Novel, fast, selective, eco-friendly and reproducible solid-phase membrane tip extraction and gas chromatography with mass spectrometry methods were developed and validated for the analysis of triazine herbicides (atrazine and secbumeton) in stream and lake waters. The retention times of atrazine and secbumeton were 7.48 and 8.51 min. The solid-phase membrane tip extraction was carried out in semiautomated dynamic mode on multiwall carbon nanotubes enclosed in a cone-shaped polypropylene membrane cartridge. Acetone and methanol were found as the best preconditioning and desorption solvents, respectively. The extraction and desorption times for these herbicides were 15.0 and 10.0 min, respectively. The percentage recoveries of atrazine and secbumeton were 88.0 and 99.0%. The linearity range was 0.50-80.0 μg/L (r(2) > 0.994), with detection limits (<0.47 μg/L, S/N = 3) and good reproducibility (<8.0%). The ease of operation, eco-friendly nature, and low cost of solid-phase membrane tip extraction made these methods novel. The Solid-phase membrane tip extraction method was optimized by considering the effect of extraction time, desorbing solvents and time.
Keywords: Gas chromatography with mass spectrometry; Multiwalled carbon nanotubes; Solid-phase membrane tip extraction; Triazine herbicides.
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