Carbon nanotubes@silicon dioxide nanohybrids coating for solid-phase microextraction of organophosphorus pesticides followed by gas chromatography-corona discharge ion mobility spectrometric detection

A high efficiency solid-phase microextraction (SPME) fiber coated with porous carbon nanotubes-silicon dioxide (CNTs-SiO2) nanohybrids was synthesized and applied for the determination of some organophosphorus pesticides (OPPs) in vegetables, fruits and water samples. Gas chromatography-corona discharge ion mobility spectrometry was used as the detection system. Glucose, as a biocompatible compound, was used for connecting CNT and SiO2 during a hydrothermal process. The electrospinning technique was also applied for the fiber preparation. The parameters affecting the efficiency of extraction, including stirring rate, salt effect, extraction temperature, extraction time, desorption temperature and desorption time, were investigated and optimized. The developed CNTs@SiO2 fiber presented better extraction efficiency than the commercial SPME fibers (PA, PDMS, and PDMS-DVB). The intra- and inter-day relative standard deviations were found to be lower than 6.2 and 9.0%, respectively. For water samples, the limits of detection were in the range of 0.005-0.020 μg L−1 and the limits of quantification were between 0.010 and 0.050 μg L−1. The results showed a good linearity in the range of 0.01-3.0 μg L−1 for the analytes. The spiking recoveries ranged from 79 (±9) to 99 (±8). The method was successfully applied for the determination of OPPs in real samples.