Determination of pesticides in waters by capillary gas chromatography with atomic emission detection

Capillary gas chromatography with atomic emission detection (GC-AED) was successfully used to separate and quantify 14 pesticides (organochlorines, organophosphorus compounds and pyrethrins) in water samples after liquid-liquid extraction with ethyl acetate. Monitoring the emission lines for elements such as chlorine, bromine and sulfur ensures nearly specific chromatograms for these elements, and markedly increases selectivity. Calibration curves were obtained by plotting peak area versus concentration and the correlation coefficients relating to linearity were at least 0.999. Each chromatographic separation takes 21 min and, since two injections are necessary, it requires approximately 1 h to analyze one sample. The method shows a precision of 4.3-8.2% (RSD), depending on the compound. The application of liquid-liquid extraction with ethyl acetate led to recoveries from spiked samples ranging from 76 to 113%. The sensitivity and linearity for the elements chlorine, sulfur, nitrogen and phosphorus were checked under the optimized conditions at their customary emission wavelength. The sensitivity and linearity for these compounds decreased in the order (atom and emission wavelength) Cl (479 nm)>S (181 nm)>P (178 nm)>N (174 nm). A study of the GC-AED system's response to chlorine concentration in eight pesticide molecules was performed and a linear relationship was found with a correlation coefficient of 0.987. (C) 2002 Elsevier Science B.V. All rights reserved.