Factorial design optimization of experimental variables in preconcentration of carbamates pesticides in water samples using solid phase extraction and liquid chromatography–electrospray-mass spectrometry determination

Abstract

An experimental design was applied for the optimization of extraction process of carbamates pesticides from surface water samples. Solid phase extraction (SPE) of carbamates compounds and their determination by liquid chromatography coupled to electrospray mass spectrometry detector were considered. A two level full factorial design 2(k) was used for selecting the variables which affected the extraction procedure. Eluent and sample volumes were statistically the most significant parameters. These significant variables were optimized using Doehlert matrix. The developed SPE method included 200mg of C-18 sorbent, 143.5 mL of water sample and 5.5 mL of acetonitrile in the elution step. For validation of the technique, accuracy, precision, detection and quantification limits, linearity, sensibility and selectivity were evaluated. Extraction recovery percentages of all the carbamates were above 90% with relative standard deviations (R.S.D.) in the range of 3-11%. The extraction method was selective and the detection and quantification limits were between 0.1 and 0.5 µg L(-1), and 1 and 3 µg L(-1), respectively.