A new method to determine pesticide residue in water is presented. The described method includes using off-line solid-phase extraction (SPE) and on-line reversed-phase liquid chromatography-gas chromatography (RPLC-GC). An interface, based on a modified programmed temperature vaporizer (PTV) injector, packed with a suitable trapping material, is used for on-line RPLC-GC. The changes made in the PTV injector affect the pneumatic system, sample introduction, and solvent elimination. The new interface is easily capable of automation. Methanol/wate (70/30) is used as the eluent in the LC preseparation step. The LC column flow during elution is different from the flow during the transfer step. The transferred volumes range from 500 to 1400 microL (volume of the fractions of interest). Solvent elimination is almost 100% before the sample reaches the GC column. The described system does not show any variation of the peak retention times. The detection limit for real samples ranges from 0.04 to 1.5 ng/L, using NP detection.
The Through Oven Transfer Adsorption Desorption (TOTAD) interface is used to directly introduce large volumes of water (1 mL or more) into a capillary gas chromatograph. The TOTAD interface is a greatly modified programmed temperature vaporizer injector incorporating changes that affect the pneumatics, sample introduction, solvent elimination, and operation mode. The system can easily be automated. The technique is applied to the analysis of pesticide residue in standard solutions and real water samples from the Ebro River (northeastern Spain). The speed of sample introduction was 1 mL/min, and the solvent elimination was almost complete. A nitrogen phosphorous detector is used, and the relative standard deviation varied from 5.7% to 11.7% for the absolute peak areas. The sensitivity achieved by introducing 1 mL of the sample is sufficient for most pesticide-residue analyses in water. The limits of detection ranged from 0.5 to 8.1 ng/L.
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