Pharmaceutical Residues Within Sewage Sludges
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Resource or Project Abstract
A total of 61 PPCPs were chosen to encompass a wide variety of therapeutic classes specifically deriving from antibiotics, analgesics, non-steroidal anti inflammatory drugs (NSAIDS), beta-blockers, anti-psychotics and illicit drugs of abuse. Many of these compounds were chosen based on sales data for the Republic of Ireland (Irish Medicines Board) and Norway. Antibiotics were of particular concern and a selection of 14 compounds covering sulfonamides, macrolides, fluoroquinolones, antibacterials, bacteriostatics and antifungals were included. An analytical method was developed to determine a large selection of frequently prescribed and consumed pharmaceuticals in biosolid enriched soils and digested sludges. Using a combination of pressurised liquid extraction (PLE), solid phase extraction (SPE) and liquid chromatography with tandem mass spectrometry (LC-MS/MS), it was possible to detect analytes in each sample type at the low-sub ng/g level. Solid phase extraction efficiencies were compared for 6 different sorbent types and it was found that Waters Oasis HLB cartridges offered enhanced selectivities with 20 analytes showing final method recoveries ≥ 60 % in both soils and digested sludges. The method was validated for linearity, range, precision and limits of detection in both sample matrices. All analytes were then determined in sludge enriched soils as well as the precursor thermally dried sludge fertilizer produced from a primary wastewater treatment plant. Levels of the antibacterial agent triclosan were found to exceed 20 µg/g in digested sludge and 5 µg/g in thermally dried sludge cake. Significant traces of carbamazepine and warfarin were also detected in the above samples. Alternative separation methods were also investigated and involved the characterisation of ultra-high pressure liquid chromatography and long monolithic column technologies to reduce ion suppression effects in mass spectrometry. A broad screening analytical method development study was conducted for the simultaneous determination of 43 PPCPs in sewage sludges from Norway and Sweden. By utilising PLE, mixed mode SPE (strong cation exchange-reversed phase) and ultra-high pressure liquid chromatography-tandem mass spectrometry, 15 PPCPs were identified in sludges taken from 5 independent wastewater treatment facilities across Scandinavia. Corroboration with Irish data was found in the occurrence of selected PPCPs at the low-mid µg/g level. A comprehensive analytical investigation of the sorption behaviour 54 PPCPs to soils and freeze-dried digested sludges is presented. Batch sorption experiments were carried out to identify which compounds could potentially concentrate in soils as a result of biosolid enrichment. Analysis of aqueous samples was carried out directly using LC-MS/MS. For solids analysis, combined PLE and SPE methods were used prior to LC-MS/MS. Solid?water distribution coefficients (Kd) were calculated based on slopes of sorption isotherms over a defined concentration range. The use of artificial neural networks to identify patterns in sorption behaviour was investigated for 54 PPCPs. Molecular descriptors such as logP, pKa, molar refractivity, aromatic ratio, hydrophilic factor and topological surface area were collected for all solutes and, along with generated Kd data, were incorporated as a training set within a developed artificial neural network to predict Kd for all solutes within both sample types. Therefore, this work represents a novel approach using combined and cross-validated analytical and computational techniques to confidently study sorption modes within the environment. The logarithm plots of predicted versus experimentally determined Kd are presented which showed excellent correlation (R2 > 0.88), highlighting that artificial neural networks could be used as an intelligent predictive tool for this application. To evaluate the developed model, it was used to predict Kd for meclofenamic acid, mefenamic acid, ibuprofen and furosemide and subsequently compared to experimentally determined values in soil. Ratios of experimental/predicted Kd values were found to be 1.00, 1.00, 1.75 and 1.65, respectively. Using a glass column packed with soil and under conditions of constant simulated rainfall, the application of sewage sludge contaminated with 12 PPCPs was studied. It was found that some PPCPs showed strong leaching potential to groundwater after 6 months average rainfall, whilst others displayed higher retention behaviour and showed the potential to concentrate in soils with added exposure. A mass balance of PPCPs in all compartments was carried out and it was found that 8 out of 12 compounds suffered some recovery losses, most likely due to biological or chemical transformation.
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Access Information For This Resource
| SAFER-Data Display URL | https://eparesearch.epa.ie/safer/iso19115/display?isoID=109 |
| Resource Keywords | Pharmaceuticals, soil, sludge, liquid chromatography, mass spectrometry, pressurised liquid extraction, solid-water partition coefficient, artificial neural networks, mobility |
| EPA/ERTDI/STRIVE Project Code | 2005-FS-30-M1 |
| EPA/ERTDI/STRIVE Project Theme | Land-use, Soils, and Transport |
| Resource Availability: |
 Public-Open |
| Limitations on the use of this Resource | In the event of obtaining access to datasets corresponding to this resource any datasets, data, or information resources being used in a journal article or other means of publication the original authors should be informed of this usage and an appropriate acknowledgement or citation is included within the published article. The EPA advise that this acknowledgement should take one of the following forms dependent upon how heavily the published work relates to the downloaded data: * Co-Authorship(s) for the original author(s)* Written acknowledgement within the body of the article* Written acknowledgement by means of the inclusion of a bibliography entry which clearly cites the original authors. |
| Number of Attached Files (Publicly and Openly Available for Download): | 0 |
| Project Start Date | Saturday 1st April 2006 (01-04-2006) |
| Earliest Recorded Date within any attached datasets or digital objects | Saturday 1st April 2006 (01-04-2006) |
| Most Recent Recorded Date within any attached datasets or digital objects | Tuesday 31st March 2009 (31-03-2009) |
| Published on SAFER | Tuesday 21st April 2009 (21-04-2009) |
| Date of Last Edit | Tuesday 21st April 2009 at 06:42:13 (21-04-2009) |
| Datasets or Files Updated On | Tuesday 21st April 2009 at 06:38:49 (21-04-2009) |
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Geographical and Spatial Information Related To This Resource
Description of Geographical Characteristics of This Project or Dataset
A total of 61 PPCPs were chosen to encompass a wide variety of therapeutic classes specifically deriving from antibiotics, analgesics, non-steroidal anti inflammatory drugs (NSAIDS), beta-blockers, anti-psychotics and illicit drugs of abuse. Many of these compounds were chosen based on sales data for the Republic of Ireland (Irish Medicines Board) A broad screening analytical method development study was conducted for the simultaneous determination of 43 PPCPs in sewage sludges from Norway and Sweden.
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Supplementary Information About This Resource
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| Lineage information about this project or dataset |
| Scope and Project Aims The potential threat of pharmaceuticals and personal care products (PPCPs) to the environment has emerged as a topic of concern in recent years. To date, there exists a dearth of analytical methods to empirically determine their occurrence in solid media. This pioneering 3-year research and development project focused on a number of topics surrounding the exposure of pharmaceuticals to the terrestrial environment through land-spreading of municipal biosolids (sludges) on agricultural land. To date, this project represents one of fewer than ten research efforts world-wide to comprehensively address this topic. More specifically, the aims of the project were: ? To identify which PPCPs may occur at significant levels in wastewater treatment sludges; ? To develop robust analytical methods for soil and sludge analysis; ? To compare any occurrence data with that from a European case-study; ? To determine the solid-water partition coefficient for all compounds in aqueous sewage sludge and soil suspensions; ? To model sorption data in order to identify preferred sorption modes in the environment; ? To assess the mobility of such compounds in sewage sludge amended soils after exposure to rainfall. Currently, there exists no legislation for PPCPs in biosolids and very few agencies have yet to characterise the effects of such compounds in the environment. However, the OSPAR convention stands alone as the only body to consider pharmaceuticals as a threat to the marine environment. Pharmaceutical agents, clotrimazole, (a common antifungal agent) and diosgenin (steroid) have very recently been listed for priority action whilst 19 other drugs including chlorpromazine (anti-psychotic) have been highlighted as of possible concern on a secondary listing which is to be further updated in 2009. |
| Supplementary Information |
| Software:
Agilent Chemstation, Bruker Daltonics Esquire and Trajan Neural Networks Software for instrument control, data aquisition and data interpretation. All figures and datasets were processed through Microsoft Office. Acknowledgements: Special thanks are due to the technical and administrative staff at the NCSR, as well as the School of Chemical Sciences for part-funding both instrument purchase, conference attendance and travel costs for visiting research collaborators specific to this project. The authors would also like to thank the members of Dr. Brian Kelleher?s research group at Dublin City University for supplementary input to the project. |
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