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Evaluation of a Sequencing Batch Reactor Sewage Treatment Rig for Investigating the Fate of Radioactively Labelled Pharmaceuticals: Case Study of Propranolol

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Evaluation of a Sequencing Batch Reactor Sewage Treatment Rig for Investigating the Fate of Radioactively Labelled Pharmaceuticals: Case Study of Propranolol Water Research 88 (2016) 83e92 Contents lists available at ScienceDirect Water Research journal homepage: www.elsevier.com/locate/watres Evaluation of a sequencing batch reactor sewage treatment rig for investigating the fate of radioactively labelled pharmaceuticals: Case study of propranolol * T. Popple a, J.B. Williams a, ,E.Mayb, G.A. Mills c, R. Oliver d, 1 a School of Civil Engineering and Surveying, University of Portsmouth, Portsmouth, PO1 3AH, UK b School of Biological Sciences, University of Portsmouth, Portsmouth, PO1 2DY, UK c School of Pharmacy and Biomedical Sciences, University of Portsmouth, Portsmouth, PO1 2DT, UK d AstraZeneca Brixham Environmental Laboratory, Freshwater Quarry, Brixham, Devon, TQ5 8BA, UK article info abstract Article history: Pharmaceuticals are frequently detected in the aquatic environment, and have potentially damaging Received 11 December 2014 effects. Effluents from sewage treatment plants (STPs) are major sources of these substances. The use of Received in revised form sequencing batch reactor (SBR) STPs, involving cycling between aerobic and anoxic conditions to pro- 15 September 2015 mote nitrification and denitrification, is increasing but these have yet to be understood in terms of Accepted 17 September 2015 removal of pharmaceutical residues. This study reports on the development of a laboratory rig to Available online 21 September 2015 simulate a SBR. The rig was used to investigate the fate of radiolabelled propranolol. This is a commonly prescribed beta blocker, but with unresolved fate in STPs. Keywords: Propranolol The SBR rig (4.5 L) was operated on an 8 h batch cycle with settled sewage. Effective treatment was Radiolabelled compounds demonstrated, with clearly distinct treatment phases and evidence of nitrogen removal. Radiolabelled 14 Sewage treatment plant C-propranolol was dosed into both single (closed) and continuous (flow-through) simulations over 13 Sequencing batch reactors SBR cycles. Radioactivity in CO2 off-gas, biomass and liquid was monitored, along with the characteristics Laboratory simulation of the sewage. This allowed apparent rate constants and coefficients for biodegradation and solid:water partitioning to be determined. Extrapolation from off-gas radioactivity measurements in the single dose 4-d study suggested that propranolol fell outside the definitions of being readily biodegradable (DegT50 ¼ 9.1 d; 60% biodegra- dation at 12.0 d). During continuous dosing, 63e72% of propranolol was removed in the rig, but less than 14 À1 4% of dose recovered as CO2, suggesting that biodegradation was a minor process (Kbiol(M) Lkgd ¼ 22 e49) and that adsorption onto solids dominated, giving rise to accumulations within biomass during the 17 d solid retention time in the SBR. Estimations of adsorption isotherm coefficients were different depending on which of three generally accepted denominators representing sorption sites was used (mixed liquor suspended solids, reactor COD or mass of waste activated sludge). With further development and evaluation, the rig developed for simulating SBR processes has po- tential to be used for informing better environmental risk assessments for those pharmaceuticals showing ambiguous results in field fate studies. © 2015 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/). Abbreviations: API, active pharmaceutical ingredient; CAS, conventional acti- 1. Introduction vated sludge; DegT50, time taken for 50% removal (or half-life); DOC, dissolved organic carbon; HRT, hydraulic retention time; LSC, liquid scintillation counting; The occurrence of active pharmaceutical ingredients (APIs) in MLSS, mixed liquor suspended solids; PNEC, predicted no effects concentration; wastewater is the result of excretion by patients and improper SBR, sequencing batch reactor; SPE, solid-phase extraction; SRT, solid retention time; SS, suspended solids; STP, sewage treatment plant; WAS, waste activated disposal of medicines. This situation is likely to worsen due to sludge. growing populations and increasingly ageing demographics, lead- * Corresponding author. ing to increased usage of these chemicals (Arnold et al., 2013; E-mail address: [email protected] (J.B. Williams). Daughton and Ternes, 1999). Sewage treatment plants (STPs) 1 Present address: Syngenta Ltd, Jealott's Hill International Research Centre, generally have a sequence of discrete unit processes with different Bracknell, West Berkshire RG42 6EY, UK. http://dx.doi.org/10.1016/j.watres.2015.09.033 0043-1354/© 2015 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/). 84 T. Popple et al. / Water Research 88 (2016) 83e92 treatment mechanisms, typically combining solids separation and many laboratory simulation studies as their operating conditions biological oxidation. Removal of APIs in STPs is therefore deter- and microbial populations are easier to maintain compared to flow mined by the treatment processes utilized and the physicochemical through systems (Seviour and Nielsen, 2010). An advantage of properties and biodegradability of the chemicals themselves controlled laboratory studies is that radiolabelled compounds can (Drewes, 2007). However, STPs are dynamic systems, receiving be used to investigate the fate of chemicals. Radiolabelled 14C variable wastewater loads and are affected by environmental con- studies enable the fate of organic compounds to be established ditions, such as temperature. Perhaps as a consequence, reported with some confidence, but the carbon compounds associated with removal rates for APIs in STPs range from complete to almost the radioactivity (apart from CO2) are not resolved, unless specif- negligible (Gros et al., 2010; Kostrich et al., 2014) and consequently ically developed analytical methods are used (Federle and Itrich, many of these substances are detected in environmental waters 1997). Some radiolabelled studies have been undertaken on labo- (Verlicchi et al., 2012; Vulliet and Cren-Olive, 2011). Although APIs ratory scale CAS systems (Bouju et al., 2011; Cirja et al., 2007; À À generally occur at low concentrations (ng L 1 to mgL 1) in the Junker et al., 2006), but to our knowledge there are no studies on environment (Kosma et al., 2010), their bioactive nature makes the fate of radiolabelled APIs in a model SBR system. The study them potentially harmful to aquatic organisms (Williams, 2005). outlined in this paper aimed to develop a laboratory simulation of a The most widely used biological sewage treatment process is SBR plant, and undertake a 14C-labelled investigation to establish conventional activated sludge (CAS) (Metcalf and Eddy, 2003)in the fate of propranolol. This compound was selected as it a widely continuous flow reactors. Various CAS operating conditions have used API, whose reported removal efficiency in STPs has been very been shown to influence the removal of APIs, including mixed li- varied and typically low (Verlicchi et al., 2012). Propranolol is also quor suspended solids (MLSS) concentration, solid retention time included in the Chemicals Investigation Programme being under- (SRT) and hydraulic retention time (HRT) (Barbieri et al., 2011; taken by the UK water industry, where concentrations of pro- Suarez et al., 2012; Verlicchi et al., 2012). The Urban Waste Water pranolol in many UK STP effluents were found to be above the À Treatment Directive of the European Union 91/271/EEC (1991) re- predicted no effects concentration (PNEC) of 0.01 mgL 1; even after quires STPs discharging to environmentally-sensitive areas to assuming an environmental dilution of 1:10 (Gardner et al., 2012). remove nitrogen and/or phosphorus. Consequently, CAS is being Developing an understanding of the fate of APIs, such as pro- replaced at many locations by variants capable of biological pranolol in a range of sewage treatment systems is therefore nutrient removal (BNR). BNR plants incorporate aerobic, anoxic and important to inform better environmental risk assessments of anaerobic zones into the treatment system to act as selectors, medicinal products. Use of standard laboratory simulations for ‘switching on’ certain groups of bacteria, enabling them to under- investigating treatment technologies may also offer opportunities take nitrification, denitrification and/or phosphorus removal for selecting conditions for the most effective removal of these (Barker and Dold, 1997). Switching between conditions has been chemicals. shown to promote the removal of APIs in laboratory and field studies (Hu et al., 2005; Lubliner et al., 2010; Okuda et al., 2008; 2. Materials and methods Suarez et al., 2012; Tran et al., 2009; Wick et al., 2009). Sequencing batch reactors (SBRs) are a type of activated sludge All work was carried out at the AstraZeneca Brixham Environ- system operating in batch mode which are capable of BNR. Con- mental Laboratory, Devon, UK. Radiolabelled 14C-propranolol was ditions alternate between aerobic and anoxic during the batch supplied by AstraZeneca UK Ltd. and was stored at À20 C, its treatment cycle due to intermittent aeration (Seviour and Nielsen, chemical structure and purity is shown in the Supplementary 2010; Shaw et al., 2009). SBRs offer a high level of operational Material (SM) (Figs. S1 and S2). Primary settled sewage and MLSS control and generally have higher SRTs than CAS, enabling stable biomass were obtained, courtesy of South West Water Ltd.,
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