Department of Analytical Chemistry, Faculty of Sciences, University of Cadiz, Agrifood Campus of International Excellence (ceiA3), IVAGRO, 11510 Puerto Real, Cadiz, Spain
Ms. Mercedes Vázquez-Espinosa
Department of Analytical Chemistry, Faculty of Sciences, University of Cadiz, Agrifood Campus of International Excellence (ceiA3), IVAGRO, 11510 Puerto Real, Cadiz, Spain
The onion is one of the most cultivated and consumed vegetables, and is a very valuable source of antioxidant substances. Every onion variety is rich in flavonols—mainly quercetin derivatives which makes onions the main dietary source of these compounds. This study intends to develop an ultrasound-assisted extraction method (UAE), an economical, green, and efficient technique, that allows us to determine the quality of onion extracts in terms of flavonol composition and antioxidant activity. For this purpose, an ultrasound-assisted extraction method has been optimized to obtain extracts with a high amount of flavonols, as well as with a high antioxidant activity, not only separately using a Box–Behnken design, but also simultaneously, based on multi-response optimization. Multiple response optimization has not only demonstrated an efficacy level similar to that of the individual ones, but it also represents a considerable reduction in terms of cost, time and work. The optimal conditions for simultaneous extractions were determined as follows: 76.8% methanol as an extraction solvent at pH 2 and 58.5 °C temperature, 85% amplitude, 0.9 s cycle, and 0.2:13 g:mL sample mass/solvent volume ratio. Furthermore, the developed method exhibited a high precision level and great recoveries in a rather short extraction time (2 min). These results, together with the development of a fast and simple UHPLC analysis method, lead us to consider the developed UAE method as a suitable technique for the extraction of bioactive compounds from onion matrices.
Interest in phenolic compounds has recently increased due to their potential as antioxidant agents. Moringa leaves (Moringa oleifera) have a high content of phenolic compounds, which presents them as a promising source for the extraction of these compounds. However, it is necessary to use analytical techniques to identify and quantify their actual compound content to determine the quality of the raw material and the potential of the final product. Ultrasound assisted extraction is a green, rapid and environmentally friendly extraction technique that produces high quality extracts from natural products. Hence, the aim of this research is to optimize the variables of the ultrasound-assisted extraction (UAE) process for the extraction of moringa leaves using response surface methodology (RSM) to extract the main flavonoids using methanol as the extraction solvent. A Box–Behnken design (BBD) has been used to evaluate the effect of the ultrasound extraction process variables. Finally, the optimal extraction time in the range between 2 and 30 min was determined. The results revealed that the methanol concentration was the most influential variable. The optimal extraction time was established at 15 min. Six of the main flavonoids were quantified by UHPLC-DAD and identified by UHPLC-QToF-MS. The results confirmed that UAE is an efficient method for the extraction and subsequent analysis and quality control of the flavonoids that can be found in moringa leaves.
The bioactive compounds in myrtle berries, such as phenolic compounds and anthocyanins, have shown a potentially positive effect on human health. Efficient extraction methods are to be used to obtain maximum amounts of such beneficial compounds from myrtle. For that reason, this study evaluates the effectiveness of a rapid ultrasound-assisted method (UAE) to extract anthocyanins and phenolic compounds from myrtle berries. The influence of solvent composition, as well as pH, temperature, ultrasound amplitude, cycle and solvent-sample ratio on the total phenolic compounds and anthocyanins content in the extracts obtained were evaluated. The response variables were optimized by means of a Box-Behnken design. It was found that the double interaction of the methanol composition and the cycle, the interaction between methanol composition and temperature, and the interaction between the cycle and solvent-sample ratio were the most influential variables on the extraction of total phenolic compounds (92.8% methanol in water, 0.2 s of cycle, 60 °C and 10:0.5 mL:g). The methanol composition and the interaction between methanol composition and pH were the most influential variables on the extraction of anthocyanins (74.1% methanol in water at pH 7). The methods that have been developed presented high repeatability and intermediate precision (RSD < 5%) and the bioactive compounds show a high recovery with short extraction times. Both methods were used to analyze the composition of the bioactive compounds in myrtle berries collected from different locations in the province of Cadiz (Spain). The results obtained by UAE were compared to those achieved in a previous study where microwave-assisted extraction (MAE) methods were employed. Similar extraction yields were obtained for phenolic compounds and anthocyanins by MAE and UAE under optimal conditions. However, UAE presents the advantage of using milder conditions for the extraction of anthocyanins from myrtle, which makes of this a more suitable method for the extraction of these degradable compounds.
Research interest regarding maqui (Aristotelia chilensis) has increased over the last years due to its potential health benefits as one of the most antioxidant-rich berries. Ultrasound-assisted extraction (UAE) is an advanced green, fast, and ecological extraction technique for the production of high quality extracts from natural products, so it has been proposed in this work as an ideal alternative extraction technique for obtaining extracts of high bioactivity from maqui berries. In order to determine the optimal conditions, the extraction variables (percentage of methanol, pH, temperature, ratio “sample mass/volume of solvent”, amplitude, and cycle) were analyzed by a Box-Behnken design, in conjunction with the response surface method. The statistical analysis revealed that the temperature and the percentage of methanol were the most influential variables on the extraction of the total phenolic compounds and total anthocyanins, respectively. The optimal extraction time was determined at 15 min for total phenolic compounds, while it was only 5 min for anthocyanins. The developed methods showed a high precision level with a coefficient of variation of less than 5%. Finally, the new methods were successfully applied to several real samples. Subsequently, the results were compared to those that were obtained in previous experiments by means of microwave assisted extraction (MAE). Similar extraction yields were obtained for phenolic compounds under optimized conditions. However, UAE proved to be slightly more efficient than MAE in the extraction of anthocyanins.
Allium cepa L. is one of the most abundant vegetable crops worldwide. In addition to its versatile culinary uses, onion also exhibits quite interesting medicinal uses. Bulbs have a high content of bioactive compounds that are beneficial for human health. This study intends to develop and optimize two appropriate ultrasound-assisted methods for the extraction of the phenolic compounds and anthocyanins present in red onion. A response surface methodology was employed and, specifically, a Box–Behnken design, for the optimization of the methods. The optimal conditions for the extraction of the phenolic compounds were the follows: 53% MeOH as solvent, pH 2.6, 60 °C temperature, 30.1% amplitude, 0.43 s cycle, and 0.2:11 g sample/mL solvent ratio. On the other hand, the optimal conditions for the anthocyanins were as follows: 57% MeOH as solvent, pH 2, 60 °C temperature, 90% amplitude, 0.64 s cycle, and 0.2:15 g sample/mL solvent ratio. Both methods presented high repeatability and intermediate precision, as well as short extraction times with good recovery yields. These results illustrate that the use of ultrasound-assisted extraction, when properly optimized, is suitable for the extraction and quantification of the compounds of interest to determine and improve the quality of the raw material and its subproducts for consumers.