Sequential cyclic-square-wave voltammetric determination of sulfanilamide and ciprofloxacin in environment water samples using a 3D-printed electrochemical device

Author(s)

Di -Oliveira, Marina ; Araujo, Diele A. G. ; Ramos, David L. O. ; de Faria, Lucas V. ; Rocha, Raquel G. ; Sousa, Raquel M. F. ; Richter, Eduardo M. ; Paixa, Thiago R. L. C. ; Munoz, Rodrigo A. A.

• Document type: Journal article
• Source: Electrochimica Acta; v. 481, p. 11-pg., 2024-02-22.

Abstract

Sulfanilamide (SAD) and ciprofloxacin (CIP) are widely used antibiotics, and their indiscriminate use and disposal contribute to the increase in the contamination levels of aquatic environments. Herein, we propose a 3Dprinted carbon black/polylactic acid (CB/PLA) electrochemically activated electrode to determine CIP and SAD concurrently by cyclic square -wave voltammetry (C-SWV) technique. Firstly, square wave voltammetry measurements were performed exploiting the oxidation processes of CIP and SAD (Ox1CIP and Ox1SAD at around +1.3 V and +1.1 V vs. Ag|AgCl|KCl(sat.)). However, the lack of selectivity was verified in the analysis of water samples. Then, the C-SWV strategy was employed and enabled the selective determination of CIP (Ox1CIP) in the forward scan and SAD (Red1SAD) at around +0.5 V vs. Ag|AgCl|KCl(sat.)) in the reverse scan. Under selected C-SWV conditions, linear ranges from 4.96 to 40.61 mu mol L-1 (r = 0.9977) for CIP (Ox1CIP) and 1.99 to 10.78 mu mol L-1 (r = 0.9989) for SAD (Red1SAD) were obtained. The limits of detection for SAD and CIP were 0.2 and 0.6 mu mol L-1, respectively, and sensitivity was enhanced by 25 % for CIP and 60 % for SAD, employing the C-SWV protocol. In addition, this technique improves the selectivity once the analytes can be determined in distinct potential scans. Satisfactory recovery values ranging from 85 to 112 % were obtained in the analysis of spiked water samples (no dilution step), suggesting no pronounced matrix interference effect, and indicating that the C-SWV methodology ensures good accuracy. This work demonstrates that the union of 3D -printed CB/PLA electrodes and the C-SWV technique can enhance selectivity and sensitivity in the sequential analysis of CIP and SAD, and it is a promising strategy to monitor other pharmacological species in water samples. (AU)

• FAPESP's process: 22/01810-5 - 3D-PRINTING AND TEXTILE THREADS-BASED MICROFLUIDIC PLATFORMS FOR ELECTROANALYSIS OF CLINICAL, ENVIRONMENTAL AND BIOLOGICAL SAMPLES
• Grantee: Diele Aparecida Gouveia Araújo
• Support Opportunities: Scholarships in Brazil - Post-Doctoral
• FAPESP's process: 18/08782-1 - Miniaturized and integrated chemical sensors: new fabrication platforms for biological, clinical and environmental applications
• Grantee: Mauro Bertotti
• Support Opportunities: Research Projects - Thematic Grants