Electrochemically controlled solid phase microextraction based on a conductive polyaniline-graphene oxide...

Tetracycline antibiotics are employed for human and animal health and for speeding up growth rates. However, their presence in food products and environmental waters has been a concern for some years. Therefore, a variety of sample preparation methods have been developed for the analysis of tetracycline residues in these matrices.

An electrochemically controlled solid phase microextraction based on a modified copper electrode with polyaniline/graphene oxide (PANI/GO) conductive nanocomposite was developed for the extraction of oxytetracycline, tetracycline and doxycycline before high-performance liquid chromatography-UV analysis. PANI/GO was synthesized by in situ chemical oxidative polymerization, characterized by scanning electron microscopy and Fourier-transform infrared spectroscopy, and bound on the electrode using high purity conductive double-sided adhesive carbon glue. The significant factors affecting the performance of microextraction were investigated and optimized. Under the optimized conditions [sample, 15 mL; sorbent, 10 mg; pH, 3.0; electroextraction voltage, -0.9 V; electroextraction time, 20 min; eluent (MeOH/NH₃ ), 500 μL; and desorption time, 5 min], the limits of detection for target analytes were in the ranges 0.32-1.01 and 2.42-7.59 μg L^-1 in water and milk samples, respectively. The linear ranges were 1.06-750 μg L^-1 for water and 8.05-750 μg L^-1 for milk samples. The intra-day and inter-day precisions were 2.32-3.80 and 3.29-4.25, respectively. The method was applied to the determination of analytes in milk and water samples with different fat contents, and the recoveries were obtained in the range 71-104%.

The developed electro-microextraction method provides a facile, rapid, cost-effective, sensitive and efficient promising procedure for the extraction of antibiotics in complex matrices. © 2020 Society of Chemical Industry.