<p>Surfactant-induced aqueous two-phase systems (ATPS) offer an environmentally friendly alternative for the separation and preconcentration of analytes, minimizing toxic waste generation and operational costs. In this work, we report for the first time the application of a surfactant-driven ATPS to the simultaneous extraction and preconcentration of cobalt and nickel from food matrices. The system was composed of Triton X-100 + Na<sub>2</sub>SO<sub>4</sub> + H<sub>2</sub>O in the presence of 4-(2-Pyridylazo)resorcinol (PAR) as the complexing agent, followed by detection via flame atomic absorption spectrometry. Key parameters, including pH, PAR concentration, centrifugation time, and incubation time, were optimized through multivariate analysis based on a desirability function approach. Optimal conditions were pH 9.2, centrifugation time 10&#xa0;min, thermostatic bath time 11&#xa0;h, and PAR concentration 0.0750% w/w. Under these conditions, the limits of detection and quantification were 0.330 and 1.10&#xa0;µg·kg<sup>−1</sup> for Co, and 0.0370 and 0.890&#xa0;µg·kg<sup>−1</sup> for Ni, respectively, with enrichment factors of 20.2 and 16.7. The method showed good precision, with RSDs of 6.3% for Co and 7.4% for Ni, and accuracy verified using the certified reference material NIST 1515 (apple leaves), yielding recoveries of 97.6 ± 2.7% for Co and 97.9 ± 2.9% for Ni. In real food samples, recoveries ranged from 96 to 106%, further confirming the reliability of the approach. This novel methodology, by combining micellar extraction with the principles of green chemistry, provides a reliable, cost-effective, and sustainable strategy for trace metal monitoring in food safety applications.</p>

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Surfactant-Induced Aqueous Two-Phase System for the Green Preconcentration and Determination of Cobalt and Nickel in Food Samples

  • Dilaine Suellen Caires Neves,
  • Robson Silva da França,
  • Anderson Santos Souza,
  • Leandro Rodrigues de Lemos

摘要

Surfactant-induced aqueous two-phase systems (ATPS) offer an environmentally friendly alternative for the separation and preconcentration of analytes, minimizing toxic waste generation and operational costs. In this work, we report for the first time the application of a surfactant-driven ATPS to the simultaneous extraction and preconcentration of cobalt and nickel from food matrices. The system was composed of Triton X-100 + Na2SO4 + H2O in the presence of 4-(2-Pyridylazo)resorcinol (PAR) as the complexing agent, followed by detection via flame atomic absorption spectrometry. Key parameters, including pH, PAR concentration, centrifugation time, and incubation time, were optimized through multivariate analysis based on a desirability function approach. Optimal conditions were pH 9.2, centrifugation time 10 min, thermostatic bath time 11 h, and PAR concentration 0.0750% w/w. Under these conditions, the limits of detection and quantification were 0.330 and 1.10 µg·kg−1 for Co, and 0.0370 and 0.890 µg·kg−1 for Ni, respectively, with enrichment factors of 20.2 and 16.7. The method showed good precision, with RSDs of 6.3% for Co and 7.4% for Ni, and accuracy verified using the certified reference material NIST 1515 (apple leaves), yielding recoveries of 97.6 ± 2.7% for Co and 97.9 ± 2.9% for Ni. In real food samples, recoveries ranged from 96 to 106%, further confirming the reliability of the approach. This novel methodology, by combining micellar extraction with the principles of green chemistry, provides a reliable, cost-effective, and sustainable strategy for trace metal monitoring in food safety applications.