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Purple potato is one of the least known and consumed potato varieties. It is as rich in nutrients, amino acids and starches as the rest of the potato varieties, but it also exhibits a high content of anthocyanins, which confer it with some attractive health-related properties, such as antioxidant, pain-relieving, anti-inflammatory and other promising properties regarding the treatment of certain diseases. A novel methodology based on ultrasound-assisted extraction has been optimized to achieve greater yields of anthocyanins. Optimal extraction values have been established at 70 degrees C using 20 mL of a 60% MeOH:H2O solution, with a pH of 2.90 and a 0.5 s(-1) cycle length at 70% of the maximum amplitude for 15 min. The repeatability and intermediate precision of the extraction method have been proven by its relative standard deviation (RSD) below 5%. The method has been tested on Vitelotte, Double Fun, Highland and Violet Queen potatoes and has demonstrated its suitability for the extraction and quantification of the anthocyanins found in these potato varieties, which exhibit notable content differences. Finally, the antioxidant capacity of these potato varieties has been determined by means of 2,2-diphenyl-1-picrylhydrazyl (DDPH) radical scavenging and the values obtained were similar to those previously reported in the literature., This work has been supported by the project "EQC2018-005135-P" (Equipment for liquid chromatography by means of mass spectrometry and ion chromatography) of the State Subprogram of Research Infrastructures and Technical Scientific Equipment.

Erica australis plants have been used in infusions and folk medicine for years for its diuretic and antiseptic properties and even for the treatment of infections. In addition, a recently published thorough study on this species has demonstrated its antioxidant, antibiotic, anti-inflammatory, anticarcinogenic and even antitumoral activities. These properties have been associated with the high content of anthocyanins in E. australis leaves and flowers. The aim of the present research is to optimize an ultrasound-assisted extraction methodology for the recovery of the anthocyanins present in E. australis flowers. For that purpose, a Box Behnken design with response surface methodology was employed, and the influence of four variables at different values was determined: namely, the composition of the extraction solvents (0–50% MeOH in water), the pH level of those solvents (3–7), the extraction temperature (10–70 C), and the sample:solvent ratio (0.5 g:10 mL–0.5 g:20 mL). UHPLC-UV-vis has been employed to quantify the two major anthocyanins detected in the samples. The extraction optimum conditions for 0.5 g samples were: 20 mL of solvent (50% MeOH:H2O) at 5 pH, with a 15 min extraction time at 70 C. A precision study was performed and the intra-day and inter-day relative standard deviations (RSDs) obtained were 3.31% and 3.52%, respectively. The developed methodology has been successfully applied to other Erica species to validate the suitability of the method for anthocyanin extraction., This work has been supported by the project "EQC2018-005135-P" (Equipment for liquid chromatography by means of mass spectrometry and ion chromatography) of the State Subprogram of Research Infrastructures and Technical Scientific Equipment.

The objective of the present study is to develop an optimized method where headspace-ion mobility spectrometry is applied for the detection and discrimination between four petroleum-derived products (PDPs) in water. A Box-Behnken design with a response surface methodology was used, and five variables (incubation temperature, incubation time, agitation, sample volume, and injection volume) with influences on the ion mobility spectrometry (IMS) response were optimized. An IMS detector was used as a multiple sensor device, in which, each drift time acts as a specific sensor. In this way, the total intensity at each drift time is equivalent to multiple sensor signals. According to our results, 2.5 mL of sample incubated for 5 min at 31 degrees C, agitated at 750 rpm, and with an injection volume of 0.91 mL were the optimal conditions for successful detection and discrimination of the PDPs. The developed method has exhibited good intermediate precision and repeatability with a coefficient of variation lower than 5%, (RSD (Relative Standard Deviation): 2.35% and 3.09%, respectively). Subsequently, the method was applied in the context of the detection and discrimination of petroleum-derived products added to water samples at low concentration levels (2 mu L center dot L-1). Finally, the new method was applied to determine the presence of petroleum-derived products in seawater samples., This work has been co-financed by the 2014-2020 ERDF Operational Program and by the Department of Economy, Knowledge, Business and University of the Regional Government of Andalusia. Project reference: "FEDER-UCA18-107214".

Petroleum remains the principal raw material for the manufacture of a wide variety of products with multiple uses. Within this framework, it is possible to find petroleum derivative products, such as paraffin waxes, with applications in the agri-food industry. Due to the above-mentioned use, the adaptation of the quality control of these products to the requirements of this industry is a factor to be considered by the producers to comply with food safety standards. The present study is focused on establishing the starting conditions for the development and optimization of an analytical methodology based on TD-GC-MS (Thermal Desorption – Gas Chromatography – Mass Spectrometry) that allows the determination and identification of the volatile organic compounds that are undesirable not only because of their smell but also because they may pose a risk to health as a result of prolonged exposure. Desorption time and temperature, as well as the chromatographic separation conditions, were studied to generate the right signals to identify the volatile organic compounds in the paraffin waxes.

In recent years, there has been increasing interest in the functional components of sweet potato because of its nutritional and medicinal value. The aim of this study is to analyse how much sweet potato phenolic compounds composition (derived from caffeoylquinic acids) varies as a result of cooking. Traditional techniques such as: boiling, oven roasting and more recent processing techniques such as microwave cooking were tested. Three sweet potato varieties were cooked for different periods of time and under different conditions. Ultrasound-assisted extraction (UAE) was used to extract the compounds of interest and then, a chemometric tool such as Box-Behnken design (BBD) was successfully used to evaluate and optimise the most influential factors in the extraction, i.e., temperature, solvent composition and sample-to-solvent ratio. The optimal settings for UAE were: solvent 100% methanol, a temperature of 39.4 degrees C and a mass/volume ratio of 0.5 g per 10 mL solvent. Oven roasting of sweet potatoes resulted in increased levels of caffeoylquinic acids, whereas prolonged cooking times in water resulted in decreasing levels of the same., This work has been supported by the project "EQC2018-005135-P" (Equipment for liquid chromatography by means of mass spectrometry and ion chromatography) of the State Subprogram of Research Infrastructures and Technical Scientific Equipment.

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 degrees 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., This work has been supported by the project "EQC2018-005135-P" (Equipment for liquid chromatography by means of mass spectrometry and ion chromatography), of the State Subprogram of Research Infrastructures and Technical Scientific Equipment. This research was funded by University of Cadiz, by the INIA (National Institute for Agronomic Research) and FEDER (European Regional Development Fund, within the framework of the Operational Programme under the Investment for Growth 2014-2020) for their financial support (Project RTA2014-00083-C03-03), and by the Ministry of Science and Innovation of Spain (FPU grant AP-2018-03811 to Ana Velasco Gonzalez de Peredo).

Capsaicinoids and capsinoids compounds have been a focus of special attention for their health benefits. An effective and rapid Ultra-High-Performance Liquid Chromatography (UHPLC-PDA) method has been developed and validated for the simultaneous separation and quantitative determination of the major capsaicinoids and capsinoids present in peppers. The separation of all the compounds of interest was achieved in less than 2 min by means of an ACQUITY UPLC BEH rp-C18 column (100 mm × 2.1 mm i.d., 1.7 µm particle size). The variables that have been optimized are the mobile phase (water as solvent A and acetonitrile as solvent B, both acidified by adding 0.1% acetic acid), separation gradient, column temperature (35–70 °C), flow rate (0.6–0.95 mL min−1), and injection volume (2.5–3.5 µL). The evaluation of the chromatographic performance revealed excellent resolution, retention factor, and selectivity. The method was satisfactorily validated in terms of linearity, detection and quantification limits, precision, and robustness.

In forensic and environmental sciences, the identification of petroleum-based products is an important task to establish not only the origin of a given residue but also the hazard level or the appropriate cleanup procedure. A new strategy for the fingerprinting of petroleum-based products (PP) in water samples (seawater and freshwater) for rapid and easy fuel spill identification has been developed. For this purpose, an HS-MS has been used in combination with chemometric tools such as linear discriminant analysis (LDA). A set of 70 samples from seven types of PPs (aromatic products, alcohols, normal alkanes, gasoline, diesel, lubricants and naphthenic-paraffinic products), all of which were added to water (seawater and freshwater), were analyzed. 100% of the samples were discriminated according to the type of petroleum-based products used regardless the nature of the water. Furthermore, a fingerprint was obtained for each petroleum product by plotting the m / z values selected by the LDA and this allowed the rapid identification of the petroleum products. The repeatability and intermediate precision were evaluated for both types of water samples and good values were obtained (RSD

Black mulberry (Morus nigra L.) is one of the most important species of the genus Morus as its fruit contains substantial levels of anthocyanins and phenolic compounds which show a potentially positive effect on the human health. Nowadays, PLE is becoming a promising extraction technology. Therefore, the development of fast extraction methods of anthocyanins and phenolic compounds from mulberry pulp using pressurized-liquid extraction (PLE) has been studied in this paper. The operating conditions (solvent, temperature, pressure, purge time, pH, and flushing) were investigated by a Box–Behnken design. Analysis of the model clearly showed that the most influential factors were temperature and solvent composition. The optimum extraction conditions for anthocyanins were 47.2% methanol in water, a temperature of 75.5 °C, pressure of 200 atm, a purge time of 90 s, pH 3.01, and 50.2% for flushing. The best conditions for the extraction of phenolics were 74.6% methanol, 99.4 °C, 100 atm, 90 s purge, pH 7, and 100% flushing. The optimum extraction time was 10 min. The precision values of the methods were also evaluated and excellent results (RSD

A rapid high-performance liquid chromatography method with a C18 reverse-phase fused-core column has been developed for the determination and quantification of the main capsaicinoids (nornordihydrocapsaicin, nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin and homodihydrocapsaicin) present in Naga Jolokia peppers. A fused-core Kinetex™ C18 column (50×2.1mm i.d.; 2.6μm) was used for the analysis. The chromatographic separation was obtained with a gradient method in which the mobile phase was water (0.1% acetic acid) as solvent A and acetonitrile (0.1% acetic acid) as solvent B. The separation of all compounds was achieved in less than 3min with a total analysis time (sample-to-sample) of 10min. The robustness of the method was evaluated. The method showed excellent repeatability and intermediate precision expressed as coefficient of variance of less than 2%. The developed method was employed for the quantification of the major capsaicinoids present in different peppers and commercial products containing chilli peppers.

Prunus spinosa L. is a shrub that produces berries—sloes—with a high content of phenolic compounds and anthocyanins. Numerous consumer products are made from sloes, such as “Pacharán” liquors or jams. For these reasons, it is crucial to design accurate analytical methods for the extraction of these bioactive compounds in order to promote their consumption and to improve our health. In this study, an ultrasound-assisted extraction method was developed to extract phenolic compounds and anthocyanins from sloes. Several process variables (methanol composition, pH, temperature, cycle, amplitude, and sample–solvent ratio) were optimized based on a Box–Behnken design. The most influential parameters for the extraction of total phenolic compounds were the cycle, the percentage of methanol, and pH of the extraction solvent, with 0.2 s, 67%, and pH 7 as their optimal values, respectively. For total anthocyanins, all parameters were influential, with 44% methanol at pH 2, 48 °C, 0.2 s cycles, 30% amplitude, and 1.5 g/20 mL ratio as the optimal values for their corresponding variables. Both methods showed high recoveries, short time use, and high precision (RSD < 5%). In addition, the sloe liqueur “Pacharán” and sloe jams were analyzed to demonstrate the applicability of these methods for the extraction of the real matrix.

In this work, two methods based on microwave-assisted extraction techniques for the extraction of both anthocyanins and total phenolic compounds from açai have been developed. For that, a full factorial design (Box-Behnken design) has been used to optimize the following four variables: solvent composition (25–75% methanol in water), temperature (50–100 °C), pH (2–7), and sample/solvent ratio (0.5 g: 10 mL–0.5 g: 20 mL). The anthocyanins and total phenolic compounds content have been determined by ultra high-pressure liquid chromatography and Folin-Ciocalteu method, respectively. The optimum conditions for the extraction of anthocyanins were 38% MeOH in water, 99.63 °C, pH 3.00, at 0.5 g: 10 mL of ratio, while for the extraction of total phenolic compounds they were 74.16% MeOH in water, 99.14 °C, pH 5.46, at 0.5 g: 20 mL of ratio. Both methods have shown a high repeatability and intermediate precision with a relative standard deviation lower than 5%. Furthermore, an extraction kinetics study was carried out using extraction periods ranging from 2 min until 25 min. The optimized methods have been applied to açai-containing real samples. The results with such real samples have confirmed that both methods are suitable for a rapid and reliable extraction of anthocyanins and total phenolic compounds.

Capsinoids are very similar antioxidant compounds to capsaicinoids, but less irritating, non-pungent and more palatable, and can thus be used in greater concentrations for food applications. To date, three capsinoids (capsiate, dihydrocapsiate, and nordihydrocapsiate) have been isolated from the pepper fruits. Due to its substantial commercial importance, it would be convenient to determine which pepper varieties have a richer content. Ultrasound- (UAE) and microwave- (MAE) assisted extraction have been implemented and analyzed using multivariate statistical methods. Firstly, different solvents were tested individually. The three best solvents were used in a set mixture design, where 42% methanol and 58% ethyl acetate were determined as the optimum combination for UAE, and 100% methanol for MAE. Subsequently, a Box&ndash, Behnken experimental design with four variables for both UAE and MAE (time, temperature, pH and sample mass:solvent volume &ldquo, ratio&rdquo, ) was performed. The sample mass:solvent volume was the most influential variable in UAE, while for MAE no variable was any more influential than the others. Finally, both optimized extraction methods were successfully applied to different varieties of peppers. Besides, to demonstrate the efficiency of both extraction methods, a recovery study was performed. The results prove the potential of both techniques as highly adequate methods for the extraction of capsinoids from peppers.

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 &ldquo, sample mass/volume of solvent&rdquo, 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.

According to European Union regulations, honey is a pure product and adding to or removing from it any kind of substance is illegal. Nevertheless, its adulteration by adding inexpensive and artificial adulterants is a common practice. This paper deals with the use of visible and near-infrared spectroscopy (Vis-NIRS) combined with chemometric tools as a screening technique for the identification and quantification of different types of adulterants (inverted sugar, rice syrup, brown cane sugar and fructose syrup) added to high-quality honey (Granada Protected Designation of Origin, Spain) at different levels (5%-50%). A complete discrimination between non-adulterated and adulterated samples was achieved. A general regression model to quantify the adulteration levels was developed as well as specific models for each adulterant. The coefficients of determination were higher than 0.96 for all the models. These results demonstrate the capacity of Vis-NIRS combined with chemometric tools for honey quality control.

Chokeberry (Aronia melanocarpa L.) contains a large number of bioactive compounds, which make of it a highly nutritional and antioxidant food with anti-cancer and anti-inflammatory properties. It has been recently seen its consumption increased because of its interesting composition and properties as a functional food. The ultrasound-assisted extraction method has been optimized, since it is a simple and fast technique to extract phenolic compounds, as well as anthocyanins, not only separately but also simultaneously. Multiple response has been optimized and demonstrated an effectiveness level similar to the individual ones. This represents a considerable reduction in costs, time and work. The optimal conditions for simultaneous extractions were: 54% methanol as extraction solvent at pH 2.72 and 69.4 &deg, C temperature, 70% amplitude, 0.7 s cycle, and 0.5:18.2 g:mL sample mass/solvent volume ratio. The developed methods showed a high precision level with coefficients of variation lower than 5%. The methods were successfully applied to commercial samples. Additionally, the extraction of other compounds of biological interest, such as organic acids and sugars, was also studied.

The evolution of individual and total capsaicinoids content in three pepper varieties of Capsicum chinense Jacq. (&lsquo, Bode&rsquo, (B), &lsquo, Habanero&rsquo, (H), and &lsquo, Habanero Roxo&rsquo, (Hr)) during fruit ripening was studied. The five major capsaicinoids (nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin) were extracted using ultrasound-assisted extraction and the extracts were analysed by ultra-performance liquid chromatography with fluorescence detection (UHPLC-Fl). The plants were grown in a glasshouse and sampled every 7 days until over-ripening. As expected, the results indicated that the total capsaicinoids content increases during the ripening of pepper fruits. The maximum contents of capsaicinoids were reached at different fruit development stages depending on the cultivar. The &lsquo, pepper presented the greatest total capsaicinoids content (3.86 mg g&minus, 1 fresh weigh, F.W.), followed by the &lsquo, pepper (1.33 mg g&minus, 1 F.W.) and &lsquo, pepper (1.00 mg g&minus, 1 F.W.). In all the samples, capsaicin represented more than 80% of the total capsaicinoids content. Due to the high variability observed in the evolution of capsaicinoids content over the ripening process, this work intends to contribute to the existing knowledge on this aspect in relation to the quality of peppers.

In recent years pollution due to hydrocarbon spills has increased markedly as a result of the numerous advances in technologies and industrial processes. Anthropogenic activities (accidental or illegal) are responsible for most of these incidents. In some cases, the spills are not detected at the moment they occur and the contaminants are subjected to different degradation phenomena that may change the chemical composition of the hydrocarbon over time. An incorrect or ineffective identification of the spill could lead to significant consequences, bearing in mind that most spills are hazardous to the environment. In the present work the capacity of the analytical technique based on the Electronic Nose (eNose) combined with chemometrics in the identification and discrimination of different weathered petroleum-derived products (PDPs) was studied. Different volumes (40 &mu, L and 80 &mu, L) of PDPs (gasoline, diesel, and paraffin) were poured onto different supports (wood, cork, paper, and cotton sheet) and subjected to a natural weathering process by evaporation for one month. The porosity of the support was also studied. The application of linear discriminant analysis allowed the full discrimination of the samples according to the presence/absence of PDP and a 97.7% of correct discrimination of the different PDPs regardless of the weathering time, support or volume used. The results show that the system is capable of detecting and discriminating the presence of petroleum-derived products in any of the situations studied.

The NIR spectra from 1000 to 2500 nm of 18 different explosives, propellant powders and energetic salts were collected and interpreted. NIR spectroscopy is known to provide information about the combination bands and overtones of highly anharmonic vibrations as those occurring in XH bonds (CH, NH and OH). Particularly intense and complex were the bands corresponding to the first combination region (2500&#-1900&;8239#nm) and first overtone stretching mode (2nu) of CH and NH bonds (1750&#-1450&;8239#nm). Inorganic oxidizing salts including sodium/potassium nitrate, sodium/potassium chlorate, and sodium/potassium perchlorate displayed low intense or no NIR bands.

Headspace mass spectrometry and near infrared spectroscopy in combination with chemometric tools, including hierarchical cluster analysis and linear discriminant analysis, have been used for the classification of gasoline according to the research octane number. Volatile components were studied by headspace mass spectrometry whereas the whole gasoline samples were studied by near infrared spectroscopy. Sample pretreatment was not required for either analysis. A set of 60 samples belonging to two different research octane numbers (95# and 98#) was analyzed by both techniques. The best results were obtained on using linear discriminant analysis, which allowed a full discrimination of the gasoline samples using only four m / z ratios (46, 59, 95 and 98) in the case of headspace mass spectrometry and three regions (below 1000 nm, 1400–1500 nm and 1600 nm) in the case of near infrared spectroscopy.

A new chromatographic method for the separation of major capsaicinoids in peppers has been developed. Nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin have been separated by reversed-phase ultra-performance liquid chromatography. A gradient method has been developed using two solvents: 0.1% acetic acid in water and 0.1% acetic acid in methanol. The developed method allows the full separation of capsaicinoids in less than 3 min, with high reproducibility (relative standard deviation < 4.3%) and repeatability (relative standard deviation < 3.6%). Robustness regarding the total amount of methanol in the sample was determined. Comparison with previous reversed-phase high-performance liquid chromatography methods using both monolithic and conventional columns was also studied. Finally, the method was applied in the determination of major capsaicinoids in 16 hot pepper samples produced in Spain.

A method for the concentration and cleaning of red grape extracts prior to the determination of anthocyanins by UPLC-DAD has been developed. This method is of special interest in the determination of phenolic maturity as it allows the analysis of the anthocyanins present in grapes. Several different SPE cartridges were assessed, including both C-18- and vinylbenzene-based cartridges. C-18-based cartridges presented a very low retention for the glucosylated anthocyanidins while vinylbenzene-based cartridges showed excellent retention for these compounds. The optimized method involves the initial conditioning of the cartridge using 10 mL of methanol and 10 mL of water, followed by loading of up to 100 mL of red grape extract. Ten mL of water was used in the washing step and anthocyanins were subsequently eluted using 1.5 mL of acidified methanol at pH 2. This method simplifies the determination of individual anthocyanins as, on the one hand, it cleans the sample of interference and, on the other hand, it increases the concentration to up to 25:1.5. The developed method has been validated with a range of different grapes and it has also been tested as a means of determining the different anthocyanins in grapes with different levels of maturity.

A method for the discrimination of different gasoline samples according to their RON has been developed using an HS-MS system. The working conditions for the HS-MS analytical procedure were optimized by experimental design. The variables optimized were incubation temperature, incubation time, and sample volume. The optimal conditions were as follows: 145 °C incubation temperature, 10 min incubation time, and 80 μL sample volume. The optimized method was applied to a set of 30 gasoline samples with different RON values (95# and 98#). An hierarchical cluster analysis was applied in which the m/z (45−200 m/z) values were used as a variable to form groups. A perfect classification (100%) of the gasoline samples according to their RON was achieved. A linear discriminant analysis was carried out and the resulting linear discriminant function enabled a perfect classification of the gasoline samples according to the RON using only the m/z values of 88, 95, and 112. These results demonstrate the capacity of the new technique for the discrimination of gasoline samples according to their RON and the applicability of this method in this field. For the first time, HS-MS was used for this purpose. The main advantage of HS-MS vs previous methodologies is that no chromatographic separation and no sample manipulation are required. HS-MS is therefore faster than the current techniques used in these kinds of studies; it is also cheaper, ecofriendly, and easy to use for routine analysis.

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 &deg, 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 &lt, 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.

The phenolic compounds and anthocyanins present in myrtle berries are responsible for its beneficial health properties. In the present study, a new, microwave-assisted extraction for the analysis of both phenolic compounds and anthocyanins from myrtle pulp has been developed. Different extraction variables, including methanol composition, pH, temperature, and sample&ndash, solvent ratio were optimized by applying a Box&ndash, Behnken design and response surface methodology. Methanol composition and pH were the most influential variables for the total phenolic compounds (58.20% of the solvent in water at pH 2), and methanol composition and temperature for anthocyanins (50.4% of solvent at 50 &deg, C). The methods developed showed high repeatability and intermediate precision (RSD &lt, 5%). Both methods were applied to myrtle berries collected in two different areas of the province of Cadiz (Spain). Hierarchical clustering analysis results show that the concentration of bioactive compounds in myrtle is related to their geographical origin.

The evolution of individual and total contents of capsaicinoids present in Peter peppers (Capsicum annuum var. annuum) at different ripening stages has been studied. Plants were grown in a glasshouse and the new peppers were marked in a temporal space of ten days. The extraction of capsaicinoids was performed by ultrasound-assisted extraction with MeOH. The capsaicinoids nordihydrocapsaicin (n-DHC), capsaicin, dihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin were analyzed by ultraperformance liquid chromatography (UHPLC)-fluorescence and identified by UHPLC-Q-ToF-MS. The results indicate that the total capsaicinoids increase in a linear manner from the first point of harvest at ten days (0.283 mg/g FW) up to 90 days, at which point they reach a concentration of 1.301 mg/g FW. The evolution as a percentage of the individual capsaicinoids showed the initial predominance of capsaicin, dihydrocapsaicin, and n-DHC. Dihydrocapsaicin was the major capsaicinoid up to day 50 of maturation. After 50 days, capsaicin became the major capsaicinoid as the concentration of dihydrocapsaicin fell slightly. The time of harvest of Peter pepper based on the total capsaicinoids content should be performed as late as possible. In any case, harvesting should be performed before overripening of the fruit is observed.

The ontogenetic variation of total and individual capsaicinoids (nordihydrocapsaicin (n-DHC), capsaicin (C), dihydrocapsaicin (DHC), homocapsaicin (h-C) and homodihydrocapsaicin (h-DHC)) present in Malagueta pepper (Capsicum frutescens) during fruit ripening has been studied. Malagueta peppers were grown in a greenhouse under controlled temperature and humidity conditions. Capsaicinoids were extracted using ultrasound-assisted extraction (UAE) and the extracts were analyzed by ultra-performance liquid chromatography (UHPLC) with fluorescence detection. A significant increase in the total content of capsaicinoids was observed in the early days (between 12 and 33). Between day 33 and 40 there was a slight reduction in the total capsaicinoid content (3.3% decrease). C was the major capsaicinoid, followed by DHC, n-DHC, h-C and h-DHC. By considering the evolution of standardized values of the capsaicinoids it was verified that n-DHC, DHC and h-DHC (dihydrocapsaicin-like capsaicinoids) present a similar behavior pattern, while h-C and C (capsaicin-like capsaicinoids) show different evolution patterns. Published