Abstract
In this work, the simultaneous separation of a group of 12 pesticides (carbaryl, fensulfothion, mecoprop, fenamiphos, haloxyfop, diclofop, fipronil, profenofos, fonofos, disulfoton, nitrofen, and terbufos) by nano-liquid chromatography with UV detection is described. For the analyses, a 100 μm internal diameter capillary column packed with silica modified with phenyl groups was used. Experimental parameters, including the use of a trapping column for increasing the sensitivity, were optimized and validated. A preliminary study of the applicability of a rapid and practical dispersive solid-phase extraction (DSPE) procedure was developed for the extraction of some of these pesticides (carbaryl, fensulfothion, fenamiphos, fipronil, profenofos, fonofos, disulfoton, nitrofen, and terbufos) from Milli-Q water samples using multi-walled carbon nanotubes (MWCNTs). The method was validated through a recovery study at three different levels of concentration, obtaining limits of detection in the range 0.016–0.067 μg/L (below European Union maximum residue limits) for the majority of the pesticides. In this work, MWCNTs were reused up to five times, representing an important reduction of the waste of stationary phase. Furthermore, DSPE permitted a clear diminution of the total sample treatment time with respect to conventional SPE.
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References
Ríos A, Escarpa A, Simonet B (2009) Miniaturization of analytical systems. Principles, designs and applications, Wiley
Karlsson KE, Novotny M (1988) Anal Chem 60:1662–1665
Hernández-Borges J, Aturki Z, Rocco A, Fanali S (2007) J Sep Sci 30:1589–1610
Tao D, Zhang L, Shan Y, Liang Z (2011) Anal Bioanal Chem 399:229–241
Iijima S (1991) Nature 354:56–58
Trojanowicz M (2006) Trends Anal Chem 25:480–489
Valcárcel M, Cárdenas S, Simonet BM (2007) Anal Chem 79:4788–4797
Ravelo-Pérez LM, Herrera-Herrera AV, Hernández-Borges J, Rodríguez-Delgado MA (2010) J Chromatogr A 1217:2618–2641
Pyrzynska K (2010) Trends Anal Chem 29:718–727
Asensio-Ramos M, Hernández-Borges J, Ravelo-Pérez LM, Rodríguez-Delgado MA (2008) Electrophoresis 29:4412–4421
Asensio-Ramos M, Hernández-Borges J, Borges-Miquel TM, Rodríguez-Delgado MA (2009) Anal Chim Acta 647:167–176
Ravelo-Pérez LM, Hernández-Borges J, Rodríguez-Delgado MA (2008) J Sep Sci 31:3612–3619
Tsai W-H, Huang T-C, Huang J-J, Hsue Y-H, Chuang H-Y (2009) J Chromatogr A 1216:2263–2269
Lu Q, Chen X, Nie L, Jiang H, Chen L, Hu Q, Du S, Zhang Z (2010) Talanta 81:959–966
Peng Y, Xie Y, Luo J, Nie L, Chen Y, Chen L, Du S, Zhang Z (2010) Anal Chim Acta 674:190–200
Fanali S, Aturki Z, D’Orazio G, Rocco A (2007) J Chromatogr A 1150:252–258
Buonasera K, D’Orazio G, Fanali S, Dugo P, Mondello L (2009) J Chromatogr A 1216:3970–3976
D’Ascenzo G, Gentili A, Marchese S, Perret D (1998) J Chromatogr A 813:285–297
Curini R, Gentili A, Marchese S, Marino A, Perret D (2000) J Chromatogr A 874:187–198
D’Orazio G, Fanali S (2009) J Sep Sci 31:2567–2571
Rosales-Conrado N, León-González ME, Pérez-Arribas LV, Polo-Díez LM (2005) J Chromatogr A 1076:202–206
Tegeler T, El Rassi Z (2001) Anal Chem 73:3365–3372
Ravelo-Pérez LM, Hernández-Borges J, Rodríguez-Delgado MA (2008) J Chromatogr A 1211:33–42
Basheer C, Alnedhary AA, Rao BSM, Valliyaveettil S, Lee HK (2006) Anal Chem 78:2853–2858
Laganà A, Fago G, Marino A (1998) J Chromatogr A 796:309–318
Biesaga M, Pyrzynska K (2006) J Sep Sci 29:2241–2244
Zhou Q, Ding Y, Xiao J (2007) Chromatographia 65:25–30
Liang P, Liu Y, Zeng J, Lu H (2004) J Anal At Spectrom 10:1489–1492
Liang P, Liu Y, Guo L (2005) Spectrochim Acta B 60:125–129
Liang P, Zhao E, Ding Q, Du D (2008) Spectrochim Acta B 63:714–717
Wu H, Wang X, Liu B, Liu Y, Li S, Lu J, Tian J, Zhao W, Yang Z (2011) Spectrochim Acta B 66:74–80
López-Feria S, Cárdenas S, Valcárcel M (2009) J Chromatogr A 1216:7346–7350
Basheer C, Alnedhary AA, Rao BSM, Lee HK (2009) J Chromatogr A 1216:211–216
Acknowledgments
M.A.R. wishes to thank the Spanish Ministry of Education for the FPU grant. J.H.B. wishes to thank the Spanish Ministry of Science and Innovation for the Ramón y Cajal contract at the University of La Laguna. M.A.R. would also like to thank Dr. S. Fanali for his helpful suggestions, as well as Dr. Z. Aturki for her help and support during the stay at the Institute of Chemical Methodologies of the CNR. Authors acknowledge Dr. M.A. Rodríguez-Delgado for his valuable comments and suggestions. This work has been supported by the Spanish Ministry of Science and Innovation (project AGL2009-07884/ALI).
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Asensio-Ramos, M., D’Orazio, G., Hernandez-Borges, J. et al. Multi-walled carbon nanotubes–dispersive solid-phase extraction combined with nano-liquid chromatography for the analysis of pesticides in water samples. Anal Bioanal Chem 400, 1113–1123 (2011). https://doi.org/10.1007/s00216-011-4885-7
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DOI: https://doi.org/10.1007/s00216-011-4885-7