Multivariate optimization by exploratory analysis applied to the determination of microelements in fruit juice by inductively coupled plasma optical emission spectrometry |
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Authors: | Roberta Eliane Santos Froes Waldomiro Borges Neto Nilton Oliveira Couto e Silva Rita Lopes Pereira Naveira Clésia Cristina Nascentes José Bento Borba da Silva |
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Institution: | 1. Departamento de Química, Universidade Federal de Minas Gerais, Campus Pampulha, Cx Postal 702, Belo Horizonte, MG, 31270-901, Brazil;2. Fundação Ezequiel Diaz, FUNED, Belo Horizonte, MG, Brazil |
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Abstract: | A method for the direct determination (without sample pre-digestion) of microelements in fruit juice by inductively coupled plasma optical emission spectrometry has been developed. The method has been optimized by a 23 factorial design, which evaluated the plasma conditions (nebulization gas flow rate, applied power, and sample flow rate). A 1:1 diluted juice sample with 2% HNO3 (Tetra Packed, peach flavor) and spiked with 0.5 mg L− 1 of Al, Ba, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Sn, and Zn was employed in the optimization. The results of the factorial design were evaluated by exploratory analysis (Hierarchical Cluster Analysis, HCA, and Principal Component Analysis, PCA) to determine the optimum analytical conditions for all elements. Central point condition differentiation (0.75 L min− 1, 1.3 kW, and 1.25 mL min− 1) was observed for both methods, Principal Component Analysis and Hierarchical Cluster Analysis, with higher analytical signal values, suggesting that these are the optimal analytical conditions. F and t-student tests were used to compare the slopes of the calibration curves for aqueous and matrix-matched standards. No significant differences were observed at 95% confidence level. The correlation coefficient was higher than 0.99 for all the elements evaluated. The limits of quantification were: Al 253, Cu 3.6, Fe 84, Mn 0.4, Zn 71, Ni 67, Cd 69, Pb 129, Sn 206, Cr 79, Co 24, and Ba 2.1 µg L− 1. The spiking experiments with fruit juice samples resulted in recoveries between 80 and 120%, except for Co and Sn. Al, Cd, Pb, Sn and Cr could not be quantified in any of the samples investigated. The method was applied to the determination of several elements in fruit juice samples commercialized in Brazil. |
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Keywords: | Metal ICP OES Fruit juice Multivariate optimization Exploratory analysis |
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