Optimization and validation of a SPME-GC-ECD methodology for the determination of organochlorine pesticides in natural spring waters from Portugal

• Autorzy: Cardoso, A.S. , Feliciano, S.A. , Rebelo, M.H.

Warianty tytułu

PL

Optymalizacja i walidacja metody SPME-GC-ECD do wykrywania pestycydów chloroorganicznych w naturalnych wodach źródlanych Portugalii

• Języki publikacji: EN

Abstrakty

EN

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.

PL

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.

Słowa kluczowe

PL

pestycydy chloroorganiczne; wody źródlane; metodologia SPME-GC-ECD; walidacja

EN

organochlorine pesticides; spring waters; SPME-GC-ECD methodology; validation

• Czasopismo: Ecological Chemistry and Engineering. S
• Rocznik: 2009
• Tom: Vol. 16, nr 2
• Strony: 137-153
• Opis fizyczny: Bibliogr. 36 poz., rys., tab.

Twórcy

autor

Cardoso, A.S.

autor

Feliciano, S.A.

autor

Rebelo, M.H.

• Chemistry and Toxicology Laboratory, Water and Soil Unit, Environmental Health Department, National Health Institute Dr. Ricardo Jorge, Av. Padre Cruz 1649-016 Lisbon, Portugal,

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