Isolation, characterization and response surface method optimization of cellulose from hybridized agricultural wastes.

This study explores the utilization of eight readily available agricultural waste varieties in Nigeria-sugarcane bagasse, corn husk, corn cob, wheat husk, melina, acacia, mahogany, and ironwood sawdust-as potential sources of cellulose. Gravimetric analysis was employed to assess the cellulose content of these wastes, following which two selected wastes were combined based on their cellulose content and abundance to serve as the raw material for the extraction process. Response Surface Methodology, including Box-Behnken design, was applied to enhance control over variables, establish an optimal starting point, and determine the most favorable reaction conditions. The cellulose extracted under various conditions was comprehensively examined for content, structure, extent of crystallinity, and morphological properties. Characterization techniques such as X-ray Diffraction, Scanning Electron Microscopy, and Fourier Transform Infrared Spectroscopy were employed for detailed analysis. Compositional analysis revealed sugarcane bagasse and corn cob to possess the highest cellulose content, at 41 ± 0.41% and 40 ± 0.32% respectively, with FTIR analysis confirming relatively low C=C bond intensity in these samples. RSM optimization indicated a potential 46% isolated yield from a hybrid composition of sugarcane bagasse and corn cob at NaOH concentration of 2%, temperature of 45 °C, and 10 ml of 38% H2O2. However, FTIR analyses revealed the persistence of non-cellulosic materials in this sample. Further analysis demonstrated that cellulose isolated at NaOH concentration of 10%, temperature of 70 °C, and 20 ml of 38% H2O2 was of high purity, with a yield of 42%. Numerical optimization within this extraction condition range predicted a yield of 45.6% at NaOH concentration of 5%, temperature of 45 °C, and 20 ml of 38% H2O2. Model validation confirmed an actual yield of 43.9% at this condition, aligning closely with the predicted value. These findings underscore the significant potential of combinning and utilizing agricultural wastes as a valuable source of cellulose, paving the way for sustainable and resource-efficient practices in various industrial applications.

Optimization of emulsification conditions with rice bran concentrates for the preliminary formulation of potential vegan dressings and their characterization.

A fraction of rice bran (RB), generated during the brown rice polishing, is utilized to extract oil, resulting in defatted RB (DRB). The aim of this study was to optimize the emulsification conditions to enhance the value of this byproduct by formulating potential vegan dressings and characterizing them. Enzymatic hydrolysis of the starch present in DRB yields the DRB concentrate (DRBC). A central composite design was applied and the results were analyzed using response surface methodology to select optimal conditions for an oil-in-water emulsion formula. Two formulations were chosen: one corresponds to the optimal conditions, with 26.5% of oil and 73.5% of DRBC dispersion (eoptimal), and the other one with 21.7% of oil and 78.3% of dispersion (eED8). The eoptimal formulation exhibited significantly lower mean De Brouckere diameter (D4,3) value and higher viscosity when compared with eED8. For both emulsions, the particle size distribution and D4,3 remained unchanged during storage, whereas viscosity decreased, and backscattering (BS) increased. Initially, both emulsions exhibited solid viscoelastic behavior, which was partially lost during quiescent storage. The increase in BS was attributed to particle disaggregation, ultimately leading to the aforementioned change in rheological behavior. In conclusion, although the designed emulsions underwent microstructural changes, they were stable against gravitational separation. To improve stability during quiescent storage, it is suggested to incorporate a thickening agent. Hence, it is propose to procced with the development of a vegan dressing based on the eoptimal emulsion, as it exhibits superior physicochemical properties.

HSPiP and QbD Program-Based Analytical Method Development and Validation to Quantify Ketoconazole in Dermatokinetic Study.

Ketoconazole (KTZ) is the most potential azole anti-mycotic drug. The quantification of KTZ from various layers of the skin after topical application of lipidic nanocarriers is critical. We addressed a sensitive, specific, simple, rapid, reproducible, and economic analytical method to quantify KTZ from the treated skin homogenate using the Hansen solubility parameter (HSP, HSPiP software)-based modeling and experimental design. The software provided various HSP values for KTZ and solvents to compose the mobile phase. The Taguchi model identified the significant sets of factors to develop a robust bioanalytical method with reduced variability. In the optimization, acetonitrile (ACN) concentration (X1 as A) and the pH of mobile phase (X2 as B) were two factors against two responses (Y1: peak area and Y2: retention time). The HPLC (high-performance liquid chromatography) method validation was carried out based on US-FDA guidelines for the developed KTZ formulations (suspension, solid nanoparticles, and commercial product) extracted from the treated rat skin. The experimental solubility of KTZ was found to be maximum in the two solvents (ACN and ethyl acetate), based on HSP values. Surface response methodology (SRM) identified remarkable impact of ACN concentration and the mobile phase pH on the peak area and retention time. Analytical limits (0.17 and 0.50 µg/mL) were established for KTZ-SLNs (extracted from the skin). The method was implemented with high reproducibility, accuracy, and selectivity to quantify KTZ from the treated rat skin.

Response surface optimization of chemical coagulation for solid-liquid separation of dairy manure slurry through Box-Behnken design with desirability function.

Discharging livestock manure slurry without proper treatment causes various environmental and sociological problems. Chemical coagulation is a widely used and easily applicable method for treating such wastewater. However, the technique requires optimization to enhance coagulation efficiency while minimizing chemical usage. In this study, we propose an efficient, low-cost, and environmentally safe chemical coagulation method for solid-liquid separation of dairy manure slurry. Experiments were conducted in laboratory jar tests using dairy manure slurry to investigate the impact of coagulants, specifically polyaluminum chloride (PAC) and cationic polyacrylamide (CPAM), as well as pH, on the process of solid-liquid separation. Preliminary ranges of PAC, CPAM, and pH were estimated through single-factor experiments. Coagulation optimization and modeling were performed using the response surface methodology (RSM) with the Box-Behnken design (BBD), wherein the desired goal of each parameter was set to maximize solid-liquid separation efficiency while reducing chemical dosage to maintain residual aluminum (Al) concentrations below water quality standards. Numerical optimization predicted that the optimal dosages were 75 mg/L of PAC and 35 mg/L of CPAM at pH 7. Under these conditions, removal efficiencies of 99% for turbidity and 97% for chemical oxygen demand (COD) were achieved, with a minimal residual Al concentration of 0.045 mg/L. Positive zeta potential values in the treated water confirmed complete separation of negatively charged solids in the dairy manure slurry. The response values predicted by BBD aligned with the experimental results, and the analysis of variance (ANOVA) demonstrated the predictability and accuracy of the response models. Consequently, this study highlights the practical application of RSM with BBD in optimizing chemical coagulation using PAC and CPAM to achieve efficient solid-liquid separation in livestock wastewater while maintaining low residual Al concentrations.

Inoculum-to-substrate ratio and solid content effects over in natura spent coffee grounds anaerobic digestion.

Coffee is the second most traded commodity worldwide, and its production is associated with the generation of a large number of residues, which are underused and disposed of in landfills. Notably, the coffee industry annually generates approximately 6 million tons of industrial spent coffee ground (ISCG) when extracting coffee flavorings to produce soluble coffee. That resource loss scenario has been highlighted in sustainable waste management contexts as an opportunity to improve the coffee circular economy. Despite ISCG bioconversion to methane potentially meets the waste-to-energy purposes of reducing residues disposal in landfills, decreasing greenhouse gas (GHG) emissions, and increasing renewable energy sources, data about anaerobic digestion (AD) of ISCG remains quite restricted. That limitation becomes more apparent owing to the lack of data focusing on AD key parameters for ISCG as substrate. This study assessed the influence of inoculum-to-substrate ratio (ISR) and the solid content influences on mesophilic (37 °C) ISCG-AD throughout the Response Surface Methodology (RSM) and Central Composite Design (CCD). Results revealed that both factors, ISR and solid content, should be kept above a certain threshold of 0.5 and 6.0 gTVS L-1 to ensure experimental reliability, as well as reproductively and above 1.0 and 8.0 gTVS L-1 to avoid underestimation on the MY potential achieved. Concerning ISCG-AD kinetics, the quadratic model optimum condition was at 1.36 and 14.83 gTVS L-1 for ISR and solid content, respectively. This optimum range for ISR and solid content could guide further development of process configurations for mono- and co-digestion of ISCG, avoiding underestimation of the MY potential and extended incubation periods.

Optimisation of Operational Conditions during the Production of Arthrospira platensis Using Pilot-Scale Raceway Reactors, Protein Extraction, and Assessment of their Techno-Functional Properties.

The aim of the present study was to identify the optimum combination of dilution rate and depth of the culture to maximise the Arthrospira platensis BEA005B (Spirulina) productivity using 80 m2 raceway reactors. By varying these two main operational conditions, the areal biomass productivity of the reactors varied by over 55%. The optimum combination, optimised using a surface response methodology, was a depth of 0.10 m and a dilution rate of 0.33 day-1, which led to a biomass productivity of 30.2 g·m-2·day-1 on a dry weight basis when operating the reactors in semi-continuous mode. The composition of the produced biomass was 62.2% proteins, 42.5% carbohydrates, 11.6% ashes, and 8.1% lipids. The isolated proteins contained all the essential amino acids (except for tryptophan, which was not determined); highlighting the content of valine (6.8%), histidine (8.3%), and lysine (7.5%). The functional properties of the proteins were also assessed, demonstrating huge potential for their use in the development of innovative and sustainable foods.

Synthesis of BiOI/Mordenite Composites for Photocatalytic Treatment of Organic Pollutants Present in Agro-Industrial Wastewater.

Recently, bismuth oxyiodide (BiOI) is an attractive semiconductor to use in heterogeneous photocatalysis processes. Unfortunately, BiOI individually shows limited photocatalytic efficiency, instability, and a quick recombination of electron/holes. Considering the practical application of this semiconductor, some studies show that synthetic zeolites provide good support for this photocatalyst. This support material permits a better photocatalytic efficiency because it prevents the quick recombination of photogenerated pairs. However, the optimal conditions (time and temperature) to obtain composites (BiOI/ synthetic zeolite) with high photocatalytic efficiency using a coprecipitation-solvothermal growth method have not yet been reported. In this study, a response surface methodology (RSM) based on a central composite design (CCD) was applied to optimize the synthesis conditions of BiOI/mordenite composites. For this purpose, eleven BiOI/mordenite composites were synthesized using a combined coprecipitation-solvothermal method under different time and temperature conditions. The photocatalytic activities of the synthesized composites were evaluated after 20 min of photocatalytic oxidation of caffeic acid, a typical organic pollutant found in agro-industrial wastewater. Moreover, BiOI/mordenite composites with the highest and lowest photocatalytic activity were physically and chemically characterized using nitrogen adsorption isotherms, scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and diffuse reflectance spectroscopy (DRS). The optimal synthesis conditions prove to be 187 °C and 9 h. In addition, the changes applied to the experimental conditions led to surface property modifications that influenced the photocatalytic degradation efficiency of the BiOI/mordenite composite toward caffeic acid photodegradation.

Evaluation of Plant-Based Byproducts as Green Fining Agents for Precision Winemaking.

Consumers are increasingly looking for foods, including wine, that are free of animal-derived proteins. This study seeks to evaluate patatin, a new, plant-based and allergen-free fining agent, by comparing it with the fining agents polyvinipolypyrrolidone, bovine serum albumin, and methylcellulose. Specifically, its effects on the phenolic profile of enological tannins were analyzed with four spectrophotometric assays: OD 280 nm, Folin−Ciocâlteu, Adams−Harbertson, and methylcellulose. In addition, changes in the polyphenol composition of Sangiovese red wine were determined by UV-Vis spectrophotometry and HPLC with adsorption trials, and the solid−liquid interaction in a wine solution was modeled by both Langmuir and Freundlich equations. Our findings highlight the occurrence of systematic proportional error between the selected spectrophotometric assays. As a result, direct comparisons of protein precipitation assays can be made only among results obtained with the same spectrophotometric method. However, it is clear that patatin has an impact on the phenolic profile of Sangiovese red wine: it removes simple phenolics (gallic acid, (+)-catechin, (−)-epicatechin, epicatechin gallate, syringic acid, fertaric acid, coutaric acid, and rutin) as well as both oligomeric and polymeric tannins to different extents. In concentrations of less than 1 g/L, the patatin isotherm showed a linear relation between the equilibrium concentration and the quantity absorbed, obeying the Freundlich model reasonably well (KF 1.46; 1/n 1.07; R2 0.996 with 1/n > 1). Thus, the adsorption process is strongly dependent on the fining dosage.

Optimization of the Physical, Optical and Mechanical Properties of Composite Edible Films of Gelatin, Whey Protein and Chitosan.

The aim of this work was to evaluate the effect of the concentration of gelatin (G) (3-6 g), whey protein (W) (2.5-7.5 g) and chitosan (C) (0.5-2.5 g) on the physical, optical and mechanical properties of composite edible films (CEFs) using the response surface methodology (RSM), as well as optimizing the formulation for the packaging of foods. The results of the study were evaluated via first- and second-order multiple regression analysis to obtain the determination coefficient values with a good fit (R ˃ 0.90) for each of the response variables, except for the values of solubility and b*. The individual linear effect of the independent variables (the concentrations of gelatin, whey protein and chitosan) significantly affected (p ≤ 0.05) the water vapor permeability (WVP), strength and solubility of the edible films. The WVP of the edible films varied from 0.90 to 1.62 × 10-11 g.m/Pa.s.m2, the resistance to traction varied from 0.47 MPa to 3.03 MPa and the solubility varied from 51.06% to 87%. The optimized values indicated that the CEF prepared with a quantity of 4 g, 5 g and 3 g of gelatin, whey protein and chitosan, respectively, provided the CEF with a smooth, continuous and transparent surface, with L values that resulted in a light-yellow hue, a lower WVP, a maximum strength (resistance to traction) and a lower solubility. The results revealed that the optimized formulation of the CEF of G-W-C allowed a good validation of the prediction model and could be applied, in an effective manner, to the food packaging industry, which could help in mitigating the environmental issues associated with synthetic packaging materials.

Mycotoxins in food: a review on liquid chromatographic methods coupled to mass spectrometry and their experimental designs.

The development of a multi-mycotoxins method using LC-MS/MS is necessary and it is clear that the development of such method involves many compromises in the choice of the different parameters. This review summarizes applications using conventional experimental designs and some recent studies using response surface methodology (RSM) as a mathematical modeling tool for the optimization of extraction procedures. The authors also discuss pros and cons of the different procedures. To our knowledge, it is the first review on experimental design for the development of multi-mycotoxin methods. This review could be useful in the development and optimization of LC-MS/MS methods with the aim of describing experimental design and variables (factors) that are likely to affect sensitivity and specificity.

Synthesis of Fe3O4@mZrO2-Re (Re = Y/La/Ce) by Using Uniform Design, Surface Response Methodology, and Orthogonal Design & Its Application for As3+ and As5+ Removal.

In this study, iron oxide (Fe3O4) was coated with ZrO2, and doped with three rare earth elements((Y/La/Ce), and a multi-staged rare earth doped zirconia adsorbent was prepared by using uniform design U14, Response Surface methodology, and orthogonal design, to remove As3+ and As5+ from the aqueous solution. Based on the results of TEM, EDS, XRD, FTIR, and N2-adsorption desorption test, the best molar ratio of Fe3O4:TMAOH:Zirconium butoxide:Y:La:Ce was selected as 1:12:11:1:0.02:0.08. The specific surface area and porosity was 263 m2/g, and 0.156 cm3/g, respectively. The isothermal curves and fitting equation parameters show that Langmuir model, and Redlich Peterson model fitted well. As per calculations of the Langmuir model, the highest adsorption capacities for As3+ and As5+ ions were recorded as 68.33 mg/g, 84.23 mg/g, respectively. The fitting curves and equations of the kinetic models favors the quasi second order kinetic model. Material regeneration was very effective, and even in the last cycle the regeneration capacities of both As3+ and As5+ were 75.15%, and 77.59%, respectively. Adsorption and regeneration results suggest that adsorbent has easy synthesis method, and reusable, so it can be used as a potential adsorbent for the removal of arsenic from aqueous solution.

Functional beverage design based on fresh milk, tarwi (Lupinus mutabilis) beverage and oatmeal (Avena sativa)

ABSTRACT The tarwi is an Andean legume with a high nutritional value from which a vegetable beverage can be obtained. Cereals, like oat, have good characteristics as a prebiotic for the production of functional drinks, whose consumption is currently increasing. The objective of the research was to design a probiotic fermented beverage based on fresh milk, tarwi beverage, and oatmeal. An optimal treatment consisted of 1.9% oatmeal, 39.9% tarwi beverage, 46.2% fresh milk, 10.0% honey, and 2.0% probiotic culture; determined by applying a rotatable central composite design of surface response methodology. It had a probiotic count of 3.47x108 cfu/mL, a protein content of 3.75%, and overall acceptability of 7 points, which corresponds to "I like it very much". The result was experimentally validated. Likewise, the shelf life of the optimal beverage was 20 days at 5 °C with appropriate functional, nutritional, and sensory characteristics.

RESUMEN El tarwi es una leguminosa andina con un alto valor nutricional a partir de la cual se puede obtener una bebida vegetal, los cereales como la avena tienen mejores características como prebióticos para la producción de bebidas funcionales, cuyo consumo está aumentando actualmente. El objetivo de la investigación fue diseñar la formulación de una bebida fermentada probiótica a base de leche fresca, bebida de tarwi y avena. Se determinó un tratamiento óptimo que consistió en 1,9% de avena, 39,9% de bebida de tarwi, 46,2% de leche fresca, 10,0% de miel y 2,0% de cultivo probiótico; mediante la aplicación de un diseño compuesto central rotable de metodología de respuesta de superficie. Se reportó un recuento de probióticos de 3,47x108 ufc/mL, un contenido de proteínas de 3,8% y una aceptabilidad general de 7 puntos, que corresponde a "Me gusta mucho"; el resultado fue validado experimentalmente. Asimismo, la vida útil de la bebida óptima fue de 20 días de almacenamiento a 5 °C con características funcionales, nutricionales y sensoriales apropiadas.

Degradation of Styrenic Plastics during Recycling: Accommodation of PP within ABS after WEEE Plastics Imperfect Sorting.

With the development of dark polymers for industrial sorting technologies, economically profitable recycling of plastics from Waste Electrical and Electronical Equipment (WEEE) can be envisaged even in the presence of residual impurities. In ABS extracted from WEEE, PP is expected to be the more detrimental because of its important lack of compatibility. Hence, PP was incorporated to ABS at different rates (2 to 8 wt%) with a twin-screw extruder. PP was shown to exhibit a nodular morphology with an average diameter around 1-2 µm. Tensile properties were importantly diminished beyond 4 wt% but impact resistance was decreased even at 2 wt%. Both properties were strongly reduced as function of the contamination rate. Various potential compatibilizers for the ABS + 4 wt% PP system were evaluated: PPH-g-MA, PPC-g-MA, ABS-g-MA, TPE-g-MA, SEBS and PP-g-SAN. SEBS was found the most promising, leading to diminution of nodule sizes and also acting as an impact modifier. Finally, a Design Of Experiments using the Response Surface Methodology (DOE-RSM) was applied to visualize the impacts and interactions of extrusion temperature and screw speed on impact resistance of compatibilized and uncompatibilized ABS + 4 wt% PP systems. Resilience improvements were obtained for the uncompatibilized system and interactions between extrusion parameters and compatibilizers were noticed.

Microwave-Assisted Extraction of Curcuma longa L. Oil: Optimization, Chemical Structure and Composition, Antioxidant Activity and Comparison with Conventional Soxhlet Extraction.

Curcuma root (Curcuma longa L.) is a very important plant in gastronomy and medicine for its unique antiseptic, anti-inflammatory, antimicrobial and antioxidant properties. Conventional methods for the extraction of curcuma oil require long extraction times and high temperatures that can degrade the active substances. Therefore, the objectives of the present study were: (i) first, to optimize the extraction yield of curcuma oil by applying a Box-Behnken experimental design using surface response methodology to the microwave-assisted extraction (MAE) technique (the independent variables studied were reaction time (10-30 min), microwave power (150-200 W) and curcuma powder/ethanol ratio (1:5-1:20; w/v); and, (ii) second, to assess the total phenolic content (TPC) and their antioxidant activity of the oil (at the optimum conditions point) and compare with the conventional Soxhlet technique. The optimum conditions for the MAE were found to be 29.99 min, 160 W and 1:20 w/v to obtain an optimum yield of 10.32%. Interestingly, the oil extracted by microwave-assisted extraction showed higher TPC and better antioxidant properties than the oil extracted with conventional Soxhlet technique. Thus, it was demonstrated that the method applied for extraction influences the final properties of the extracted Curcuma longa L. oil.

Synthesis of magnetic core-shell amino adsorbent by using uniform design and response surface analysis (RSM) and its application for the removal of Cu2+, Zn2+, and Pb2.

The magnetic Fe3O4 was synthesized by using a one-step solvothermal method. Then, anhydrous ethanol as a solvent, tetramethyl ammonium hydroxide (TMAOH) as an auxiliary agent, tetraethyl orthosilicate (TEOS) as a silicon source, and (3-aminopropyl) triethoxysilane (APTES) as amino source were used to prepare Fe3O4@mSiO2-NH2 by using the sol-gel method. Uniform design U14*(145) and the response surface method (RSM) were used to optimize the synthesis ratio. According to the results of TEM, SEM, N2 adsorption-desorption test, VSM, and XRD, it found that the best coating effect obtained when the relative molar ratio of TMAOH:TEOS:APTES:Fe3O4 was 5:4:6:0.45. The results of EDS and elemental analysis confirmed the success of amino group coating; VSM magnetization after surface modification was 32 emu/g; BET results show that specific surface area is 236 m2/g, size 5 nm, and the pore volume is 0.126 cm3/g. The removal of Cu2+, Zn2+, and Pb2+ by Fe3O4@mSiO2-NH2 was studied at the optimal initial pH value 6 of the adsorption test system. The isothermal adsorption results show that the Langmuir model and Redlich-Peterson model are more suitable than the Freundlich model to describe the adsorption behavior, and Cu2+, Zn2+, and Pb2+ adsorption is mainly single molecular layer. The maximum adsorption capacity qm of the Langmuir model for Cu2+, Zn2+, and Pb2+ removal was 48.04 mg/g, 41.31 mg/g, and 62.17 mg/g, respectively. The adsorption kinetic rates of Cu2+, Zn2+, and Pb2+ on Fe3O4@mSiO2-NH2 relatively more suitable for pseudo-second-order kinetic model, i.e., R2, were ranged between 0.995 and 0.999, and the suitable reaction time was 60 min. These results proved that Fe3O4@m-SiO2-NH2 prepared by using this method is easy to synthesize, has easy recovery, is ecofriendly, and can be potential adsorbent for Cu2+, Zn2+, and Pb2+ removal.

Using a mixture design and fraction-based formulation to better understand perceptions of plant-protein-based solutions.

The food industry is focused on developing plant-based foods that incorporate pea protein isolates. However, these ingredients are often described as having persistent beany, bitter, and astringent notes, which can decrease the desirability of the resulting foods. These perceptions are rooted in the complex composition of volatile and non-volatile compounds in foods. The aim of our study was to better understand how the volatile and non-volatile fractions of pea protein isolates influence the perception of pea-protein-based foods. To this end, a mixture design was used. First, we obtained three fractions (the pellet, permeate, and retentate) from two pea protein isolates, resulting in a total of six fractions. Second, we used various combinations of the six fractions to create a set of 46 pea-protein-based solutions via various processes (solubilization, centrifugation, filtration, and mixing). Each fraction was specifically representative of the following constituent groups: insoluble proteins (the pellet); soluble compounds, such as volatiles, peptides, and phenolics (the permeate); and soluble proteins interacting with volatiles (the retentate). Factor levels were chosen with two aims: to explore the widest possible range of combinations and to realistically represent protein concentrations so as to build optimal mixture models. Third, 17 trained panelists were asked to score the attributes of the solutions using sensory profiling. Model performance was assessed using analysis of variance; results were significant for 18/18 attributes, and there was no significant lack-of-fit for 17/18 attributes. It was also assessed using the results of trials conducted with six supplementary solutions. These results clarified the origin of the perceived beany, bitter, and astringent notes. Beaniness was mainly influenced by the retentate and permeate fractions and was strongly affected by hexanal levels. Bitterness was mainly influenced by the retentate fraction, whereas astringency was influenced by the retentate and pellet fractions. Additionally, perception of these latter two attributes was affected by caffeic acid levels. This study has increased understanding of the relationship between pea protein fractions and the undesirable sensory attributes of pea protein isolates. It has also revealed how fraction-based formulation could be used to reduce the beaniness, bitterness, and astringency of pea-protein-based foods.

Use of New Glycerol-Based Dendrimers for Essential Oils Encapsulation: Optimization of Stirring Time and Rate Using a Plackett-Burman Design and a Surface Response Methodology.

Essential oils are used in an increasing number of applications including biopesticides. Their volatility minimizes the risk of residue but can also be a constraint if the release is rapid and uncontrolled. Solutions allowing the encapsulation of essential oils are therefore strongly researched. In this study, essential oils encapsulation was carried out within dendrimers to control their volatility. Indeed, a spontaneous complexation occurs in a solution of dendrimers with essential oils which maintains it longer. Six parameters (temperature, stirring rate, relative concentration, solvent volume, stirring time, and pH) of this reaction has been optimized by two steps: first a screening of the parameters that influence the encapsulation with a Plackett-Burmann design the most followed by an optimization of those ones by a surface response methodology. In this study, two essential oils with herbicide properties were used: the essential oils of Cinnamomum zeylanicum Blume and Cymbopogon winterianus Jowitt; and four biosourced dendrimers: glycerodendrimers derived from polypropylenimine and polyamidoamine, a glyceroclikdendrimer, and a glyceroladendrimer. Meta-analysis of all Plackett-Burman assays determined that rate and stirring time were effective on the retention rate thereby these parameters were used for the surface response methodology part. Each combination gives a different optimum depending on the structure of these molecules.

Do Flavonoids from Durum Wheat Contribute to Its Bioactive Properties? A Prospective Study.

A clear gap with respect to the potential biological properties of wheat flavonoids exists in the available literature. This information is crucial for breeding programs aiming to produce new varieties presenting improved health benefits. Accordingly, advanced breeding lines of whole durum wheat were evaluated in this contribution. The highest recovery of phenolics was achieved using aqueous acetone (50:50, v/v), as verified by multi-response optimization, thus showing that phenolics could be largely underestimated by employing an inappropriate extraction. The concentration of derivatives of apigenin, the main phenolics present, ranged from 63.5 to 80.7%, as evaluated by LC-ESI-QTOF-MS. Phenolics from the breeding line 98 exhibited the highest ability in scavenging peroxyl radicals, reducing power as well as in terms of inhibition of pancreatic lipase activity, a key enzyme regulating the absorption of triacylglycerols. In contrast, none of the samples exhibited a significant anti-diabetic potential. Despite their high concentration compared to that of phenolic acids, results of this work do not support a significant antioxidant and pancreatic lipase inhibitory effect of durum wheat flavonoids. Therefore, breeding programs and animal and/or human trials related to the effect of durum wheat flavonoids on oxidative stress and absorption of triacylglycerols are discouraged at this point.

Optimization of ultrasonication curcumin-hydroxylated lecithin nanoemulsions using response surface methodology.

Ultrasonication technology was used to enhance the solubility and availability of lipophilic compounds as curcumin. This study aimed to know the optimal conditions to produce ultrasonication curcumin nanoemulsions stabilized with hydroxylated lecithin using response surface methodology and to evaluate some physical characteristics. Nanoemulsions were produced according to a Central Composite Face-center Design: surfactant oil ratio (SOR, 0.33-1.17), amplitude (A, 8-92%), and ultrasonication time (t, 2-18.4 min). Dynamic light scattering was used to measure the droplet size and polydispersity index of the nanoemulsions. Our results showed that a second-order polynomial function of amplitude and ultrasonication time model fitted well with the mean droplet size and polydispersity of the emulsions. Predicted droplet size was 122.2 nm and polydispersity index was 0.13 obtained at optimal conditions: SOR = 0.72, A = 92%, and t = 12 min. The nanoemulsions remained stable during 15 days of storage at 20 °C. Nanoemulsion remained stable to the aggregation in the pH range from 7.0 to 3.0, while the droplet size increased at lower pH values due to a loss of charge of the lecithin. Nanoemulsion applied in a sugar-beverage showed a yellow-green translucent color, showing better stability on the droplet size than the beverage with the coarse emulsion. Nanoemulsion could be used as a natural colorant in beverages.

Chitosan-caseinate-dextran ternary complex nanoparticles for potential oral delivery of astaxanthin with significantly improved bioactivity.

Astaxanthin (ASTX) has been reported as a potential therapeutic agent for hepatic fibrosis treatment. However, its therapeutic effect is limited due to low bioavailability and poor aqueous solubility. In this study, biopolymer-based nanoparticles were fabricated using stearic acid-chitosan conjugate (SA-CS) and sodium caseinate (NaCas) via ionic gelation. Its nanostructure was cross-linked using oxidized dextran (Odex) via Schiff base reaction. Concentration of cross-linker, cross-linking temperature and time were systematically optimized by response surface methodology (RSM) to achieve superior particulate properties and colloidal stability. The optimized nanoparticles exhibited a diameter of 120 nm with homogeneous size distribution. A good ASTX encapsulation capacity with up to 6% loading ratio and high encapsulation efficiency was obtained. The final ASTX concentration in nanoparticles was 140 µM. The aqueous dispersibility of encapsulated ASTX was greatly improved, which was confirmed by significantly increased ABTS radical scavenging capacity. Compared to the anti-fibrogenic effect of free ASTX in LX-2 cells, the encapsulated ASTX demonstrated dramatically enhanced cellular bioactivity, as evidenced by significantly lower TGFß1-induced fibrogenic gene (ACTA2 and COL1A1) expression level, as well as α-SMA and COL1A1 protein levels. This study suggests that the as-prepared biopolymer nanoparticles hold promising features as an oral delivery vehicle for lipophilic bioactives.