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  • A solid-phase extraction method for rapidly determining the adsorption coefficient of pharmaceuticals in sewage sludge.

A solid-phase extraction method for rapidly determining the adsorption coefficient of pharmaceuticals in sewage sludge.

Water research (2014-10-10)
Laurence Berthod, Gary Roberts, David C Whitley, Alan Sharpe, Graham A Mills
ABSTRACT

The partitioning of pharmaceuticals in the environment can be assessed by measuring their adsorption coefficients (Kd) between aqueous and solid phases. Measuring this coefficient in sewage sludge gives an indication of their partitioning behaviour in a wastewater treatment plant and hence contributes to an understanding of their subsequent fate. The regulatory approved method for measuring Kd in sewage sludge is the US Environmental Protection Agency's Office of Prevention, Pesticides and Toxic Substances (OPPTS) guideline 835.1110, which is labour intensive and time consuming. We describe an alternative method for measuring the Kd of pharmaceuticals in sewage sludge using a modified solid-phase extraction (SPE) technique. SPE cartridges were packed at different sludge/PTFE ratios (0.4, 6.0, 24.0 and 40.0% w/w sludge) and eluted with phosphate buffer at pH 7.4. The approach was tested initially using three pharmaceuticals (clofibric acid, diclofenac and oxytetracycline) that covered a range of Kd values. Subsequently, the sorption behaviour of ten further pharmaceuticals with varying physico-chemical properties was evaluated. Results from the SPE method were comparable to those of the OPPTS test, with a correlation coefficient of 0.93 between the two approaches. SPE cartridges packed with sludge and PTFE were stable for up to one year; use within one month reduced variability in measurements (to a maximum of 0.6 log units). The SPE method is low-cost, easy to use and enables the rapid measurement of Kd values for a large number of chemicals. It can be used as an alternative to the more laborious full OPPTS test in environmental fate studies and risk assessments.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ibuprofen
Supelco
Ibuprofen, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Clofibric acid, analytical standard
Ibuprofen for peak identification, European Pharmacopoeia (EP) Reference Standard
Ibuprofen, European Pharmacopoeia (EP) Reference Standard
Felodipine, European Pharmacopoeia (EP) Reference Standard
USP
Oxytetracycline, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
2-(p-Chlorophenoxy)-2-methylpropionic acid, 97%
Sigma-Aldrich
Felodipine, solid
Sigma-Aldrich
Ibuprofen, ≥98% (GC)
Bicalutamide, European Pharmacopoeia (EP) Reference Standard
USP
Ibuprofen, United States Pharmacopeia (USP) Reference Standard
Supelco
Oxytetracycline, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Methanol, Absolute - Acetone free
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
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Methanol, NMR reference standard
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Methanol, anhydrous, 99.8%
Supelco
Methanol, analytical standard
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Methanol, suitable for HPLC, gradient grade, ≥99.9%
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Methanol, HPLC Plus, ≥99.9%
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Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
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Methanol, suitable for HPLC, ≥99.9%
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Methanol, anhydrous, ≥99.5%
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Methanol, AR, ≥99.5%
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Methanol, LR, ≥99%
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Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%