Technological prospecting and obtaining natural dye from butterfly bean flowers (Clitoria Ternatea L.) using macroporous adsorption resins.
Key Word: Clitoria ternatea, natural dye, macroporous resin, patentability.
The sensory characteristics of foods are largely responsible for the acceptance of products by the consumer, including color. Artificial colors have been used for a long time by the industry, however consumers are currently looking for more natural ingredients, with a reduction in synthetic additives and with less impact on the environment. In this context, the replacement of artificial dyes by natural pigments is of particular interest and has gained great relevance in many researches and also by the marked consumer who has preferred clean label products. Among the natural dyes, anthocyanins stand out which, in addition to their vibrant colors in the most different shades of red, purple and blue, have high solubility in water, a positive factor for application in various products, such as beverages and aqueous systems. Hydroelectrolytic supplements, better known as isotonics, are products specially formulated with the objective of replacing water and mineral salts, in addition to acting as a source of energy. Although this category of beverages is associated with healthiness, as its main consumers are sports practitioners. Traditionally, synthetic dyes have been used in the coloring of different flavors of isotonic drinks. This work aimed to extract a natural dye from the anthocyanins present in the petals of the butterfly bean (Clitoria Ternatea L.) flowers and to evaluate the thermal stability of this pigment in an isotonic model-system, as well as the in vitro digestive stability of the functional compounds present in the beverage, in addition to studying the process of separation and purification of anthocyanins from the petals of butterfly beans using macroporous resins, a process that stands out for its low cost and lower solvent consumption. To achieve the general objective, the thesis was carried out in 4 chapters, Chapter I being a literature review, and the other chapters of results, which addressed the technological prospection on the topic, stability studies of anthocyanins in a beverage model system isotonic and extraction and purification of anthocyanins from butterfly bean flowers using macroporous resins. In the literature review on the use of anthocyanins, from different sources, as colorant in beverage and aqueous model-systems, addressing the technological characteristics for the feasibility of applying these natural colorants in different products. Regarding the results, in Chapter II it was performed a study of technological prospecting, in patent databases, regarding the use of macroporous resins for the extraction and purification of anthocyanins. It was possible to verify that the growth of patent application filings in this technological area showed greater prominence after the year 2000 and that China was the main country in the number of patent filings. In Chapter III, the thermal degradation kinetics in an isotonic model system were studied, submitting the samples to 60, 70 and 80 ºC, to evaluate the thermal stability of anthocyanins in the petals of butterfly bean and also the stability of ascorbic acid. It was observed that the samples submitted to 60 and 70 ºC showed greater stability compared to samples submitted to 80 ºC, the degradation constant (k) of anthocyanins presented the highest value (46.40×10−4 min−1) in the sample of buffer solution, without addition of ascorbic acid, submitted to 80 ºC, while the isotonic sample, submitted to the same temperature, presented k of 26.50×10−4 min−1. The half-life time (t1/2) on ascorbic acid stability of isotonic samples showed 95.87 min at 60 ºC and 79.49 min at 80 ºC, which indicates the influence of temperature on the stability of these compounds. The study of in vitro bioaccessibility of both ascorbic acid and anthocyanins from butterfly bean petals in isotonics showed that both presented greater stability in the gastric phase and that temperature also influenced the bioaccessible percentage of these compounds at the end of the intestinal phase, where the samples submitted to 80 ºC showed 69.13% degradation of ascorbic acid and 59.00% degradation of anthocyanins. In Chapter IV, the behavior of adsorption and recovery of anthocyanins from butterfly bean petals in six different types of macroporous resins was studied, evaluating the influence of pH, temperature and concentration on the extraction process. Of the six macroporous resins studied, XAD7HP and DAX8 were selected for having the highest adsorption capacity, 248.55 mg/g and 228.84 mg/g, respectively, and also the best recovery percentages of anthocyanins, 75.66% for DAX7HP resin and 52.64% for DAX8 resin. After the selection of resins, studies of adsorption kinetics were carried out, in which the results were better fitted to the pseudo-second order kinetic model, for the two resins; the Freundlich and Langmuir models were evaluated and the isotherm data for the XAD7HP resin best fit the Freundlich model, and for the DAX8 resin the model that best fit the data was the Langmuir model. In addition, a basic manual was prepared to guide the initial process of applying for a patent (Appendix I), and this manual was also applied for the understanding and feasibility of the patentability of this study, appendix II, where they were selected, after structuring of the search strategy, four patent documents that show that the present study is already revealed in the state of the art and that it does not meet the inventive step requirement for patentability.