Magnetic nanocellulose hybrid nanoparticles and ionic liquid for extraction of neonicotinoid insecticides from milk samples prior to determination by liquid chromatography-mass spectrometry

A simple and rapid microextraction procedure is reported on the use of ionic liquid in combination with magnetic nanocellulose hybrid nanoparticles. The procedure is ultrasound-assisted and applicable to selective preconcentration of neonicotinoid insecticides from milk samples, prior to being analysed by liquid chromatography-mass spectrometry. The extraction procedure uses small volume of organic solvents (<1 mL), and there is no need for centrifugation. In the experimental approach the ionic liquid was quickly disrupted by an ultrasonic probe and dispersed in milk samples in a cloudy form. At this stage, neonicotinoid insecticides were extracted into the fine droplets of ionic liquid. Then small amounts of magnetic nanocellulose hybrid nanoparticles were dispersed into the sample solutions to adsorb the ionic liquid containing the analytes and phase separation was completed. The ionic liquid allowed the microextraction of the analytes and a small volume of acetonitrile was used for elution. Magnetic nanocellulose favoured the adsorption of the ionic liquid with the analytes and improved the final recovery with respect to the use of simple magnetic nanoparticles as a sorbent material. Under the optimum conditions, decision capabilities were achieved in the 0.02–0.06 mg kg−1 range, with recoveries between 91.0% and 109.5%.