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

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 560 nm) 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 90 µg L-1 of OPPs, with limits of detection and quantification of 0.74 and 5 µg L-1 and precision of 3.67%, expressed as relative standard deviation. The pre-concentration factor was about 164 times.

A spectrophotometric flow injection system for streptomycin determination in veterinary samples.

In this work a spectrophotometric flow injection analysis system for streptomycin determination in veterinary samples, is being proposed. The method is based on streptomycin alkaline hydrolysis that forms guanidine, followed by the reaction with Fe(II). The colored product has absorption peak at 520 nm. To evaluate and optimize the system parameters, chemometrics tools, such as factorial design, Pareto chart and Doelhert design, were used. The veterinary samples are diluted in water and introduced in the FIA system, therefore no sample preparation is required. The optimized system presented: linear range of 60 up to 1000 mg L(-1), limit of detection of 18 mg L(-1) and sampling rate of 36 readings per hour. The precision was checked and the CV for veterinary sample readings were always less than 6.5%. The accuracy was studied by comparison with chromatographic method, thus, five samples of pharmaceutical veterinary were determined by HPLC and by the proposed method, and the results are in agreement (t-test, p=0.05).