alexa Combined microwave-assisted extraction and continuous solid-phase extraction prior to gas chromatography-mass spectrometry determination of pharmaceuticals, personal care products and hormones in soils, sediments and sludge.
Pharmaceutical Sciences

Pharmaceutical Sciences

Pharmaceutica Analytica Acta

Author(s): Azzouz A, Ballesteros E

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Abstract This paper reports a sensitive analytical method based on microwave-assisted extraction and continuous solid-phase extraction (SPE), followed by gas chromatography-mass spectrometry (GC-MS), for the simultaneous determination of residues of 18 pharmaceuticals (analgesics, antibacterials, anti-epileptics, β-blockers, lipid regulators and non-steroidal anti-inflammatories), one personal care product and 3 hormones in soils, sediments and sludge. The analytes are extracted with 3:2 methanol/water under the action of microwave energy and the resulting extract is passed through a SPE column to clean up the sample matrix and preconcentrate the analytes. Then, the analytes, trapped on Oasis-HLB sorbent, are eluted with ethyl acetate, silylated and determined by GC-MS. The proposed method provides a linear response over the concentration range 2.5-20,000 ng/kg with correlation coefficients higher than 0.994 in all cases. Also, it features low limits of detection (0.8-5.1 ng/kg), good precision (within- and between-day relative standard deviation less than 7\%) and recoveries ranging from 91 to 101\%. The method was successfully applied to agricultural soils, river and pond sediments, and sewage sludge. All samples contained some target analyte and sludge contained most -some at considerably high concentrations. Copyright © 2011 Elsevier B.V. All rights reserved. This article was published in Sci Total Environ and referenced in Pharmaceutica Analytica Acta

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