Magnetic restricted-access carbon nanotubes for the extraction/pre-concentration of organophosphates from food samples followed by spectrophotometric determination

Abstract

In this work, magnetic restricted-access carbon nanotubes (M-RACNTs) were synthesized, characterized and used in the dispersive solid-phase extraction (d-SPE) of organophosphate pesticides (OPPs) from food samples (broccoli, eggplant, cauliflower, and soy milk), followed by spectrophotometric determination in a flow injection analysis system. Fe3O4 nanoparticles were incorporated in the multi-walled carbon nanotubes employing dimethylformamide. The dimethylformamide was used as a solvent in the incorporation process, forming the suspension of both particles. The resulting M-CNTs were covered with an external bovine serum albumin (BSA) layer, chemically crosslinked. M-RACNTs were able to efficiently capture OPPs, excluding about 95% of the proteins from food matrices. The analyses were carried out in a flow injection analysis system (FIA), with the spectrophotometric detection (at 560nm) of the complex formed by the reaction between OPPs, N-bromosuccinimide and rhodamine B. A fractional factorial design method was used to optimize the experimental parameters. The addition/recovery test showed results from 95.5% to 108.9%. Accuracies were checked by comparing the results obtained with the proposed and standard HPLC methods, which were in agreement. The proposed method was linear from 5 to 90μgL-1 of OPPs, with limits of detection and quantification of 0.74 and 5μgL-1 and precision of 3.67%, expressed as relative standard deviation. The pre-concentration factor was about 164 times.