Determination of antibiotic residues in southern Baltic Sea sediments using tandem solid-phase extraction and liquid chromatography coupled with tandem mass spectrometry

• Autorzy: Siedlewicz G. , Borecka M. , Białk-Bielińska A. , Sikora K. , Stepnowski P. , Pazdro K.

Identyfikatory

DOI

10.1016/j.oceano.2016.04.005

• Języki publikacji: EN

Abstrakty

EN

The main objective of this study was to adapt analytical procedures for determining antibiotic residues in solid and aquatic samples to marine sediments and to investigate the occurrence of 9 sulfonamides, trimethoprim and 2 quinolones in southern Baltic Sea sediments. The analytical procedure was applied to sediment samples characterized as sand and silty sand. The validation results showed that a sensitive and efficient method applying tandem solid-phase extraction (SPE) and liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) was obtained. Analytes were determined in the lower ng g⁻¹ range with good accuracy and precision. The proposed analytical procedure was applied to the analysis of 13 sediment samples collected from the Baltic Sea along the Polish coast. Concentrations of antibiotic residues in environmental samples were calculated based on external matrix-matched calibration. Residues of nine out of twelve of the above antibiotics were detected in sediment samples in a concentrations of up to 419.2 ng g⁻¹ d.w. (dry weight). Sulfamethoxazole and sulfachloropyridazine were the most frequently detected compounds (58% of the analyzed samples). The occurrence frequency of trimethoprim was 42% and it was always detected simultaneously with sulfamethoxazole. Preliminary studies on the spatial distribution of the analyzed antibiotics indicate a high level of antibiotics occurring in the Pomeranian Bay and close to the mouths of Polish rivers. The study is the first one to demonstrate the occurrence of antibiotic residues in sediments of the Polish coastal area. The obtained results suggest that sediment can be an important secondary source of antibiotic residues in the marine environment.

Słowa kluczowe

EN

antibiotic residues; sediments; SPE; LC–MS/MS; Baltic Sea

PL

pozostałości antybiotyków; osady; SPE; LC-MS/MS; Morze Bałtyckie

• Wydawca: Polish Academy of Sciences, Institute of Oceanology ; Elsevier
• Czasopismo: Oceanologia
• Rocznik: 2016
• Tom: No. 58 (3)
• Strony: 221--234
• Opis fizyczny: Bibliogr. 92 poz., tab., mapy

Twórcy

autor

Siedlewicz G.

• Department of Marine Chemistry and Biochemistry, Institute of Oceanology, Polish Academy of Sciences, Sopot, Poland

autor

Borecka M.

• Department of Environmental Analysis, Faculty of Chemistry, University of Gdańsk, Gdańsk, Poland

autor

Białk-Bielińska A.

• Department of Environmental Analysis, Faculty of Chemistry, University of Gdańsk, Gdańsk, Poland

autor

Sikora K.

• Physicochemical Laboratories, Faculty of Chemistry, University of Gdańsk, Gdańsk, Poland

autor

Stepnowski P.

• Department of Environmental Analysis, Faculty of Chemistry, University of Gdańsk, Gdańsk, Poland

autor

Pazdro K.

• Department of Marine Chemistry and Biochemistry, Institute of Oceanology, Polish Academy of Sciences, Sopot, Poland

Bibliografia

• [1] Arnold, K. E., Brown, A. R., Ankley, T. G., Sumpter, J. P., 2014. Medicating the environment: assessing risks of pharmaceuticals to wildlife and ecosystem. Phil. Trans. R. Soc. B 369 (1656), 1—11, http://dx.doi.org/10.1098/rstb.2013.0569.
• [2] Babić, S., Ašperger, D., Mutavdžić, D., Horvat, A. J. M., Kaštelan- Macan, M., 2006. Solid phase extraction and HPLC determination of veterinary pharmaceuticals in wastewater. Talanta 70 (4), 732—738, http://dx.doi.org/10.1016/j.talanta.2006.07.003.
• [3] Bayen, S., Zhang, H., Desai, M. M., Ooi, S. K., Kelly, B. C., 2013. Occurrence and distribution of pharmaceutically active and endocrine disrupting compounds in Singapore's marine environment: influence of hydrodynamics and physical-chemical properties. Environ. Pollut. 182, 1—8, http://dx.doi.org/10.1016/j.envpol. 2013.06.028.
• [4] Beck, I. C., Bruhn, R., Gandrass, J., Ruck, W., 2005. Liquid chromatography—tandem mass spectrometry analysis of estrogenic compounds in coastal surface water of the Baltic Sea. J. Chromatogr. A 1090 (1—2), 98—106, http://dx.doi.org/10.1016/j.chroma.2005. 07.013.
• [5] Benotti, M. J., Brownawell, B. J., 2009. Microbial degradation of pharmaceuticals in estuarine and costal seawater. Environ. Pollut. 157 (3), 994—1002, http://dx.doi.org/10.1016/j.envpol. 2008.10.009.
• [6] Beretta, M., Britto, V., Tavares, T. M., da Silva, S. M. T., Pletsch, A. L., 2014. Occurrence of pharmaceutical and personal care products (PPCPs) in marine sediments in the Todos os Santos Bay and the north coast of Salvador, Bahia, Brazil. J. Soil. Sedim. 14 (7), 1278—1286, http://dx.doi.org/10.1007/s11368-014-0884-6.
• [7] Białk-Bielińska, A., Kumirska, J., Borecka, M., Caban, M., Paszkiewicz, M., Pazdro, K., Stepnowski, P., 2016. Selected analytical challenges in the determination of pharmaceuticals in drinking/marine waters and soil/sediment samples. J. Pharmaceut. Biomed. 121, 271—296, http://dx.doi.org/10.1016/j.jpba.2016.01.016.
• [8] Białk-Bielińska, A., Kumirska, J., Palavinskas, R., Stepnowski, P., 2009. Optimization of multiple reaction monitoring mode for the trace analysis of veterinary by LC-MS/MS. Talanta 80 (2), 947— 953, http://dx.doi.org/10.1016/j.talanta.2009.08.023.
• [9] Białk-Bielińska, A., Maszkowska, J., Mrozik, W., Bielawska, A., Kołodziejska, M., Palavinskas, R., Stepnowski, P., Kumirska, J., 2012. Sulfadimethoxine and sulfaguanidine: their sorption potential on natural soils. Chemosphere 86 (10), 1059—1065, http://dx.doi. org/10.1016/j.chemosphere.2011.11.058.
• [10] Boeckel, T. P., van Gandra, S., Ashok, A., Caudron, Q., Grenfell, B. T., Levin, S. A., Laxminarayan, R., 2014. Global antibiotic consumption 2000 to 2010: an analysis of national pharmaceutical sales data. Lancet Infect. Dis. 14 (8), 742—750, http://dx.doi.org/ 10.1016/S1473-3099(14)70780-7.
• [11] Borecka, M., Białk-Bielińska, A., Siedlewicz, G., Kornowska, K., Kumirska, J., Stepnowski, P., Pazdro, K., 2013. A new approach for the estimation of expanded uncertainty of results of an analytical method developed for determining antibiotics in sea-water using solid-phase extraction disks and liquid chromatography coupled with tandem mass spectrometry technique. J. Chromatogr. A 1304, 138—146, http://dx.doi.org/10.1016/j.chroma.2013.07.018.
• [12] Borecka, M., Siedlewicz, G., Haliński, Ł. P., Sikora, K., Pazdro, K., Stepnowski, P., Białk-Bielińska, A., 2015. Contamination of the southern Baltic Sea waters by the residues of selected pharmaceuticals: method development and field studies. Mar. Pollut. Bull. 94 (1—2), 62—71, http://dx.doi.org/10.1016/j.marpol- bul.2015.03.008.
• [13] Boxall, A. B., 2008a. Fate and transport of veterinary medicines in the soil environment. In: Aga, D. S. (Ed.), Fate of Pharmaceuticals in the Environment and in Water Treatment Systems. CRC Press, Boca Raton, 123—137.
• [14] Boxall, A. B., 2008b. Fate of veterinary medicines applied to soils. In: Kümmerer, K. (Ed.), Pharmaceuticals in the Environment: Sources, Fate, Effects and Risk. Springer, Berlin, 103—119, http://dx.doi.org/10.1007/978-3-540-74664-5_8.
• [15] Boxall, A. B., Blackwell, P., Cavallo, R., Kay, P., Tolls, J., 2002. The sorption and transport of a sulphonamide antibiotic in soil systems. Toxicol. Lett. 131 (1—2), 19—28.
• [16] Bu, Q., Wang, B., Huang, J., Deng, S., Yu, G., 2013. Pharmaceuticals and personal care products in the aquatic environment in China: a review. J. Hazard. Mater. 262, 189—211, http://dx.doi.org/ 10.1016/j.jhazmat.2013.08.040.
• [17] Caban, M., Migowska, N., Stepnowski, P., Kwiatkowski, M., Kumirska, J., 2012. Matrix effects and recovery calculations in analyses of pharmaceuticals based on the determination of b-blockers and b-agonists in environmental samples. J. Chromatogr. A 1258, 117— 127, http://dx.doi.org/10.1016/j.chroma.2012.08.029.
• [18] Capone, D. G., Weston, D. P., Millera, V., Shoemakera, C., 1996. Antibacterial residues in marine sediments and invertebrates following chemotherapy in aquaculture. Aquaculture 145 (1— 4), 55—75, http://dx.doi.org/10.1016/S0044-8486(96)01330-0.
• [19] Chang, H., Hu, J., Asami, M., Kunikane, S., 2008. Simultaneous analysis of 16 sulfonamide and trimethoprim antibiotics in environmental waters by liquid chromatography-electrospray tandem mass spectrometry. J. Chromatogr. A 1190 (1—2), 390—393, http://dx.doi.org/10.1016/j.chroma.2008.03.057.
• [20] Chen, K., Zhou, J. L., 2014. Occurrence and behavior of antibiotics in water and sediments from the Huangpu River, Shanghai, China. Chemosphere 95, 604—612, http://dx.doi.org/10.1016/j.chemosphere.2013.09.119.
• [21] Ciborowski, T., 2010. Organic matter. In: Bolałek, J. (Ed.), Physical, Biological and Chemical Studies on Marine Sediments, Wyd. UG, Gdańsk, 287—290, (in Polish).
• [22] Claessens, M., Vanhaecke, L., Wille, K., Janssen, C. R., 2013. Emerging contaminants in Belgian marine waters: single toxicant and mixture risks of pharmaceuticals. Mar. Pollut. Bull. 71 (1—2), 41— 50, http://dx.doi.org/10.1016/j.marpolbul.2013.03.039.
• [23] Daughton, C. G., Ternes, T. A., 1999. Pharmaceuticals and personal care products in the environment: agents of subtle changes. Environ. Health Perspect. 107 (6), 907—938.
• [24] Dzierżawski, A., Cybulski, W., 2012. The need for rational use of antibiotics in veterinary practice. Życie Weterynar. 87 (4), 316— 321, (in Polish).
• [25] García-Galán, M. J., Villagrasa, M., Diaz-Cruz, M. S., Barceló, D., 2010. LC-QqLIT MS analysis of nine sulfonamides and one of their acetylated metabolites in the Llobregat River basin. Quantitative determination and qualitative evaluation by IDA experiments. Anal. Bioanal. Chem. 397 (3), 1325—1334, http://dx.doi.org/ 10.1007/s00216-010-3630-y.
• [26] Gaw, S., Thomas, K. V., Hutchinson, T. H., 2014. Sources, impacts and trends of pharmaceuticals in the marine and coastal environment. Phil. Trans. R. Soc. B 369 (1656), 1—11, http://dx.doi.org/ 10.1098/rstb.2013.0572.
• [27] Gbylik-Sikorska, M., Posyniak, A., Mirowska, K., Gajda, A., Błądek, T., Śniegocki, T., Żmudzki, J., 2014. Occurrence of veterinary antibiotics and chemotherapeutics in fresh water, sediment, and fish of the rivers and lakes in Poland. B. Vet. I. Puławy 58 (3), 399— 404, http://dx.doi.org/10.2478/bvip-2014-0062.
• [28] González-Pleiter, M., Gonzalo, S., Rodea-Palomares, I., Leganés, F., Rosal, R., Boltes, K., Marco, E., Fernández-Piñas, F., 2013. Toxicity of five antibiotics and their mixtures towards photosynthetic aquatic organisms: implications for environmental risk assessment. Water Res. 47 (6), 2050—2064, http://dx.doi.org/10.1016/ j.watres.2013.01.020.
• [29] Halling-Sørensen, B., Nielsen, S. N., Lanzky, P. F., Ingerslev, F., Holten Lützhøft, H. C., Jørgensen, S. E., 1998. Occurrence, fate and effects of pharmaceutical substances in the environment — a review. Chemosphere 36 (2), 357—393, http://dx.doi.org/10.1016/ S0045-6535(97)00354-8.
• [30] Hampel, M., Mauffret, A., Pazdro, K., Blasco, J., 2012. Anionic surfactant linear alkylbenzene sulfonates (LAS) in sediments from the Gulf of Gdańsk (southern Baltic Sea, Poland) and its environmental implications. Environ. Monit. Assess. 184 (10), 6013— 6023, http://dx.doi.org/10.1007/s10661-011-2399-6.
• [31] Hektoen, H., Berge, J. A., Hormazabal, V., Yndestad, M., 1995. Persistence of antibacterial agents in marine sediments. Aquaculture 133 (3—4), 175—184, http://dx.doi.org/10.1016/0044- 8486(94)00310-K.
• [32] HELCOM, 2010. Hazardous substances in the Baltic Sea — an integrated thematic assessment of hazardous substances in the Baltic Sea, Baltic Sea Environment Proceedings No. 120B, http://www. helcom.fi/Lists/Publications/BSEP120B.pdf (accessed: 5 December 2015).
• [33] Hirsch, R., Ternes, T., Haberer, K., Kratz, K. L., 1999. Occurrence of antibiotics in the aquatic environment. Sci. Total Environ. 225 (1—2), 109—118, http://dx.doi.org/10.1016/S0048-9697 (98)00337-4.
• [34] Hörsing, M., Ledin, A., Grabic, R., Fick, J., Tysklind, M., la Cour, J. J., Andersen, H. R., 2011. Determination of sorption of seventy-five pharmaceuticals in sewage sludge. Water Res. 45 (15), 4470— 4482, http://dx.doi.org/10.1016/j.watres.2011.05.033.
• [35] Kemper, N., 2008. Veterinary antibiotics in the aquatic and terrestrial environment. Ecol. Indic. 8 (1), 1—13, http://dx.doi.org/ 10.1016/j.ecolind.2007.06.002.
• [36] Khetan, K., Collins, T. J., 2007. Human pharmaceuticals in the aquatic environment: a challenge to green chemistry. Chem. Rev. 107 (6), 2319—2364, http://dx.doi.org/10.1021/cr020441w.
• [37] Kim, S. C., Carlson, K., 2005. LC-MS2 for quantifying trace amounts of pharmaceutical compounds in soil and sediment matrices. TrAC-Trends Anal. Chem. 24 (7), 635—644, http://dx.doi.org/10.1016/ j.trac.2005.04.006.
• [38] Konat, J., Kowalewska, G., 2001. Polychlorinated biphenyls (PCBs) in sediments of the southern Baltic Sea. Sci. Total Environ. 280 (1—3), 1—15, http://dx.doi.org/10.1016/S0048-9697(01) 00785-9.
• [39] Kot-Wasik, A., Dębska, J., Namieśnik, J., 2007. Analytical techniques in studies of the environmental fate of pharmaceutical and personal-care products. TrAC-Trends Anal. Chem. 26 (6), 557— 568, http://dx.doi.org/10.1016/j.trac.2006.11.004.
• [40] Kotlarska, E., Łuczkiewicz, A., Pisowacka, M., Burzyński, A., 2015. Antibiotic resistance and prevalence of class 1 and 2 integrons in Escherichia coli isolated from two wastewater treatment plants, and their receiving waters (Gulf of Gdańsk, Baltic Sea, Poland). Environ. Sci. Pollut. Res. 22 (3), 2018—2030, http://dx.doi.org/ 10.1007/s11356-014-3474-7.
• [41] Kümmerer, K., 2008a. Antibiotics in the environment. In: Kümmerer, K. (Ed.), Pharmaceuticals in the Environment: Sources, Fate, Effects and Risk. Springer, Berlin, 75—93.
• [42] Kümmerer, K., 2008b. Effects of antibiotics and virustatics in the environment. In: Kümmerer, K. (Ed.), Pharmaceuticals in the Environment: Sources, Fate, Effects and Risk. Springer, Berlin, 223—244.
• [43] Kümmerer, K., 2008c. Pharmaceuticals in the environment — a brief summary. In: Kümmerer, K. (Ed.), Pharmaceuticals in the Environment: Sources, Fate, Effects and Risk. Springer, Berlin, 3—22.
• [44] Lalumera, G. M., Calamari, D., Galli, P., Castiglioni, S., Crosa, G., Fanelli, R., 2004. Preliminary investigation on the environmental occurrence and effects of antibiotics used in aquaculture in Italy. Chemosphere 54 (5), 661—668.
• [45] Lara-Martín, P., González-Mazo, E., Petrovic, M., Barceló, D., Brownawell, B. J., 2014. Occurrence, distribution and partitioning of nonionic surfactants and pharmaceuticals in the urbanized Long Island Sound Estuary (NY). Mar. Pollut. Bull. 85 (2), 710 pp., http://dx.doi.org/10.1016/j.marpolbul.2014.01.022.
• [46] Le, T. X., Munekage, Y., 2004. Residues of selected antibiotics in water and mud from shrimp ponds in mangrove areas in Viet Nam. Mar. Pollut. Bull. 49 (11—12), 922—929.
• [47] Le-Minh, N., Khan, S. J., Drewes, J. E., Stuetz, R. M., 2010. Fate of antibiotics during municipal water recycling treatment processes. Water Res. 44, 4295—4323.
• [48] Li, W., Shi, Y., Gao, L., Liu, J., Cai, Y., 2012. Occurrence of antibiotics in water, sediments, aquatic plants, and animals from Baiyangdian Lake in North China. Chemosphere 89 (11), 1307—1315, http://dx.doi.org/10.1016/j.chemosphere.2012.05.079.
• [49] Liang, X. M., Chen, B., Nie, X., Shi, Z., Huang, X., Li, X., 2013. The distribution and partitioning of common antibiotics in water and sediment of the Pearl River Estuary, South China. Chemosphere 92 (11), 1410—1416, http://dx.doi.org/10.1016/j.chemosphere. 2013.03.044.
• [50] Löffler, D., Ternes, T. A., 2003. Determination of acidic pharmaceuticals, antibiotics and ivermectin in river sediment using liquid chromatography-tandem mass spectrometry. J. Chromatogr. A 1021 (1—2), 133—144, http://dx.doi.org/10.1016/j.chroma.2003. 08.089.
• [51] Łuczkiewicz, A., Felis, E., Ziembińska, A., Gnida, A., Kotlarska, E., Olańczuk-Neyman, K., Górska-Surmacz, J., 2013. Resistance of Escherichia coli and Enterococcus spp. to selected antimicrobial agents present in municipal wastewater. J. Water Health 11 (4), 600—612, http://dx.doi.org/10.2166/wh.2013.130.
• [52] Luo, Y., Xu, L., Rysz, M., Wang, Y., Zhang, H., Alvarez, P. J., 2011. Occurrence and transport of tetracycline, sulfonamide, quinolone, and macrolide antibiotics in the Haihe River Basin, China. Environ. Sci. Technol. 45 (5), 1827—1833, http://dx.doi.org/ 10.1021/es104009s.
• [53] Majka, M., 2010. Development of methods for the isolation of sulfonamides from soils and preliminary analysis of processes of sorption. (MSc thesis). Univ. Gdańsk (in Polish).
• [54] Maszkowska, M., Kołodziejska, M., Białk-Bielińska, A., Mrozik, W., Kumirska, J., Stepnowski, P., Palavinskas, R., Krüger, O., Kalbe, U., 2013. Column and batch tests of sulfonamide leaching from different types of soil. J. Hazard. Mater. 260, 468—474, http:// dx.doi.org/10.1016/j.jhazmat.2013.05.053.
• [55] McEneff, G., Barron, L., Kelleher, B., Paull, B., Quinn, B., 2014. A year-long study of the spatial occurrence and relative distribution of pharmaceutical residues in sewage effluent, receiving marine waters and marine bivalves. Sci. Total Environ. 476—477, 317— 326, http://dx.doi.org/10.1016/j.scitotenv.2013.12.123.
• [56] Minh, T. B., Leung, H. W., Loi, I. H., Chan, W. H., So, M. K., Mao, J. Q., Choi, D., Lam, J. C., Zheng, G., Martin, M., Lee, J. H., Lam, P. K., Richardson, B. J., 2009. Antibiotics in the Hong Kong metropolitan area: ubiquitous distribution and fate in Victoria Harbour. Mar. Pollut. Bull. 58 (7), 1052—1062, http://dx.doi.org/10.1016/j.marpolbul.2009.02.004.
• [57] Molander, L., Gerstrand, M., Rudén, C., 2009. WikiPharma — a freely available, easily accessible, interactive and comprehensive database for environmental effect data for pharmaceuticals. Regul. Toxicol. Pharmacol. 55 (3), 367—371, http://dx.doi.org/ 10.1016/j.yrtph.2009.08.009.
• [58] Moreno-González, R., Rodriguez-Mozaz, S., Gros, D., Barceló, M., León, V. M., 2015. Seasonal distribution of pharmaceuticals in marine water and sediment from a Mediterranean coastal lagoon (SE Spain). Environ. Res. 138, 326—344, http://dx.doi.org/10.1016/j.envres.2015.02.016.
• [59] Mutavdžić-Pavlović, D. M., Babić, B., Horvat, A. J. M., Kaštelan- Macan, M., 2007. Sample preparation in analysis of pharmaceuticals. TrAC-Trends Anal. Chem. 26 (11), 1062—1875, http://dx. doi.org/10.1016/j.trac.2007.09.010.
• [60] Mutavdžić-Pavlović, D. M., Pinušić, T., Periša, M., Babić, S., 2012. Optimization of matrix solid-phase dispersion for liquid chromatography tandem mass spectrometry analysis of 12 pharmaceuticals in sediments. J. Chromatogr. A 1258, 1—15, http://dx.doi. org/10.1016/j.chroma.2012.08.025.
• [61] Na, G., Fang, X., Cai, Y., Ge, L., Zong, H., Yuan, X., Yao, Z., Zhang, Z., 2013. Occurrence, distribution, and bioaccumulation of antibiotics in coastal environment of Dalian, China. Mar. Pollut. Bull. 69 (1—2), 233—237, http://dx.doi.org/10.1016/j.marpolbul. 2012.12.028.
• [62] Na, G., Gu, J., Ge, L., Zhang, P., Wang, Z., Liu, Ch., Zhang, L., 2011. Detection of 36 antibiotics in costal waters using high performance liquid chromatography-tandem mass spectrometry. Chin. J. Oceanol. Limnol. 29 (5), 1039—1102, http://dx.doi.org/10.1007/s00343-011-0225-1.
• [63] Nikolaou, A., Meric, S., Fatta, D., 2007. Occurrence patterns of pharmaceuticals in water and wastewater environments. Anal. Bioanal. Chem. 387 (4), 1225—1234, http://dx.doi.org/10.1007/ s00216-006-1035-8.
• [64] Nödler, K., Voutsa, D., Licha, T., 2014. Polar organic micropollutants in the coastal environment of different marine systems. Mar. Pollut. Bull. 85 (1), 50—59, http://dx.doi.org/10.1016/j.marpol- bul.2014.06.024.
• [65] Pazdro, K., 2004. Persistent organic pollutants in sediments from the Gulf of Gdańsk. Ann. Environ. Prot. 6, 63—76.
• [66] Pazdro, K., Borecka, M., Siedlewicz, G., Białk-Bielińska, A., Stepnowski, P., 2016. Analysis of the residues of pharmaceuticals in marine environment: state-of-the-art, analytical problems and challenges. Curr. Anal. Chem. 12 (3), 202—226, http://dx.doi. org/10.2174/1573411012666151009193536.
• [67] Piekarek-Jankowska, H., 2010. Sediments classification. In: Bolałek, J. (Ed.), Physical, Biological and Chemical Studies on Marine Sediments, Wydawnictwo Uniwersytetu Gdańskiego, Gdańsk, 287—290, (in Polish).
• [68] Raich-Montiou, J., Folch, J., Compano, R., Granados, M., Prat, M. D., 2007. Analysis of trace sulfonamides in surface water and soil sample by liquid chromatography-fluorescence. J. Chromatogr. A 1172 (2), 186—193, http://dx.doi.org/10.1016/j.chroma.2007.10.010.
• [69] Ramirez, A. J., Brain, R. A., Usenko, S., Mottaleb, M. A., O'Donnell, J. G., Stahl, L. L., Wathen, J. B., Snyder, B. D., Pitt, J. L., Perez- Hurtado, P., Dobbins, L. L., Brooks, B. W., Chambliss, C. K., 2009. Occurrence of pharmaceuticals and personal care products in fish: results of a national pilot study in the United States. Environ. Toxicol. Chem. 28 (12), 2587—2597, http://dx.doi.org/10.1897/08-561.1.
• [70] Sacher, F., Lange, F. T., Brauch, H. J., Blankenhorn, I., 2001. Pharmaceuticals in groundwaters: analytical methods and results of a monitoring program in Baden-Württemberg, Germany. J. Chromatogr. A 938 (1—2), 199—210, http://dx.doi.org/10.1016/ S0021-9673(01)01266-3.
• [71] Sarmah, A., Meyer, M., Boxall, B., 2006. A global perspective on the use, sales, exposure pathways, occurrence, fate and effects of veterinary antibiotics (VAs) in the environment. Chemosphere 65 (5), 725—759.
• [72] Shepard, E. P., 1954. Nomenclature based on sand-silt-clay relation. J. Sedim. Petrol. 24 (3), 151—158.
• [73] Shi, H., Yang, Y., Liu, M., Yan, C., Yue, H., Zhou, J., 2014. Occurrence and distribution of antibiotics in the surface sediments of the Yangtze Estuary and nearby costal areas. Mar. Pollut. Bull. 83 (1), 317—323, http://dx.doi.org/10.1016/j.marpolbul.2014.04.034.
• [74] Siedlewicz, G., Pazdro, K., Borecka, M., Kornowska, K., Białk-Bielińska, A., Stepnowski, P., 2014. Determination of tetracyclines residues in the Gulf of Gdańsk (Southern Baltic Sea) sediments using a tandem solid-phase extraction with liquid chromatography coupled with tandem mass spektrometry. In: Zieliński, T., Pazdro, K., Dragan-Górska, A., Weydmann, A. (Eds.), Insights on Environmental Changes: Where the World is Heading. Springer International Publishing, Switzerland, 33—48.
• [75] Stewart, M., Olsen, G., Hickey, C. W., Ferreira, B., Jelić, A., Petrović, M., Barceló, D., 2014. A survey of emerging contaminants in the estuarine receiving environment around Auckland, New Zealand. Sci. Total Environ. 468—469, 202—210, http://dx.doi.org/10.1016/j.scitotenv.2013.08.039.
• [76] Sukul, P., Spiteller, M., 2006. Sulfonamides in the environment as veterinary drugs. Rev. Environ. Contam. Toxicol. 187, 67—101, http://dx.doi.org/10.1007/0-387-32885-8_2.
• [77] Szefer, P., Glasby, G. P., Pempkowiak, J., Kaliszan, R., 1995. Extraction studies of heavy-metal pollutants in surficial sediments from the southern Baltic Sea of Poland. Chem. Geol. 120 (1—2), 111— 126, http://dx.doi.org/10.1016/0009-2541(94)00103-F.
• [78] Taverniers, I., De Loose, M., Bockstaele, E., 2004. Trends in quality in the analytical laboratory. II. Analytical method validation and quality assurance. TrAC-Trends Anal. Chem. 23 (8), 535—551, http://dx.doi.org/10.1016/j.trac.2004.04.001.
• [79] Thiele-Bruhn, S., 2003. Pharmaceutical antibiotics compounds in soils — a review. J. Plant Nutr. Soil Sci. 166 (2), 145—167, http://dx.doi.org/10.1002/jpln.200390023.
• [80] Tolls, J., 2001. Sorption of veterinary pharmaceuticals in soils: a review. Environ. Sci. Technol. 35 (17), 3397—3406, http://dx.doi.org/10.1021/es0003021.
• [81] Van De Steene, J. C., Lambert, W. E., 2008. Comparison of matrix effects in HPLC-MS/MS and UPLC-MS/MS analysis of nine basic pharmaceuticals in surface waters. J. Am. Soc. Mass Spectrom. 19 (5), 713—718, http://dx.doi.org/10.1016/j.jasms.2008.01.013.
• [82] Vazquez-Roig, P., Andreu, V., Blasco, C., Picó, Y., 2012. Risk assessment on the presence of pharmaceuticals in sediments, soils and waters of the Pego-Oliva Marshlands (Valencia, eastern Spain). Sci. Total Environ. 440, 24—32, http://dx.doi.org/10.1016/j.sci- totenv.2012.08.036.
• [83] Weigel, S., Kuhlmann, J., Hühnerfuss, H., 2002. Drugs and personal care products as ubiquitous pollutants: occurrence and distribution of clofibric acid, caffeine and DEET in the North Sea. Sci. Total Environ. 295 (1—3), 131—141, http://dx.doi.org/10.1016/ S0048-9697(02)00064-5.
• [84] Wille, K., De Brabander, H. F., De Wulf, E., Van Caeter, P., Janssen, C. R., Vanhaecke, L., 2012. Coupled chromatographic and mass spectrometric techniques for the analysis of emerging pollutants in the aquatic environment. TrAC-Trends Anal. Chem. 35, 87— 108, http://dx.doi.org/10.1016/j.trac.2011.12.003.
• [85] Wille, K., Noppe, H., Verheyden, K., Vanden Bussche, J., De Wulf, E., Van Caeter, P., Janssen, C. R., De Brabander, H. F., Vanhaecke, L., 2010. Validation and application of an LC-MS/MS method for the simultaneous quantification of 13 pharmaceuticals in seawater. Anal. Bioanal. Chem. 397 (5), 1797—1808, http://dx.doi.org/10.1007/s00216-010-3702-z.
• [86] Wise, R., 2002. Antimicrobial resistance: priorities for action. J. Antimicrob. Chemother. 49 (4), 585—596, http://dx.doi.org/10.1093/jac/49.4.585.
• [87] Xu, J., Zhang, Y., Zhou, C., Guo, C., Wang, D., Du, P., Luo, Y., Wan, J., Meng, W., 2014. Distribution, sources and composition of antibiotics in sediment, overlying water and pore water from Taihu Lake, China. Sci. Total Environ. 497—498, 267—273, http://dx.doi.org/10.1016/j.scitotenv.2014.07.114.
• [88] Yang, J. F., Ying, G. G., Zhao, J. L., Tao, R., Su, H. C., Chen, F., 2010. Simultaneous determination of four classes of antibiotics in sediments of the Pearl Rivers using RRLC-MS/MS. Sci. Total Environ. 408 (16), 424—432, http://dx.doi.org/10.1016/j.scitotenv. 2010.03.049.
• [89] Yang, Y., Fu, J., Peng, H., Hou, L., Liu, M., Zhou, J. L., 2011. Occurrence and phase distribution of selected pharmaceuticals in the Yangtze Estuary and its coastal zone. J. Hazard. Mater. 190 (1—3), 588—596, http://dx.doi.org/10.1016/j.jhazmat.2011. 03.092.
• [90] Zhang, R., Tang, J., Li, J., Cheng, Z., Chaemfa, C., Liu, D., Zheng, Q., Song, M., Luo, C., Zhang, G., 2013. Occurrence and risks of antibiotics in the coastal aquatic environment of the Yellow Sea, North China. Sci. Total Environ. 450—451, 197—204, http://dx.doi.org/10.1016/j.scitotenv.2013.02.024.
• [91] Zhang, R., Zhang, G., Zheng, Q., Tang, J., Chen, Y., Xu, W., Zou, Y., Chen, X., 2012. Occurrence and risks of antibiotics in the Laizhou Bay, China: impacts of river discharge. Ecotoxicol. Environ. Safe. 80, 208—215, http://dx.doi.org/10.1016/j.ecoenv.2012. 03.002.
• [92] Zhou, L., Ying, G., Zhao, J., Yang, J., Wang, L., Yang, B., Liu, S., 2011. Trends in the occurrence of human and veterinary antibiotics in the sediments of the Yellow River, Hai River and Liao River in northern China. Environ. Pollut. 159 (7), 1877—2188, http://dx.doi.org/10.1016/j.envpol.2011.03.034.