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Microwave-assisted digestion for multi-elemental determination in beans, basil, and mint by ICP OES and flame
Iago J S da Silva1, Micherlane M da Silva2, Ryan G M F da Silva2
1Unidade Acadêmica de Belo Jardim (UABJ), Universidade Federal Rural de Pernambuco (UFRPE), Rodovia PE 166, km 5, Euno Andrade da Silva, CEP 55156-580, Belo Jardim, PE, Brazil; Departamento de Engenharia Civil e Ambiental, Laboratório de Saneamento Ambiental (LSA), Universidade Federal de Pernambuco (UFPE), Av. Acadêmico Hélio Ramos, s/n, Cidade Universitária, CEP 50740-530, Recife, PE, Brazil.
Abstract:
A microwave-assisted digestion method using diluted HNO3 was proposed for subsequent determination of Ca, Cd, Co, Cu, K, Mg, Mn, Mo, Na, P, Pb, S, V, and Zn in beans, basil, and mint using ICP OES and flame photometry. After applying factorial design, the optimized conditions were an HNO3 concentration of 1 mol L-1, 2.5 mL of H2O2, and a digestion time of 20 min. The method accuracy was assessed using seven reference materials, with statistical agreement between determined and certified values and an RSD of up to 11 %. Linearity was satisfactory (r > 0.999), and limits of quantification ranged from 0.031 mg kg-1 (Mn by ICP OES) to 60 mg kg-1 (K and Na by flame photometry). Applying the method to real samples, the concentrations obtained met the Cd limits established by international regulations. Finally, low agreement was verified between measured concentrations and those reported on food packaging.
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