Abstract
QuEChERS methodology is a new alternative for polyphenol analysis in foods and beverages. This extractive and clean up method includes several steps that should be optimized to accomplish a fast and efficient extraction. In this work, chemometrics tools were applied to optimize QuEChERS parameters for polyphenol extraction from beers. By means of D-optimal screening design, the most influential extraction parameters were defined, i.e., acetonitrile volume, acidity, PSA, and C18 amount. These parameters were optimized applying a central composite design with desirability function, establishing the following optimal conditions: 2.5 mL of acetonitrile as extraction volume, 0.5% v/v of formic acid for sample acidification, 40 mg PSA for d-SPE step, and 175 mg of C18. Method validation was carried out according to International Conference on Harmonization recommendations. Data calibration curves (0.10–10.00 mg L−1) fitted a linear regression model with determination coefficients (R2) ≥ 0.992. Repeatability (relative standard deviation, RSD) and intermediate precision (RSD) showed values ≤ 4.81% (n = 6) and ≤ 6.71% (n = 3), respectively. Recovery (n = 3) at three levels ranged from 93.98 to 119.92% (RDS ≤ 4.40%) and quantification limits ranged from 0.009 to 0.118 μg mL−1. Applying the optimized and validated method, 10 beer samples were analyzed. The principal phenolic acids found were t-ferulic acid, caffeic acid, p-coumaric acid, and p-hydroxybenzoic acid. Individually, t-ferulic acid showed the highest concentration in all samples presenting a content ranged from 0.01 ± 0.01 to 2.25 ± 0.02 μg mL−1. The proposed methodology proved to be fast, reliable, and efficient for the determination of polyphenols in beer.
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Acknowledgments
This work is part of Oscar Galarce-Bustos thesis to obtain the degree of Doctor in Science and Analytical Technology from the University of Concepcion, Chile. Authors want to thank to the National Commission of Scientific and Technological Research (CONICYT) of the Chilean Government for the doctoral scholarship granted.
Funding
This study was funded by the National Fund for Scientific and Technological Development (FONDECYT) project No. 1171857, by the National Fund for Scientific and Technological Equipment (FONDEQUIP) project No. 130209, and by the University of Concepcion.
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Oscar Galarce-Bustos declares that he has no conflict of interest. Lissette Novoa declares that she has no conflict of interest. Jessy Pavon declares that she has no conflict of interest. Karem Henríquez-Aedo declares that she has no conflict of interest. Mario Aranda declares that he has no conflict of interest.
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Galarce-Bustos, O., Novoa, L., Pavon-Perez, J. et al. Chemometric Optimization of QuEChERS Extraction Method for Polyphenol Determination in Beers by Liquid Chromatography with Ultraviolet Detection. Food Anal. Methods 12, 448–457 (2019). https://doi.org/10.1007/s12161-018-1376-x
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DOI: https://doi.org/10.1007/s12161-018-1376-x