Abstract
Organic micropollutants such as pharmaceuticals, perfluorinated compounds (PFCs), and pesticides, are important environmental contaminants. To obtain more information regarding their presence in marine organisms, an increasing demand exists for reliable analytical methods for quantification of these micropollutants in biotic matrices. Therefore, we developed extraction procedures and new analytical methods for the quantification of 14 pesticides, 10 PFCs, and 11 pharmaceuticals in tissue of marine organisms, namely blue mussels (Mytilus edulis). This paper presents these optimized analytical procedures and their application to M. edulis, deployed at five stations in the Belgian coastal zone. The methods consisted of a pressurized liquid extraction and solid-phase extraction (SPE) followed by ultra high-performance liquid chromatography coupled to triple quadrupole mass spectrometry for pharmaceuticals and pesticides, and of a liquid extraction using acetonitrile and SPE, followed by liquid chromatography coupled to time-of-flight mass spectrometry for PFCs. The limits of quantification of the three newly optimized analytical procedures in M. edulis tissue varied between 0.1 and 10 ng g−1, and satisfactory linearities (≥0.98) and recoveries (90–106%) were obtained. Application of these methods to M. edulis revealed the presence of five pharmaceuticals, two PFCs, and seven pesticides at levels up to 490, 5, and 60 ng g−1, respectively. The most prevalent micropollutants were salicylic acid, paracetamol, perfluorooctane sulfonate, chloridazon, and dichlorvos.
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Van De Vijver KI, Hoff PT, Das K, Esmans EL, Jauniaux T, Bouquegneau J-M, Blust R, De Coen W (2003) Environ Sci Technol 37:5545–5550
Hogenboom AC, van Leerdam JA, de Voogt P (2009) J Chromatogr A 1216:510–519
Weigel S, Bester K, Hühnerfuss H (2001) J Chromatogr A 912:151–161
Noppe H, Ghekiere A, Verslycke T, De Wulf E, Verheyden K, Monteyne E, Polfliet K, Van Caeter P, Janssen CR, De Brabander HF (2007) Environ Pollut 147:668–676
Ahrens L, Felizeter S, Ebinghaus R (2009) Chemosphere 76:179–184
Wille K, Noppe H, Verheyden K, Vanden Bussche J, De Wulf E, Van Caeter P, Janssen CR, De Brabander HF, Vanhaecke L (2010) Anal Bioanal Chem 397:1797–1808
Wille K, Vanden Bussche J, Noppe H, De Wulf E, Van Caeter P, Janssen CR, De Brabander HF, Vanhaecke L (2010) J Chromatogr A 1217:6616–6622
Torres MA, Barros MP, Campos SCG, Pinto E, Rajamani S, Sayre RT, Colepicolo P (2008) Ecotoxicol Environ Saf 71:1–15
Corcoran J, Winter MJ, Tyler CR (2010) Crit Rev Toxicol 40:287–304
Falandysz J, Taniyasu S, Gulkowska A, Yamashita N, Schukte-Oehlmann U (2006) Environ Sci Technol 40:748–751
Haug LS, Thomson C, Brantsaeter AL, Kvalem HE, Haugen M, Becher G, Alexander J, Meltzer HM, Knutsen HK (2010) Environ Int 36:772–778
The Food and Agriculture Organization of the United Nations (2010) A Regional Survey of the Aquaculture Sector in Eastern and Northwestern Europe. http://www.faoorg/docrep/t7799e/t7799e03htm Accessed 6
Dussault ÈB, Balakrishnan VK, Solomon KR, Sibley PK (2009) Can J Chem 87:662–672
Kwadijk CJAF, Korytár P, Koelmans AA (2010) Environ Sci Technol 44:3746–3751
Bossi R, Strand J, Sortkjaer O, Larsen MM (2008) Environ Int 34:443–450
Schuetze A, Heberer T, Effkemann S, Juergensen S (2010) Chemosphere 78:647–652
Powley CR, George SW, Russell MH, Hoke RA, Buck RC (2008) Chemosphere 70:664–672
Van de Vijver KI, Hoff PT, Van Dongen W, Esmans EL, Blust R, De Coen W (2003) Environ Toxicol Chem 22:2037–2041
Ramirez AJ, Mottaleb MA, Brooks BW, Chambliss CK (2007) Anal Chem 79:3155–3163
Cueva-Mestanza R, Torres-Padrón ME, Sosa-Ferrera Z, Santana-Rodriguez JJ (2008) Biomed Chromatogr 22:1115–1122
Carafa R, Wollgast J, Canuti E, Ligthart J, Dueri S, Hanke G, Eisenreich SJ, Viaroli P, Zaldívar JM (2007) Chemosphere 69:1625–1637
Buyuksonmez F, Sekeroglu S (2005) J Residuals Sci Tech 2:31–40
Jelic A, Petrovic M, Barcelo D (2009) Talanta 80:363–371
Radjenovic J, Jelic A, Petrovic M, Barcelo D (2009) Anal Bioanal Chem 393:1685–1695
Vazquez-Roig P, Segarra R, Blasco C, Andreu V, Picó Y (2010) J Chromatogr A 1217:2471–2483
Verheyden K, Noppe H, Vanden Bussche J, Wille K, Bekaert K, De Boever L, Van Acker J, Janssen CR, De Brabander HF, Vanhaecke L (2010) Anal Bioanal Chem 397:345–355
Balmer ME, Buser H-R, Müller MD, Poiger T (2005) Environ Sci Technol 39:953–962
Buser H-R, Balmer ME, Schmid P, Kohler M (2006) Environ Sci Technol 40:1427–1431
Wen Y, Wang Y, Feng Y-Q (2006) Talanta 70:153–159
Schwaiger J, Ferling H, Mallow U, Wintermayr H, Negele RD (2004) Aquat Toxicol 68:141–150
Stubbings G, Tarbin J, Cooper A, Sharman M, Bigwood T, Robb P (2005) Anal Chim Acta 547:262–268
Pang G-F, Fan C-L, Liu Y-M, Cao Y-Z, Zhang J-J, Fu B-L, Li X-M, Li Z-Y, Wu Y-P (2006) Food Addit Contam 23:777–810
van Leeuwen SPJ, Swart CP, van der Veen I, de Boer J (2009) J Chromatogr A 1216:401–409
Sinclair E, Kannan K (2006) Environ Sci Technol 40:1408–1414
Quiñones O, Snyder SA (2009) Environ Sci Technol 43:9089–9095
Hao C, Clement R, Yang P (2007) Anal Bioanal Chem 387:1247–1257
García-Reyes JF, Hernando MD, Ferrer C, Molina-Díaz A, Fernández-Alba AR (2007) Anal Chem 79:7308–7323
Martins-Júnior HA, Lebre DT, Wang AY, Pires MAF, Bustillos OV (2009) Rapid Commun Mass Spectrom 23:1029–1034
Veyrand B, Sticca P, Pagliuca G, Durand S, Duigou A, Monteau F, Cariou R, Marchand P, Antignac JP, Le Bizec B (2007) Proceeding of the 27th International Symposium on Halogenated Environmental Organic Pollutants and POPs, Tokyo, Japan
Veyrand B, Kadar H, Barbarossa A, Durand S, Marchand P, Antignac JP, Pagliuca G, Le Bizec B (2010) Proceedings of the 29th International Symposium on Halogenated Environmental Organic Pollutants and POPs, San Antonio, Texas, United States
De Voogt P, Sáez M (2006) Trends Analyt Chem 25:326–342
Berger U, Haukas M (2005) J Chromatogr A 1081:210–217
SANCO/10684/2009 (2010) Method validation and quality control procedures for pesticide residues analysis in food and feed. http://www.crl-pesticides.eu/library/docs/allcrl/AqcGuidance_Sanco_2009_10684.pdf Accessed 6 Dec 2010
Commission Decision 2002/657/EC (2002) Off J Eur Commun L221:8–36
Quinete N, Wu Q, Zhang T, Yun SH, Moreira I, Kannan K (2009) Chemosphere 77:863–869
Powley CR, George SW, Ryan TW, Buck RC (2005) Anal Chem 77:6353–6358
Regulation EC 396/2005 (2005) J Eur Union L70:1–16
So MK, Taniyasu S, Lam PK, Zheng GJ, Giesy JP, Yamashita N (2006) Arch Environ Contam Toxicol 50:240–248
Acknowledgments
Mieke Naessens, Dirk Stockx, Lucie Dossche, and Vera Paltousova are greatly acknowledged for their assistance in the lab. This study is part of the INRAM project (http://www.vliz.be/projects/inram) which is funded by The Belgian Federal Science Policy Office (BELSPO). Lynn Vanhaecke is a postdoctoral fellow from the Research Foundation—Flanders (Fonds voor Wetenschappelijk Onderzoek (FWO)-Vlaanderen).
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Wille, K., Kiebooms, J.A.L., Claessens, M. et al. Development of analytical strategies using U-HPLC-MS/MS and LC-ToF-MS for the quantification of micropollutants in marine organisms. Anal Bioanal Chem 400, 1459–1472 (2011). https://doi.org/10.1007/s00216-011-4878-6
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DOI: https://doi.org/10.1007/s00216-011-4878-6