Determination of organochlorine pesticides in leather by solid-phase microextraction and gas chromatography-mass spectrometry

Silveira, Cristine Durante de Souza; Carasek, Eduardo

Palavras-chave: organochlorine pesticides, HS-SPME, GC-MS, leather.

Resumo: An analytical procedure based on the solid-phase microextraction technique (SPME) combined with gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS) for the determination of organochlorine pesticides (OCPs) extracted directly from leather samples is proposed. The extraction conditions for the headspace SPME (HS-SPME) procedure were optimized using experimental designs. The fibers and the ionic strength were optimized by the univariate procedure, while a Doehlert matrix was used to optimize the extraction time and temperature. The best extraction conditions were obtained using a PDMS/DVB fiber with extraction time and temperature of 35 min and 80 oC, respectively. No salt addition was necessary. Detection limits ranging from 3.3 to 11 ng g -1 and relative standard deviations (RSD, n = 5) lower than 14.2% were obtained. The recovery was studied at three concentration levels by adding different amounts of organochlorine pesticides to the leather samples (600, 900 and 1500 ng g -1 ) and excellent recoveries ranging from 93.7 to 107.3% were obtained.

Referências Bibliográficas

1. J.W.F. Pacheco, Curtumes. São Paulo: CETESB, 2005. Available at
2. R.P.B.Câmara, E.V. Gonçalves Filho, XIII SIMPEP, Bauro, SP, Brazil, November 6 to 8, 2006.
3. J. Font, A. Marsal, J. Chromatogr. A, 811, 256-260 (1998).
4. K.C. Jones, P. De Voogt, Environ. Pollution, 100, 209-221 (1999).
5. W.F. Tordoir, N.J. Van Sittert, Toxicology, 91, 51-57 (1994).
6. S.H. Safe, Eur. J. Lipid Sci. Tech., 102, 52-53 (2000).
7. C.D. de Souza Silveira, E. Martendal, V. Soldi, E. Carasek, J. Sep. Sc., 35, 602-607 (2012).
8. C. Dong, Z. Zeng, M. Yang, Water Res., 39, 4204-4210 (2005).
9. C.B. Prates, S.S. Gebara, N. Ré-Poppi, N., Química Nova, 37, 1260-1264 (2011).
10. J. Pawliszyn, Applications of Solid Phase Microextraction. Royal Society of Chemistry, Ontário (1999).
11. J. Pawliszyn, Handbook of Solid Phase Microextraction. Chemical Industry Press, Canada (2009).