Abstract
This work describes the development, optimization, and validation of a new method for the simultaneous determination of a wide range of pharmaceuticals (beta-blockers, lipid regulators…) and personal care products (fragrances, UV filters, phthalates…) in both aqueous and solid environmental matrices. Target compounds were extracted from sediments using pressurized hot water extraction followed by stir bar sorptive extraction. The first stage was performed at 1,500 psi during three static extraction cycles of 5 min each after optimizing the extraction temperature (50–150 °C) and addition of organic modifiers (% methanol) to water, the extraction solvent. Next, aqueous extracts and water samples were processed using polydimethylsiloxane bars. Several parameters were optimized for this technique, including extraction and desorption time, ionic strength, presence of organic modifiers, and pH. Finally, analytes were extracted from the bars by ultrasonic irradiation using a reduced amount of solvent (0.2 mL) prior to derivatization and gas chromatography–mass spectrometry analysis. The optimized protocol uses minimal amounts of organic solvents (<10 mL/sample) and time (≈8 h/sample) compared to previous existing methodologies. Low standard deviation (usually below 10 %) and limits of detection (sub-ppb) vouch for the applicability of the methodology for the analysis of target compounds at trace levels. Once developed, the method was applied to determine concentrations of these compounds in several types of sample (wastewater, seawater, pore water, and sediment) from Cadiz Bay (SW Spain). To our knowledge, these findings represent the first information available on the presence of some of the target compounds in the marine environment.
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Network of reference laboratories for monitoring of emerging environmental pollutants /http://www.norman-network.net/index_php.php?module=public/about_us/comment_substances&menu2=public/.
Bisceglia KJ, Yu JT, Coelhan M, Bouwer EJ, Roberts AL (2010) J Chromatogr A 1217:558–564
Quintana JB, Rodil R, Muniategui-Lorenzo S, López-Mahía P, Prada-Rodríguez D (2007) J Chromatogr A 1174:27–39
Durán-Alvarez JC, Becerril-Bravo E, Castro VS, Jiménez B, Gibson R (2009) Talanta 78:1159–1166
Azzouz A, Souhail B, Ballesteros E (2010) J Chromatogr A 1217:2956–2963
Xu J, Wu L, Chen W, Chang AC (2008) J Chromatogr A 1202:189–195
Pomati F, Castiglioni S, Zuccato E, Fanelli R, Vigetti D, Rossetti C, Calamari D (2006) Environ Sci Technol 40:2442–2447
Peck A (2006) Anal Bioanal Chem 386:907–939
Cottell A, Denyer SP, Hanlon GW, Ochs D, Maillard JY (2009) J Hosp Infect 72:71–76
Kuster M, López de Alda MJ, Barceló D (2004) TrAC-Trends Anal Chem 23:790–798
Winkler M, Headley JV, Peru KM (2000) J Chromatogr A 903:203–210
Baltussen E, Sandra P, David F, Cramer C (1999) J Microcol Sep 11:737–747
Pérez-Carrera E, León VM, Gómez-Parra A, González-Mazo E (2007) J Chromatogr A 1170:82–90
Lara-Martín PA, Gómez-Parra A, González-Mazo E (2006) J Chromatogr A 1114:205–210
Göbel A, Thomsen A, McArdell CS, Alder AC, Giger W, Theib N, Löffler D, Ternes TA (2005) J ChromatogrA 1085:179–189
Rice SL, Mitra S (2007) Anal Chim Acta 589:125–132
Hawthorne SB, Yang Y, Miller DJ (1994) Anal Chem 66:2912–2920
Concha-Graña E, Fernández-González V, Grueiro-Noche G, Muniategui-Lorenzo S, López-Mahía P, Fernández-Fernández E, Prada-Rodríguez D (2010) Chemosphere 79:698–705
Saleh A, Larsson E, Yamini Y, Jönsson JA (2011) J Chromatogr A 1218:1331–1339
Camino-Sánchez FJ, Zafra-Gómez A, Pérez-Trujillo JP, Conde-González JE, Marques JC, Vílchez JC (2011) Chemosphere 84:869–881
Ramírez N, Marcé RM, Borrull F (2011) J Chromatogr A 1218:156–161
Liu WM, Hu Y, Zhao JH, Xu Y, Guan YF (2005) J Chromatogr A 1095:1–7
León VM, Álvarez B, Cobollo MA, Muñoz S, Valor I (2003) J Chromatogr A 999:91–101
Gomez MJ, Herrera S, Sole D, Garcia-Calvo E, Fernandez-Alba AR (2011) Anal Chem 83:2638–2647
Rodil R, Moeder M (2008) J Chromatogr A 1179:81–88
Silva ARM, Nogueira JMF (2010) Anal Bioanal Chem 396:1853–1862
Lara-Martín PA, Petrovic M, Gómez-Parra A, Barceló D, González-Mazo E (2006) Environ Pollut 144:483–491
Petrovic M, Lacorte S, Viana P, Barceló D (2002) J Chromatogr A 959:15–23
Kawaguchi M, Ito R, Honda H, Endo N, Okanouchi N, Saito K, Seto Y, Nakazawa H (2008) J Chromatogr A 1200:260–263
Shrivastava A, Gupta VB (2011) Chron Young Sci 2:21–25
Valcarcel Y, Alonso SG, Rodriguez-Gil JL, Maroto RR, Gil A, Catalá M (2011) Chemosphere 82:1062–1071
Jonkers N, Laane RW, de Voogt P (2002) Environ Sci Technol 37:321–327
International Marketing Service, Pharmaceutical Market, Supplement generic pharmaceuticals (2010, December).
Kupper T, Plagellat C, Brändli RC, de Alencastro LF, Grandjean D, Tarradellas J (2006) Water Res 40:2603–2612
Cantwell MG, Wilson BA, Zhu J, Wallace GT, King JW, Olsen CR, Burgess RM, Smith JP (2010) Chemosphere 78:347–352
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This study has been supported under two regional research projects (RNM 5417 and RNM 6613) and a FPI fellowship funded by the “Consejería de Economía, Innovación y Ciencia” of the Regional Government of Andalusia.
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Pintado-Herrera, M.G., González-Mazo, E. & Lara-Martín, P.A. Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction–stir bar sorptive extraction–derivatization and gas chromatography–mass spectrometry. Anal Bioanal Chem 405, 401–411 (2013). https://doi.org/10.1007/s00216-012-6453-1
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DOI: https://doi.org/10.1007/s00216-012-6453-1