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Ojemaye Phd 2020 12.Pdf IDENTIFICATION AND QUANTIFICATION OF CHEMICALS OF EMERGING CONCERN (PERSISTENT ORGANIC AND INORGANIC POLLUTANTS) IN SOME SELECTED MARINE ENVIRONMENTS OF CAPE TOWN, SOUTH AFRICA By Cecilia Yejide Ojemaye B.Sc (Chemistry) - University of Ilorin, Kwara, Nigeria M.Sc (Analytical Chemistry) - University of Lagos, Lagos, Nigeria A thesis submitted in fulfillment of the requirements for the degree of Doctor of Philosophy in Chemistry in the Department of Chemistry, University of the Western Cape, South Africa Supervisor: Prof. Leslie F. Petrik October 2020 http://etd.uwc.ac.za/ KEYWORDS Bioaccumulation Cape Town Chemicals of emerging concern Contaminants Ecological risk Endocrine disrupting compounds Fish Gas chromatography-mass sectrometry Herbicides Human health risk Hydrophilic-lipophilic balance Inductively Coupled Plasma Optical Emission Spectrometry Industrial chemicals Liquid chromatography-mass sectrometry Marine biota Marine environment Marine organisms Metals Perfluorinated compounds Pharmaceuticals and personal care product Pollutants Risk assessment I http://etd.uwc.ac.za/ Seawater Seaweed Sediment Solid phase extraction II http://etd.uwc.ac.za/ ABSTRACT The increasing evidence of chemicals of emerging concern (CECs) in water bodies is causing major concern around the world because of their toxicological effects upon humans and aquatic organisms. The release of wastewater to the aquatic environment is most likely to introduce some trace levels of organic contaminants, some of which may be toxic, carcinogenic, or endocrine disruptors, as well as, persistent in the environment. These compounds are often persistent but not regularly monitored because they are mostly still excluded from environmental legislation. Their fate and persistence in the environment are not well understood. Additionally, increasing contamination of marine ecosystem due to the inability of wastewater treatment plants to remove these contaminants have become a global issue. The presence of these pollutants in the marine ecosystem may have negative effects on marine biota and often pose potential human health risks through consumption of contaminated seafood. Why this study focused on the identification and quantification of chemicals of emerging concern is because of the very large volumes of untreated sewage discharged into the marine in the marine environment of Cape Town including Kalk Bay, Green Point, Camps Bay and False Bay. Solid phase extraction (SPE) method based on Oasis HLB cartridges were used to extract and clean-up the samples for 16 target chemical compounds (pharmaceuticals and personal care products, perfluorinated compounds and industrial chemicals) using Liquid chromatography–mass spectrometry analysis. A miniature QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was used to extract herbicides samples and analyse them using Gas chromatography–mass spectrometry III http://etd.uwc.ac.za/ analysis. Metal extraction was carried out using acid digestion method followed by inductively coupled plasma - optical emission spectrometry. These analysis were done on selected commercially exploited, wild caught small and medium sized pelagic fish species (Thyrsites atun, Sarda orientalis, Pachymetopon blochii and Pterogymnus laniarius) obtained from Kalk Bay harbour only as well as on seawater, sediments and marine biota samples sea (Ulva sp., Codium fragile, Gelidium pristoides, Bifurcaria brassicac formis, Caulerpa filiformis, Aeodes Orbitosa, Oxystele sinensis, Oxystele tigrina, Cymbula granatina, Marthasterias glacialis, Mytilus galloprovincialis and Parechinus angulosus) sampled from Green Point, Camps Bay and False Bay. The results revealed that perfluorodecanoic acid, perfluorononanoic acid and perfluoroheptanoic acid were the most predominant among the perfluorinated compounds. They were discovered at concentration ranges of 20.13-179.2 ng/g, 21.22 - 114.0 ng/g and 40.06 -138.3 ng/g respectively, measured from dry weight (dw) of fish species and their organs. Also diclofenac had the highest concentration in these edible fish species out of all the pharmaceuticals detected (range: 551.8 – 1812 ng/g). The concentration detected for herbicides in the fish samples ranged from atrazine: not detected (nd) to 65.87 ng/g dw, simazine: nd to 157.82 ng/g dw, alachlor: nd to 47.44 µg/g dw, metolachlor: nd to 94.30 ng/g dw and butachlor: nd to 8.52 ng/g dw. The heavy metal concentrations found in fish tissues varied for Cu: 18.0 – 131.0, Zn: 105.6 – 234.5, Mn: 2.12 – 10.3, Fe: 362.6 – 443.9, Cr: nd – 11.5, Co: 0.6 – 3.7, Ni: 9.9 – 26.5, Sr: 71.6 – 687.7 and Nb: 418.3 - 420.9 mg/kg dry weight. Cd was not detected in any tissues of the fish species all in dry weight. The results observed from Green Point samples showed that all the PFCs were dominant in seawater (0.01 – 1.06 ng/ L), sediment (0.65 – 3.51 ng/g dry weight (dw)), benthic IV http://etd.uwc.ac.za/ organisms (0.15 – 12.72 ng/g dw) and seaweed samples (0.19 – 1.94 ng/g dw). Pharmaceuticals and personal care product ranged from: seawater (0.07 – 4.79 ng/L), sediments (0.79 - 4.48 ng/g dw), benthic organisms (0.38 - 10.72 ng/g dw) and seaweed (0.51- 6.60 ng/g dw). Bisphenol A was the most dominant compound out of the industrial chemical compounds, and ranged between: 0.07 – 0.20 ng/L, 3.14 -3.25 ng/g, 2.45 – 7.97 ng/g in seawater, sediment and benthic organisms, respectively and was 3.60 ng/g in seaweed. The results revealed the presence of four of these sewage derived compounds in seawater samples, seven compounds in sediment samples, five compounds in seaweed and seven in benthic organisms from Camps Bay. The results showed that diclofenac was the dominant pharmaceutical in seawater (range: 0.73-2.86 ng/ L), sediments (range: 110.9-357.45 ng/g dry weight (dw)) and marine organisms (range: 67.47-314.04 ng/g dw) while perfluoroheptanoic acid was the dominant PFC in seawater (range: 0.21-0.46 ng/ L), sediments (range: 86.28-149.73 ng/g dw) and marine organisms (range: 258.97-282.58 ng/g dw). Especially, seaweed was an excellent accumulation matrix for perfluorodecanoic, perfluorononanoic and perfluorooctanoic acids, since their concentrations were 764 ng/g, 504.52 ng/g and 597.04 ng/g in dried sample, respectively. The average concentration of the herbicides were from their quantification limit concentrations up to 45.32 ng/g (dw) and 157 ng/g (dw) in sediment and benthic organisms, respectively, and at 12.25-87.04 ng/g (dw) level in seaweed samples. The toxic metal concentrations found in sediment and biota samples varied from Cu: 1.18 – 58.76, Zn: 2.40 – 821.50, Mn: 5.38 – 50.37, Fe: 291.94 – 9287.87, Cr: not detected – 12.73, Co: 0.03 – 11.09, Ni: 4.28 – 19.90, Sr: 250.32 – 5146.24, Pb: 2.03 – 233.17, As: 0.35 – 19.70, Ti: V http://etd.uwc.ac.za/ 4.90 – 97.44, Mo: 0.13 – 13.04 and Nb: 0.47 – 422.3 mg/kg dry weight while the detected metal concentration in seawater varied from Zn: not detected – 0.01, Sr: 5.67 – 5.97, As: 0.01 – 0.02, Mo: 0.01 mg/L. The results observed from False Bay sample analysis showed that all the PFCs were dominant in seawater (range: 1.23-18.76 ng/ L), sediment (range: 43.85 -239.65 ng/g dry weight (dw)), benthic organisms (ranged: 36.48 – 2444.87 ng/g dw) and seaweed samples (range: 13.86 – 2309.23 ng/g dw). Pharmaceuticals ranged from: seawater (0.07 – 4.79 ng/L), sediments (8.89-171.89 ng/g (dw)), benthic organisms (14.02 -780.26 ng/g dw) and seaweed (8.46 - 309.11 ng/g dw). Nonylphenol was the most dominant compound out of the industrial chemical compounds, however it was not detected in seawater samples and its concentration ranged from: sediment (5.18 – 582.58 ng/g), marine organisms (339.20 – 2235.35 ng/g) and seaweed (41.57 – 1358.82 ng/g). Out of the sampling locations, False Bay samples had the highest concentrations of these contaminants, this may be due to the very large volume of partially treated sewage discharged in that location because there are about five sewage plants situated around the Bay. Also, among the matrices, marine organisms including fish have highly accumulated the contaminants followed by sediment samples compared to concentrations found in seawater. This indicates and confirms the bioaccumulating nature of the contaminants in marine organisms. Furthermore, diclofenac, simazine and atrazine for pharmaceuticals and pesticides respectively were the predominant contaminants in the different environmental matrices across the different sampling locations/sites, an indication of the frequent use of these compounds by residents and industries in Cape Town. VI http://etd.uwc.ac.za/ Ecological risk assessment values for acute and chronic risk calculated following the US Environmental Protection Agency method were above acceptable limit, (that is) the assessment results were greater than 0.5 for acute risk and 1.0 chronic risk which show that these chemicals have a high health risk to the pelagic fish, aquatic organisms and to humans who consume them. The human risk evaluation (non-carcinogenic and carcinogenic risk) were also above the acceptable level, indicating that the concentration of these chemical contaminants in the selected fish samples and marine organisms were at levels where there is a possibility of developing cancers should the seafood and fish be consumed over a period of time. Therefore, it can be concluded that these contaminants in edible parts of the examined species could pose health problems for consumers, if agricultural and recreational practices in the surroundings of the bay increases. This study reveals the impact of the chemical load being discharged together with sewage, upon the local marine environment.
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