Development of a portable electroanalytical method using nickel modified screen-printed carbon electrode for ethinylestradiol determination in organic fertilizers

• Published in: Ecotoxicology and environmental safety 2021-01, Vol.208, p.111430, Article 111430
• Main Authors: Silva, Luiz R.G., Rodrigues, José G.A., Franco, Juliana P., Santos, Layla P., D'Elia, Eliane, Romão, Wanderson, Ferreira, Rafael de Q.
• Format: Article
• Language: English
• Subjects: Carbon - chemistry; Electrodes; Environmental Monitoring - methods; Ethinyl Estradiol - analysis; Ethinylestradiol; Fertilizers - analysis; Humans; Nickel - chemistry; Organic fertilizer; Research Design; SPCE-Ni; Struvite; SWV; Urine
• ISSN: 0147-6513; 1090-2414
• DOI: 10.1016/j.ecoenv.2020.111430

Urine and struvite are organic fertilizers that have all nutritional requirements for the growth of a plant. However, these fertilizers may contain some emerging organic contaminants, such as ethinylestradiol, which is one of the most common hormones found in aquatic environments and can cause several changes in living organisms. Thus, the present study developed a fast, sensitive, inexpensive, and portable method for determining ethinylestradiol in urine and struvite, using square wave voltammetry (SWV) and screen-printed carbon electrodes modified with electrodeposited nickel film (SPCE-Ni). The electrodeposition of the nickel film on the screen-printed electrode was performed by cyclic voltammetry and optimized using complete factorial design 23 and central composite design. The parameters optimized for SPCE-Ni were: number of cycles (1000); scan rate (5 V s−1) and Ni2+ concentration (9.4 mmol L−1). The operational parameters of the SWV for ethinylestradiol analysis were also optimized by experimental designs and obtained the following optimal values: step potential (10 mV), modulation amplitude (40 mV), and frequency (20 Hz). The method used 0.1 mol L−1 BR buffer (pH 8.0) as support electrolyte and presented a limit of detection of 0.052 µmol L−1 (R2 = 0.996). Ethinylestradiol recovery test in struvite, human urine, synthetic urine, and pharmaceutical tablets ranged from 93.9% to 107.5%, indicating that there is no matrix effect. Furthermore, an interference test was performed with several drugs did not show any significant changes in the ethinylestradiol analytical signal, guaranteeing a greater precision of the method. These results reinforce the possibility of applying the proposed method in loco with a practical and fast way, without the need to use significant amounts of sample. [Display omitted] •In loco monitoring of emerging contaminants using green chemistry practices.•Ethinylestradiol determination in organic fertilizers (urine and struvite).•Simple, fast, and very low reagent consumption (µL) electroanalytical method.•Portable equipment associated with modified screen-printed carbon electrodes.