Optimization of Polyphenols Extraction Using Response Surface Methodology and Application of Near Infrared Spectroscopy to Phenolic Content Analysis of Pine Bark

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2010
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Abstract
The utilization of pine bark for processing water resistant phenol-formaldehyde adhesive for plywood production encounters difficulties due to the very high reactivity of the formaldehyde condensable phenolics and other un-intended compounds (sugars) extracted into solution, as well as time consuming and costly chemical analysis. The potential of near infrared reflectance spectroscopy (NIRS) for rapidly and accurately determining the polyphenolic contents in Pinus caribaea bark extracts was assessed by means of multivariate calibration techniques. To optimize the polyphenol content, four different solvents (aqueous acetone, aqueous ethanol, aqueous NaOH and water) were used in the extractions. Batch experiments were performed at different solvent concentrations, time, temperature and liquidsolid ratio. Mathematical polynomial models were proposed to identify the effects of individual interactions of these variables on the extraction of polyphenols and optimum content using response surface methodology (RSM). The optimized conditions were used to extract polyphenols which were used in the formulation of resol resins for plywood manufacture. The first derivative spectra with PLS regression were found to provide the best prediction of the tannin content and Stiasny number of pine bark with a SECV = 0.14 and 1.26 and r2 = 0.97 and 0.95 respectively. The predicted values were thus highly correlated with costly measured values of tannin content and Stiasny number. The highest extraction model efficiency (78.98%) was observed for aqueous extraction when only tannin content was maximized in the numerical optimization process. This corresponded to optimum extraction conditions of 69°C extraction temperature, 126 min extraction time and 23:1 liquid-solid ratio. The RSM model that gave a high tannin content (18.85%) with a corresponding good quality resin (shear strength = 2.4 MPa, 10% delamination) was found for aqueous ethanol extraction when the objective function was to maximize both the tannin content and Stiasny number and minimize the sugar content simultaneously.
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A thesis submitted to the Department of Chemical Engineering,Kwame Nkrumah University of Science and Technology in partial fulfillment of the requirements for the degree of Doctor of Philosophy.
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