Automated in-tube solid-phase microextraction–high-performance liquid chromatography for carbamate pesticide analysis

Abstract

In-tube solid-phase microextraction (SPME) is an automated version of SPME that can be easily coupled to a conventional HPLC autosampler for on-line sample preparation, separation and quantitation. It has been termed “in-tube” SPME because the extraction phase is coated inside a section of fused-silica tubing rather than coated on the surface of a fused-silica rod as in the conventional syringe-like SPME device. The new in-tube SPME technique has been demonstrated as a very efficient extraction method for the analysis of polar and thermally labile analytes. The in-tube SPME–HPLC method used with the FAMOS autosampler from LC Packings was developed for detecting polar carbamate pesticides in clean water samples. The main parameters relating to the extraction and desorption processes of in-tube SPME (selection of coatings, aspirate/dispense steps, selection of the desorption solvents, and the efficiency of desorption solvent, etc.) were investigated. The method was evaluated according to the reproducibility, linear range and limit of detection. This method is simple, effective, reproducible and sensitive. The relative standard deviation for all the carbamates investigated was between 1.7 and 5.3%. The method showed good linearity between 5 and 10 000 μg/l with correlation coefficients between 0.9824 and 0.9995. For the carbamates studied, the limits of detection observed are lower than or similar to that of US Environmental Protection Agency or National Pesticide Survey methods. Detection of carbaryl present in clean water samples at 1 μg/l is possible.