: 350 °C
Collision cell pressure: 2.23 ×10-3 mbar
Figure 1
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ResultsConclusions
A single robust method for the solid-phase extraction of 19 pharmaceuticals has been developed. It forms the basis of a generic
approach to analyte extraction to which additional compounds can be included with minimal method development time.
Acknowledgements
We would like to thank Anthony Gravell & Richard Brodrick (Environment Agency, National Laboratory Service, 19 Penyfai Lane,
Furnace, Llanelli, SA15 4EL, UK) for their invaluable contribution to the development of the SPE method.
Matthew Cleeve, Lee Williams, Helen Lodder and Joanna Smith, Biotage UK Ltd, Hengoed, Mid Glamorgan, UK.
Biotage UK Ltd
Dyffryn Business Park, Ystrad Mynach, Hengoed,
Mid Glamorgan CF82 7RJ, UK
tel. +44 1443 811811 fax: +44 1443 816552
E-mail: order@eu.biotage.com
Website: http://www.biotage.com/
