Czasopismo
2009
|
Vol. 16, nr 2
|
137-153
Tytuł artykułu
Autorzy
Wybrane pełne teksty z tego czasopisma
Warianty tytułu
Optymalizacja i walidacja metody SPME-GC-ECD do wykrywania pestycydów chloroorganicznych w naturalnych wodach źródlanych Portugalii
Języki publikacji
Abstrakty
A simple and reliable methodology for the quantification of eight known organochlorine pesticides and metabolites, using a solid-phase microextraction technique (SPME) followed by gas chromatographic analysis with electron capture detection (GC-ECD) is described herein. Several parameters are studied for the SPME procedure, using two different fibres coatings (polydimethylsiloxane and polyacrylate) and the extraction efficiency is discussed using statistic tests and considering the properties of the extracted compounds, salt concentration of the water solution and the structure of the fibre coating. After selecting the best extraction conditions, the method performance is tested in terms of linearity, limits of detection and quantification, trueness, repeatability and intermediate precision, following the recommendations of the international standard ISO/IEC 17025. The method shows good linearity for the tested concentration range, with coefficients of estimation ranging from 0.9931 to 0.9984. Limits of detection from 6.1 to 10.3 ngldm3 are obtained. Analytical recoveries, repeatability and intermediate precision are calculated in ultra-pure, bottled and lap water, with recoveries values ranging from 75.3 to 117.0%, repeatability of relative standard deviation (RSD) values from 6.4 to 17.0% and precision RSD values from 7.8 to 20.8%. The methodology is then successfully applied to fifty natural spring waters from Sintra and Odivelas municipalities in Portugal.
Opisano prostą i wiarygodną metodę ilościowego oznaczania 8 powszechnie używanych pestycydów chloroorganicznych i ich metabolitów. Do analizy stosowano technikę mikroekstrakcji do fazy stacjonarnej (SPME), a następnie chromatografii gazowej z detektorem wychwytu elektronów (GC-ECD). Metodą SPME było badanych kilka parametrów z użyciem dwóch różnych włókien (polidimetylosiloksanu i poliakrylanu). Wydajność ekstrakcji badano za pomocą testów statystycznych i biorąc pod uwagę właściwości ekstrahowanych substancji, stężenie soli w badanych roztworach wodnych i strukturę powierzchni włókien. Po wybraniu najlepszych warunków ekstrakcji omawiana metoda była sprawdzana zgodnie z zaleceniami normy międzynarodowej ISO/IEC 17025. Przedstawiana procedura była z sukcesem wykorzystana do analizy 50 wód źródlanych z 15 miejscowości powiatów Sintra i Odivelas w Portugalii.
Czasopismo
Rocznik
Tom
Strony
137-153
Opis fizyczny
Bibliogr. 36 poz., rys., tab.
Twórcy
autor
autor
autor
- Chemistry and Toxicology Laboratory, Water and Soil Unit, Environmental Health Department, National Health Institute Dr. Ricardo Jorge, Av. Padre Cruz 1649-016 Lisbon, Portugal, ana.s.cardoso@insa.min-saude.pt
Bibliografia
- [1] Carreño J., Rivas A., Granada A., Lopez-Espinosa M.J., Mariscal M., Olea N. and 0lea-Serrano F.: Exposure of young men to organochlorine pesticides in southern Spain. Environ. Res., 2007, 103, 55-61.
- [2] Bretveld R.W., Thomas C.M.G., Scheepers P.T.J., Zielhuis G.A. and Roeleveld N.: Pesticide exposure: the hormonal function of the female reproductive system disrupted? Reprod. Biol. Endocrinol., 2006, 4, 30-43.
- [3] Garcia A.M.: Pesticide exposure and women 's health. Am. J. Ind. Med., 2003, 44, 584-594.
- [4] Lemaire G., Mnif W., Mauvais P., Balaguer P. and Rahmani R.: Activation of a-estrogen and p-estrogen receptors by persistent pesticides in reporter cell lines. Life Sci., 2006, 79, 1160-1169.
- [5] Hayes T.B., Case P., Chui S., Chung D., Haeffele C., Haston K., Lee M., Mai V.P., MaIjuoa Y., Parker J. and Tsui M.: Pesticides mixtures, endocrine disruption, and amphibian declines: Are we underestimating the impact? Environ. Health Persp., 2006,114(11),40-50.
- [6] Waliszewski S.M., Bermudez M.T., Infanzon R.M., Silva C.S., Carvajal O., Trujillo P., Arroyo S.G., Pietrine R.V., Saldaña V.A, Melo G., Esquivel S., Castro F., Ocampo H., Torres J. and Hayward-Jones P.M.: Persistent organochlorine pesticide levels in breast adipose tissue in women with malignant and benign breast tumors. B. Environ. Contam. Tox., 2005, 75, 752-759.
- [7] De Roos A.J., Hartge P., Lubin J.H., Colt J.S., Davis S., Cerhan J.R, Severson R.K., Cozen W., Patterson D.G. Jr., Needham L.L. and Rothman N.: Persistent organochlorine chemicals in plasma and risk of non-Hodgkin's lymphoma. Cancer Res., 2005, 65(23), 11214-11226.
- [8] Wolff M.S., Britton J.A, Teitelbaum S.L., Eng S., Deych E., Ireland K., Liu Z., Neugut AJ., Santella R.M. and Gammon M.D.: Improving organochlorine biomarker models for cancer research. Cancer Epidem. Biomar., 2005, 14(9), 2224-2236.
- [9] Purdue M., Hoppin J.A, Blair A., Dosemeci M. and Alavanja M.C.R: Occupational exposure to organochlorine insecticides and cancer incidence in the agricultural health study. Int. J. Cancer., 2006, 120, 642-649.
- [10] Graham K.N., Sarma L.P., Webster G.RB., Gaynor J.D. and Ng H.Y.F.: Solid-phase microextraction of the herbicide metolachlor in runoff and tile-drainage water samples. J. Chromatogr. A, 1996, 725, 129-136.
- [11] Eaton A.D., Clesceri L.S. and Greenberg AE.: Standard methods for the examination of water and wastewater, 21st Edition. APHA, AWWA, WEF, Washington OC, 2005, 6,100-115.
- [12] Scheyer A., Briand O., Morville S., Philippe M. and Millet M.: Analysis of trace levels of pesticides in rainwater by SPME and GC-tandem mass spectrometry after derivatisation with PFFBr. Anal. Bioanal. Chem., 2006, 367, 359-368.
- [13] Beceiro-González E., Concha-Graña E., Guimaraes A, Gonçalves C, Muniategui-Lorenzo S. and Alpendurada M.E: Optimization and validation of a solid-phase microextraction method for simultaneous determination of different types of pesticides in water by gas chromatography-mass spectrometry. J. Chromatogr. A, 2007, 1141, 165-173.
- [14] Campillo N., Peñalver R. and Hernández-Córdoba M.: Pesticides analysis in herbal in fusions by solid-phase microextraction and gas chromatography with atomic emission detection. Talanta, 2007, 71, 14177-1423.
- [15] Dong C., Zeng Z. and Yang. M.: Determination of organochlorine pesticides and their derivations in water after HS-SPME using polymethyl-phenyvinylsiloxane-coated fibre by GC-ECD. Water Res., 2005, 39, 4204-4210.
- [16] Gonçalves C. and Alpendurada M.F.: Comparison of three different poly(dimethylsiloxane)-divinylbenzene fibres for the analysis of pesticide multiresidues in water samples: structure and efficiency. J. Chromatogr. A, 2002, 963, 19-26.
- [17] Brás I., Santos L. and Alves A: Monitoring organochlorine pesticides from landfill leachates by gas chromatography-electron-capture detection after solid-phase microextraction. J. Chromatogr. A, 2000, 891, 305-311.
- [18] Beltran J., López FJ. and Hemández E: Solid-phase microextraction in pesticide residue analysis. J. Chromatogr. A, 2000, 885, 389-404.
- [19] Hemández F., Beltran J., Lopez F.J. and Gaspar J.V.: Use of solid-phase microextration for the quantitative determination of herbicides in soil and water samples. Anal. Chem., 2000, 72, 2313-2322.
- [20] Aguilar C., Peñalver A., Pocurull E., Ferre J., Borrul F. and Marce R.M.: Optimization of solid-phase microextraction conditions using a response methodology to determine organochlorine pesticides in water by gas chromatography and electron-capture detection. J. Chromatogr. A, 1999, 844, 425-432.
- [21] Battle R., Sánchez C. and Neŕin C.: Determination of pesticides in ethanol/water mixtures used as food simulants. Anal. Chem., 1999, 71, 2417-2422.
- [22] Berladi R.P. and Pawliszyn J.: The application of chemically modified fused silica fibers in the extraction of organics from water matrix samples and their rapid transfer to capillary columns. Water Pollut. Res. J. Can., 1989, 24, 179-191.
- [23] Raposo Júnior J.L. and Ré-Poppi N:: Determination of organochlorine pesticides in ground water samples using solid-phase microextraction by gas chromatography-electron capture detection. Talanta, 2007, 72, 1833-1841
- [24] Pérez-Trujillo J.P., Frías S., Conde J.E. and Rodriguez-Delgado M.A: Comparison of different coatings in solid-phase microextraction for the determination of organochlorine pesticides in ground water. J. Chromatogr. A, 2002, 963, 95-105.
- [25] Boussahel R., Bouland S., Moussaoui K.M., Baudu M. and Montiel A: Determination of chlorinated pesticides in water by SPME/GC. Water Res., 2002, 36, 1909-1911.
- [26] Tomkins B.A. and Bamard A.R.: Determination of organochlorine pesticides in groun water using a solid-phase microextraction followed by dual-column gas chromatography with electron-capture detection. J. Chromatogr. A, 2002, 964, 21-33.
- [27] Aguilar C., Penalver S., Pocurull E., Borrul F., Marçé R.M..: Solid-phase microextraction and gas chromatography with mass spectrometric detection for the determination of pesticides in aqueous samples. J. Chromatogr. A, 1998, 795, 105-115.
- [28] Magdic S. and Pawliszyn J.B.: Analysis of organochlorine pesticides using solid-phase microextration. J. Chromatogr. A, 1996,723, 111-122.
- [29] Boyd-Boland A.A., Magdic S. and Pawliszyn J.B.: Simultaneous Determination of 60 Pesticides in Water Using Solid-phase Microextraction and Gas Chromatography-Mass Spectrometry. Analyst, 1996, 121, 929-938.
- [30] Ekmekci M.: Pesticide and nutrient contamination in the kestel polje-kirkgoz karst springs, Southern Turkey. Environ. 0001., 2005, 49(1), 19-29.
- [31] Karasali H., Hourdakis A., Anagnostopoulos H. and Doulia D.: Pesticides residues in thermal mineral water in Greece. J. Environ. Sci. Health B, B37(5), 465-474.
- [32] Dugay J., Miège C. and Hennion M.-C.: Effect of the various parameters governing solid-phase microextraction for the trace-determination of pesticides in water. J. Chromatogr. A, 1998, 795, 27-42.
- [33] LaGrega M.D., Buckingham P.L. and Evans J.C.: Hazardous Waste Management, 2nd Edition. McGraw-Hill Higher Education, New York 2001.
- [34] Louch D., Motlagh S. and Pawliszyn J.: Dynamics of organic compound extraction from water using liquid-coated fused silica fibers. Anal. Chem., 1992, 64(10), 1187-1199.
- [35] Validação de Métodos Internos de Ensaio em Anáilise Química. Guia Relacre 13, Relacre, 2000.
- [36] IUPAC. Harmonized Guidelines for internal quality control in analytical chemistry laboratories. Pure Appl. Chero., 1995, 67(4), 649-666.
Typ dokumentu
Bibliografia
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Identyfikator YADDA
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