Use of Mixture Design with Minimal Restrictions to Optimize an Extraction Procedure Employing Diluted Acids Assisted by Ultrasound and Microwave for Nutrient Element Determination in Vegetal Samples

In this work, it was developed an alternative analytical strategy for the preparation of vegetal samples extracted with diluted acids and assisted by ultrasound and microwave radiation for the determination of nutrients elements by fast sequential flame atomic absorption spectrometer. The conditions optimized using univariate and multivariate methodologies for the procedure were as follows: 200 mg of sample; extraction solution comprising a mixture of 6.3 mL HNO3, 2.1 mL HCl, and 1.7 mL CH3COOH; extractor with a final concentration of 2.5 mol L-1; a sonication time of 30 min; and a microwave radiation time of 6 s. The accuracy of the procedure was confirmed by analyzing the certified reference material NIST 1515 (apple leaves) and by comparison with the results obtained through microwave-assisted total digestion method. The procedure was applied to determine Ca, Mg, Cu, Mn, Fe, and Zn in several cassava peel samples used in animal nutrition, and proved to be simple, reliable, fast, easy to implement, and inexpensive.

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Detalles Bibliográficos
Autores principales: Costa,Vinícius C., Silva,Erik G. P., Lima,Daniel C., Franco,Marcelo, Jesus,Raildo M., Bezerra,Marcos A., Amorim,Fábio A. C.
Formato: Digital revista
Idioma:English
Publicado: Sociedade Brasileira de Química 2018
Acceso en línea:http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532018000601189
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Sumario:In this work, it was developed an alternative analytical strategy for the preparation of vegetal samples extracted with diluted acids and assisted by ultrasound and microwave radiation for the determination of nutrients elements by fast sequential flame atomic absorption spectrometer. The conditions optimized using univariate and multivariate methodologies for the procedure were as follows: 200 mg of sample; extraction solution comprising a mixture of 6.3 mL HNO3, 2.1 mL HCl, and 1.7 mL CH3COOH; extractor with a final concentration of 2.5 mol L-1; a sonication time of 30 min; and a microwave radiation time of 6 s. The accuracy of the procedure was confirmed by analyzing the certified reference material NIST 1515 (apple leaves) and by comparison with the results obtained through microwave-assisted total digestion method. The procedure was applied to determine Ca, Mg, Cu, Mn, Fe, and Zn in several cassava peel samples used in animal nutrition, and proved to be simple, reliable, fast, easy to implement, and inexpensive.