AJAC  Vol.3 No.3 , March 2012
Multiresidue Method for Determination of 67 Pesticides in Water Samples Using Solid-Phase Extraction with Centrifugation and Gas Chromatography-Mass Spectrometry
Abstract: A new multi-residue method based on solid-phase extraction (SPE) with centrifugation was developed for determination and quantitation of 67 pesticides in water samples. Two SPE cartridges were tested: Chromabond C18 and Oasis HLB. Parameters that influence the extraction efficiency such as the eluent volume, the sample loading volume, the addition of organic solvent to water sample, sorbent drying and elute concentration were optimized. The innovation of this work was the examination of the use of a centrifugation technique in both the drying and elution steps. When combined with centrifugation, the volume of the elution solvent was reduced to 2 mL and the time for sorbent drying decreased also to 10 min under vacuum. Under the optimized conditions, this method showed good recoveries higher than 65% - 68% for the 67 analyzed pesticides using the C18 and HLB cartridges with relative standard deviations lower than 9.7% - 12.3%. Limits of quantification were between 2 and 20 ng.L–1. The simplicity of the described method, use of less of organic solvent, short procedure time, and good recoveries demonstrate the advantages of this environmentally friendly approach for routine analysis of numerous samples.
Cite this paper: A. Kouzayha, A. Rahman Rabaa, M. Al Iskandarani, D. Beh, H. Budzinski and F. Jaber, "Multiresidue Method for Determination of 67 Pesticides in Water Samples Using Solid-Phase Extraction with Centrifugation and Gas Chromatography-Mass Spectrometry," American Journal of Analytical Chemistry, Vol. 3 No. 3, 2012, pp. 257-265. doi: 10.4236/ajac.2012.33034.

[1]   T. Reemtsma and M. Jekel, “Organic Pollutants in the Water Cycle, Wiley-VCH VerlagGmBH& Co. KGaA, Weinheim,” Journal of Chromatography A, Vol. 1150, 2006, pp. 267-278.

[2]   J. A. C. Barth, P. Grathwohl and K. C. Jones, “Introduction to special Issue AquaTerra: Pollutant Behavior in the Soil, Sediment, Ground, and Surface Water System,” Environmental Pollution, Vol. 148, No. 3, 2007, p. 693. doi:10.1016/j.envpol.2007.01.043

[3]   H. Bailey, L. Deanovic, E. Reyes, T. Kimball, K. Larson, K. Cortright, V. Conner and D. E. Hinton, “Diazinon and Chlorpyrifos in Urban Waterways in Northern California, USA,” Environmental Toxicology and Chemistry, Vol. 19, No. 1, 2000, p. 82. doi:10.1002/etc.5620190109

[4]   European Union (EU), “Council Directive 98/83/EC of 3 November 1998 on the Quality of Water Intended for Human Consumption,” 1998.

[5]   European Union (EU), “Directive 2000/60/EC of the European Parliament and of the Council Establishing a Frame- work for the Community Action in the Field of Water Policy,” 2000.

[6]   J. J. Vreuls, A. J. H. Louter and U. A. Th. Brinkman, “OnLine Combination of Aqueous-Sample Preparation and Capillary Gas Chromatography,” Journal of Chromatography A, Vol. 856, 1999, pp. 279-314. doi:10.1016/S0021-9673(99)00432-X

[7]   M. E. Baez, M. Rodriguez, O. Lastra and P. Contreras, “Solid-Phase Extraction of Organophosphorus, Triazine, and Triazole-Derived Pesticides from Water Samples. A Critical Study,” Journal of High Resolution Chromatography, Vol. 20, No. 11, 1997, pp. 591-596. doi:10.1002/jhrc.1240201105

[8]   H. Sabik, R. Jeannot and B. Rondeau, “Multiresidue Methods Using Solid-Phase Extraction Techniques for Monitoring Priority Pesticides, Including Tri-azines and Degradation Products, in Ground and Surface Waters,” Journal of Chromatography A, Vol. 885, No. 1-2, 2000, pp. 217-236. doi:10.1016/S0021-9673(99)01084-5

[9]   M. J. M. Wells and L. Z. Yu, “Solid-Phase Extraction of Acidic Her-bicides,” Journal of Chromatography A, Vol. 885, No. 1-2, 2000, pp. 237-250. doi:10.1016/S0021-9673(00)00206-5

[10]   A. Kouzayha, M. Al Iskandarani, S. Mokh, A. R. Rabaa, H. Budzinski and F. Jaber, “Optimization of a Solid-Phase Extraction Method Using Centrifugation for the Determination of 16 Polycyclic Aromatic Hydrocarbons in Water,” Journal of Agricultural and Food Chemistry, Vol. 59, No. 14, 2011, pp. 7592-7600. doi:10.1021/jf200123v

[11]   M. Asi, A. Hussain and S. Muh-mood, “Solid Phase Extraction of Pesticide Residues in Water Samples: Ddt and Its Metabolites,” International Journal of Environmental Research, Vol. 2, No. 1, 2008, pp. 43-48.

[12]   E. Concha-Grana, M. Turnes-Carou, S. Muniategui-Lorenzo, P. Lopez-Mahia, D. Prada-Rodriguez and D. Fernandez-Fernandez, “Evaluation of HCH Isomers And Metabolites in Soils, Leachates, River Water and Sedi- ments of a Highly Contaminated Area,” Chemosphere, Vol. 64, 2006, p. 588. doi:10.1016/j.chemosphere.2005.11.011

[13]   C. De la Colina, A. P. Heras, G. D. Cancela and F. San- chez Rasero, “Determination of Organophosphorus and Nitrogen-Containing Pesticides in Water By Solid-Phase Extraction with Gas Chromatography with Nitrogen— Phosphorus Detection,” Journal of Chromatography A, Vol. 655, No. 1, 1993, pp. 127-132. doi:10.1016/0021-9673(93)87020-M

[14]   United States Environmental Protection Agency (US-EPA), “Method 525: Determination of Organic Compounds in Drinking-Water by Liquid—Solid Extraction and GC-MS”.

[15]   M. Forcada, J. Bel-tran, F. J. Lopez and F. Hernandez, “Multiresidue Procedures for Determination of Triazine and Organophosphorus Pesticides in Water by Use of Large-Volume PTV Injection in Gas Chromatography,” Chromatographia, Vol. 51, No. 5-6, 2000, pp. 362- 368. doi:10.1007/BF02490618

[16]   Waters Corporation, “Organo-phosphorus Pesticides in Drinking Water and Fruit. Environmental and Agro- chemical Applications Notebook,” 2002, p. 9.

[17]   M. Tahara, R. Kubota, H. Nakazawa, H. Tokunaga and T. Nishimura, “Analysis of Active Oxon Forms of Nine Organophosphorus Pesticides in Water Samples Using Gas Chromatography with Mass Spectrometric Detection,” Journal of Health Science, Vol. 52, 2006, pp. 313-319. doi:10.1248/jhs.52.313

[18]   A. M. Rodrigues, V. Ferreira, V. V. Cardoso, E. Ferreira and M. J. Benoliel, “Determination of Several Pesticides in Water by Solid-Phase Extraction, Liquid Chromatography and Electrospray Tandem Mass Spectrometry,” Journal of Chromatography A, Vol. 1150, No. 1-2, 2007, pp. 267-278. doi:10.1016/j.chroma.2006.09.083

[19]   M. C. Hennion, C. Cau-Dit-Coumes and V. Pichon, “Trace Analysis of Polar Organic Pollutants in Aqueous samples. Tools for the Rapid Prediction and Optimization of the Solid-Phase Extraction Parameters,” Journal of Chromatography. A, Vol. 823, No. 1-2, 1998, pp. 147- 161. doi:10.1016/S0021-9673(98)00479-8

[20]   M. C. Hennion, “Solid-Phase Extraction: Method Development, Sorbents, and Coupling with Liquid Chromatography,” Journal of Chromatography A, Vol. 856, No. 1-2, 1999, pp. 3-54. doi:10.1016/S0021-9673(99)00832-8

[21]   V. Pichon, “Solid-Phase Extraction for Multiresidue Analysis of Organic Contaminants in Water,” Journal of Chro- matography A, Vol. 885, No. 1-2, 2000, pp. 195-215. doi:10.1016/S0021-9673(00)00456-8

[22]   United States Environmental Protection Agency (US- EPA), “Metalaxyl. Prevention, Pesticides and Toxic Substances (7508W) EPA-738-F-94-013,” 1994.