http://dx.doi.org/10.4322/sc.2014.025

 

SPME-GC-MS determination of selected aniline pesticides in surface water

Muhlen, Carin Von; Lanças, Fernando M.

Palavras-chave: water, anilines, pesticides, SPME, GC-MS, herbicides.

Resumo: An analytical methodology to determine Alachlor, Butralin, and Metolachlor herbicides, and Metalaxyl fungicide, in surface water was developed using Solid Phase Microextraction (SPME) and Gas Chromatography coupled to Mass Spectrometry (GC-MS). The developed method was validated, and the quantification limits were found to be between 0.2 to 1.8 μg.L-1, depending upon the compound. The precision, as measured by the relative standard deviations (RSD), was in the range 3.5% to 27%. The higher RSD was found for Butralin due to the occurrence of adsorption of this compound in the extraction fiber. After validation the developed methodology was employed to the determination of these four pesticides in water samples that supplies Araraquara and São Carlos cities (São Paulo – Brazil). Samples from Feijão Creek, Anhumas Creek, Cruzes Creek and Paiol Brook, as well as samples from after-treatment at SAAE (Water and Sewer Supply Service – São Carlos, SP, Brazil) and DAAE (Water and Sewer Supply Department – Araraquara, SP, Brazil) were evaluated. Samples from both winter and summer seasons were collected and analysed. The results show that the samples analyzed using the in-house validated methodology were not contaminated with these pesticides within the investigated concentrations.


Referências Bibliográficas

1. E. F. G. C. Dores and E.M. De-Lamonica-Freire. Aquatic environment contamination by pesticides. Case study: Water used for human consumption in Primavera do Leste, Mato Grosso – Preliminary analyses. Quim. Nova 24: (1), 27-36 (2001).
2. R. Soniassy, P. Sandra, and C. Schlett. Water Analysis: Organic Micropolutants, Hewlett Packard, Germany (1994).
3. Chem Service Pesticide and Metabolite Standards Catalog PS 2001-2004.
4. CONAMA Resolution 357, Publicação DOU nº 053, de 18/03/2005, págs. 58-63.
5. G. S. Rodrigues, L. C. Paraíba and C. C. Buschinelli. Pesticides: Ecotoxicologycal and Environmental Journal (Pesticidas: Revista de Ecotoxicologia e Meio ambiente), CEPPA, Curitiba-PR, 7: 89-108 (1997).
6. C. Sanchezbrunete, L. Martínez and J. L. Tadeo. Determination of Corn Herbicides by GC-MS and GC-NPD in Environmental-Samples. Agr. Food Chem. 42: 2210-2214 (1994).
7. Yasmine Souissi, Stéphane Bouchonnet, Sophie Bourcier, Kresten Ole Kusk, Michel Sablier, Henrik Rasmus Andersen. Identification and ecotoxicity of degradation products of chloroacetamide herbicides from UV-treatment of water. Science of The Total Environment, Volumes 458–460, 1 August 2013, Pages 527-534.
8. An Ghekiere, Frederik Verdonck, Michiel Claessens, Els Monteyne, Patrick Roose, Klaas Wille, Annelies Goffin, Karen Rappé, Colin R. Janssen. Monitoring micropollutants in marine waters, can quality standards be met? Marine Pollution Bulletin, Volume 69, Issues 1–2, 15 April 2013, Pages 243-250
9. Beatriz Jurado-Sánchez, Evaristo Ballesteros, Mercedes Gallego. Comparison of microwave assisted, ultrasonic assisted and Soxhlet extractions of N-nitrosamines and aromatic amines in sewage sludge, soils and sediments. Science of The Total Environment, Volumes 463-464, 1 October 2013, Pages 293-301.
10. Lei Zhang, Fang Han, Yanyun Hu, Ping Zheng, Xuan Sheng, Hao Sun, Wei Song, Yaning Lv. Selective trace analysis of chloroacetamide herbicides in food samples using dummy molecularly imprinted solid phase extraction based on chemometrics and quantum chemistry. Analytica Chimica Acta, Volume 729, 4 June 2012, Pages 36-44
11. Maciej Tankiewicz, Calum Morrison, Marek Biziuk. Multi-residue method for the determination of 16 recently used pesticides from various chemical groups in aqueous samples by using DI-SPME coupled with GC–MS. Talanta, Volume 107, 30 March 2013, Pages 1-10
12. R.W. Barrinuevo and F.M. Lancas. Comparison of liquid-liquid extraction (LLE), solid-phase extraction (SPE), and solid-phase microextraction (SPME) for pyrethroid pesticides analysis from enriched river water. B. Environ. Contam. Tox. 69: 123-128 (2002).
13. M.E.C. Queiroz, S.M. Silva, D. Carvalho and F.M. Lancas. Comparison between solid-phase extraction methods for the chromatographic determination of organophosphorus pesticides in water. J. Environ. Sci. Heal. B 36: 517-527 (2001).
14. Rocío Inés Bonansea, María Valeria Amé, Daniel Alberto Wunderlin. Determination of priority pesticides in water samples combining SPE and SPME coupled to GC–MS. A case study: Suquía River basin. Chemosphere, Volume 90, Issue 6, February 2013, Pages 1860-1869.
15. L. Pan, J. M. Chong and J. B. Pawliszyn. Determination of Amines in air and water using derivatization combined with solid-phase microextraction. J. Chromatogr. A 773: 249-260 (1997).
16. R. Doong, S.Chang and Y. Sun. Solid phase microextraction for determining the distribution of sixteen US Environmental Protection Agency polycyclic aromatic hydrocarbons in water samples. J. Chromatogr. A 879: (2), 177-188 (2000).
17. E. Baltussen, P. Sandra, F. David and C. Cramers. Stir bar sorptive extraction (SBSE), a novel extraction technique for aqueous samples: Theory and principles. J. Microcolumn Sep. 11: 737-747 (1999).