Microextraction of organophosphorus pesticides on a screw coated with PAN/calcined ZnMgAl-LDH electrospun nanofibers.

ABSTRACT

The present research is an attempt to expand the recently reported microextraction on screw method. For this purpose, polyacrylonitrile/calcined ZnMgAl-LDH nanofiber was fabricated by the electrospinning technique on the surface of a screw. It was applied to the extraction of organophosphorus pesticides (OPP) from agricultural samples. The separation and determination of OPPs were carried out by gas chromatography-mass spectrometry. The characterization of the fabricated nanofiber was performed utilizing Fourier transform infrared spectroscopy, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction instruments. Effective parameters on the extraction efficiency of the analytes including sample pH, ionic strength, sample flow rate and number of cycles, type, volume, and flow rate of desorption solvent were optimized by one-variable-at-a-time method. Under optimized conditions, the limits of detection were 0.03 and 0.07 µg L-1 for diazinon and chlorpyrifos, respectively. This method showed wide linearity in the range 0.10-1000 µg L-1 for diazinon and 0.25-1000 µg L-1 for chlorpyrifos with R2 > 0.996. The intra- and inter-day precisions (RSD%, n = 3) were ≤ 6.4% and ≤ 7.7%, respectively. Also, RSD% values less than 11.1% were obtained for screw-to-screw reproducibility. The applicability of the method for the extraction and determination of the analytes in complex agricultural environments such as cabbage, potato, tomato, cucumber, and beetroot was investigated. The results led to acceptable relative recoveries in the range 81.0-108.2%.