Development and validation of a liquid chromatography isotope dilution mass spectrometry method for the reliable quantificationof alkylphenols in environmental water samples by isotopepattern deconvolution
Fabregat Cabello, Neus; Sancho, Juan V.; Vidal, Andreuet al.
[en] We present here a new measurement method for the rapid extraction and accurate quantification of technical nonylphenol (NP) and 4-t-octylphenol (OP) in complex matrix water samples by UHPLC-ESI-MS/MS. The extraction of both compounds is achieved in 30min by means of hollow fiber liquid phase microextraction (HF-LPME) using 1-octanol as acceptor phase, which provides an enrichment (preconcentration) factor of 800. On the other hand we have developed a quantification method based on isotope dilution mass spectrometry (IDMS) and singly (13)C1-labeled compounds. To this end the minimal labeled (13)C1-4-(3,6-dimethyl-3-heptyl)-phenol and (13)C1-t-octylphenol isomers were synthesized, which coelute with the natural compounds and allows the compensation of the matrix effect. The quantification was carried out by using isotope pattern deconvolution (IPD), which permits to obtain the concentration of both compounds without the need to build any calibration graph, reducing the total analysis time. The combination of both extraction and determination techniques have allowed to validate for the first time a HF-LPME methodology at the required levels by legislation achieving limits of quantification of 0.1ngmL(-1) and recoveries within 97-109%. Due to the low cost of HF-LPME and total time consumption, this methodology is ready for implementation in routine analytical laboratories.
Disciplines :
Chemistry
Author, co-author :
Fabregat Cabello, Neus ; Université de Liège - ULiège > Département de pharmacie > Chimie médicale
Sancho, Juan V.
Vidal, Andreu
Gonzalez, Florenci V.
Roig-Navarro, Antoni F.
Language :
English
Title :
Development and validation of a liquid chromatography isotope dilution mass spectrometry method for the reliable quantificationof alkylphenols in environmental water samples by isotopepattern deconvolution
(2013), Directive 2013/39/EU of the European Parliament and of the Council of 12 August 2013 amending Directives 2000/60/EC and 2008/105/EC as regards priority substances in the field of water policy
Stottmeister, E., Heemken, O.P., Hendel, P., Donnevert, G., Frey, S., Allmendinger, H., Sawal, G., Spilker, R., (2009) Anal. Chem., 81, p. 6765
Gallart-Ayala, E., Moyano, E., Galceran, M.T., (2010) Mass Spectrom. Rev., p. 776
Rabouan, S., Dupuis, A., Cariot, A., Albouy-Llaty, M., Legube, B., Migeot, V., (2012) Trends Anal. Chem., 37, p. 112
Olkowska, E., Polkowska, Z., Namieśnik, J., (2012) Talanta, 88, p. 1
Bello-López, M.Á., Ramos-Payán, M., Ocaña-González, J.A., Fernández-Torres, R., Callejón-Mochón, M., (2012) Anal. Lett., 45, p. 804
Pedersen-Bjergaard, S., Rasmussen, K.E., (2008) J. Chromatogr. A, 1184, p. 132
Villar-Navarro, M., Ramos-Payán, M., Fernández-Torres, R., Callejón-Mochón, M., Bello-López, M.Á., (2013) Sci. Total Environ., 443, p. 1
Salgueiro-González, N., Concha-Graña, E., Turnes-Carou, I., Muniategui-Lorenzo, S., López-Mahía, P., Prada-Rodríguez, D., (2012) J. Chromatogr. A, 1223, p. 1
Fischer, A.R., Lan, N.T.P., Wiedemann, C., Heide, P., Werner, P., Schmidt, A.W., Theumer, G., Knölker, H.-J., (2010) J. Chromatogr. A, 1217, p. 2950
Basheer, C., Lee, H.K., (2004) J. Chromatogr. A, 1057, p. 163
Müller, S., Möder, M., Schrader, S., Popp, P., (2003) J. Chromatogr. A, 985, p. 99
Taylor, P.J., (2005) Clin. Biochem., 38, p. 328
Niessen, W.M.A., Manini, P., Andreoli, R., (2006) Mass Spectrom. Rev., 25, p. 881
Furey, A., Moriarty, M., Bane, V., Kinsella, B., Lehane, M., (2013) Talanta, 115, p. 104
Trufelli, H., Palma, P., Famiglini, G., Cappiello, A., (2011) Mass Spectrom. Rev., 30, p. 491
Vega-Morales, T., Sosa-Ferrera, Z., Santana-Rodríguez, J.J., (2012) J. Chromatogr. A, 1230, p. 66
González-Antuña, A., Rodríguez-González, P., Centineo, G., García Alonso, J.I., (2010) Analyst, 135, p. 953
González-Antuña, A., Rodríguez-González, P., Lavandera, I., Centineo, G., Gotor, V., García Alonso, J.I., (2012) Anal. Bioanal. Chem., 402, p. 1879
González-Antuña, A., Domínguez-Romero, J.C., García-Reyes, J.F., Rodríguez-González, P., Centineo, G., García Alonso, J.I., Molina-Díaz, A., (2013) J. Chromatogr. A, 1288, p. 40
Castillo, A., Gracia-Lor, E., Roig-Navarro, A.F., Sancho, J.V., Rodríguez-González, P., García Alonso, J.I., (2013) Anal. Chim. Acta, 765, p. 77
Fabregat-Cabello, N., Castillo, Á., Sancho, J.V., González, F.V., Roig-Navarro, A.F., (2013) J. Chromatogr. A, 1301, p. 19
Tyman, J.H.P., (1996) Synthetic and Natural Phenols, p. 358. , Elsevier B.V., Amsterdam
Loos, R., Locoro, G., Contini, S., (2010) Water Res., 44, p. 2325
García Alonso, J.I., (1995) Anal. Chim. Acta, 312, p. 57
Salgueiro-González, N., Concha-Graña, E., Turnes-Carou, I., Muniategui-Lorenzo, S., López-Mahía, P., Prada-Rodríguez, D., (2012) Talanta, 101, p. 413
Meija, J., Yang, L., Caruso, J.A., Mester, Z., (2006) J. Anal. At. Spectrom., 21, p. 1294
Rodríguez-González, P., García Alonso, J.I., (2010) J. Anal. At. Spectrom., 25, p. 239
Ramaley, L., Cubero Herrera, L., (2008) Rapid Commun. Mass Spectrom., 22, p. 2707
Ahel, M., Giger, W., (1993) Chemosphere, 26, p. 1471
Saraji, M., Bidgoli, A.A.H., Farajmand, B., (2011) J. Sep. Sci., 34, p. 1708
(2002) Off. J. Eur. Commun., L221, p. 8. , European Union Decision 2002/657/EC, August
(2011) Method validation and quality control procedures for pesticide residues analysis in food and feed, Document No. SANCO/12495/2011, Brussels, , http://ec.europa.eu/food/plant/protection/pesticides/docs/qualcont2012, European Commission, DG-SANCO