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There is a broad research interest in the search for alternatives to chemical additives for use as natural food preservatives. Although many natural compounds have biological in vitro properties evidenced, in situ studies are still scarce. This study evaluated the effect of oregano essential oil (OEO) and salt (NaCl) concentrations against Escherichia coli (ATCC 8739), in salad dressing, using the response surface methodology. The experiment included a 2 2 central composite rotatable design (CCRD) in a total of 11 formulations of salad dressings. Oregano essential oil was characterized by gas chromatography and salad dressings by ash, lipids, proteins and moisture. OEO was composed mainly by carvacrol (65.1%) and p-cymene (12.0%). Salad dressings showed similar chemical profiles. A mathematical model for the prediction of the antibacterial activity in salad dressing was obtained. The results revealed that the interaction between OEO and salt showed effect on the bacterial count. However, the effect of salt was negative suggesting that the highest NaCl concentrations decreases the bacterial count. Therefore, within the parameters studied, the use of OEO to control E. coli in salad dressing can be considered promising and allows reduction in the levels of salt to be incorporated in food., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

This study evaluated the effect of oat flour and milk protein on the functional properties and sensory acceptability of shelf stable high protein dairy beverages containing at least 0.75 g of oat-β-glucan per serving size. Formulations adjusted to levels of 1.50% to 2.30% oat flour and 2.50% to 4.00% milk protein isolate (MPI) were thermal processed in a rotary retort. The finished product exhibited good suspension stability (>80%). The increase of oat and MPI contents lead to nectar-like beverages (51 to 100 mPas). However, oat flour was the component showing the highest effect on the viscosity coefficient values of the beverages. Sensory evaluation indicated that formulations with less than 1.9% oat flour and 2.5% MPI (thin liquid, <50 mPas) were the most accepted. Mouthfeel (perceived thickness), sweetness and aftertaste had the most influence on overall liking of the beverages., Practical Application: Overall, this study comprises the development of a functional food product. Supplementation of beverages with fiber from oats is an innovative approach to stabilize high protein beverages. Ready to drink protein beverage formulations use gums to stabilize the product and provide a desirable mouthfeel. The levels of oat-β-glucan used in the beverage increased the thickness and meet the requirement of the FDA approved health claim for reduction of the cardiovascular disease risk (21 CFR 101.81)., (© 2018 Institute of Food Technologists®.)

Spent coffee grounds are waste material generated during coffee beverage preparation. This by-product disposal causes a negative environmental impact, in addition to the loss of a rich source of nutrients and bioactive compounds. A rotating central composition design was used to determine the optimal conditions for the bioactivity of phenolic compounds obtained after the solid state fermentation of spent coffee grounds by Bacillus clausii . To achieve this, temperature and fermentation time were varied according to the experimental design and the total phenolic and flavonoid content, antioxidant activity and antimicrobial activity were determined. Surface response methodology showed that optimum bioprocessing conditions were a temperature of 37 °C and a fermentation time of 39 h. Under these conditions, total phenolic and flavonoid contents increased by 36 and 13%, respectively, in fermented extracts as compared to non-fermented. In addition, the antioxidant activity was increased by 15% and higher antimicrobial activity was observed against Gram positive and negative bacteria. These data demonstrated that bioprocessing optimization of spent coffee grounds using the surface response methodology was an important tool to improve phenolic extraction, which could be used as an antioxidant and antimicrobial agents incorporated into different types of food products.

Response surface methodology (RSM) was applied to optimise the extraction of curcuminoids (curcumin, demethoxycurcumin and bisdemethoxycurcumin) from turmeric using ethyl lactate (EL), ethanol and water under mild conditions (magnetic stirring at room temperature). An augmented simplex-centroid mixture design was used to monitor the dependence of the extraction efficiency from the proportions of the three solvents in the extraction medium. HPLC was used to establish the content of curcuminoids in turmeric and in the extracts. Surface plots for the extracted amount of each curcuminoid covering the whole composition domain were generated by interpolation of the experimental data with quadratic canonical polynomial models. The response surfaces of the three curcuminoids are qualitatively similar and the maximum extraction efficiency was obtained with water-EL 30:70v/v that ensured the almost quantitative recovery of the three compounds from turmeric. While degradation of the three curcuminoids in water at moderate alkaline pH is relatively fast (half-times are between 0.23 and 8.5h at pH=8.6), their stability is noticeably greater in EL (half-times are within 21-69days). Addition of EL to water is also able to inhibit the alkaline hydrolysis of curcumin and its derivatives, their half-times in the water-EL 30:70v/v, being within 40-70h at pH=8.6. The above evidences suggest that EL is a promising solvent for the extraction of curcuminods from turmeric and a suitable medium for vehiculation of these compounds into drugs or foods., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Sodium methoxide (CH 3 ONa) with glycerol pretreatment (CWGP) was performed to improve the enzymatic digestibility of sugarcane bagasse (SCB). Response surface methodology was utilized to optimize the CWGP parameters for pretreating SCB from the perspective of total fermentable sugar yield (TFSY) and total fermentable sugar concentration (TFSC). Under the optimal CWGP conditions, 0.5666g/g of TFSY (0.82% CH 3 ONa, 1.11h, 150°C) and 17.75g/L of TFSC (0.87% CH 3 ONa, 1.38h, 149.27°C) were achieved, corresponding to delignification of 79.05% and 79.34%, respectively. Compared the pretreatment using glycerol or CH 3 ONa alone, the CWGP has significant synergies to enhance the enzymatic efficiency of SCB. The physical and chemical characteristics of untreated and pretreated SCBs were analyzed using FT-IR, XRD, and SEM, and the results suggest that CWGP significantly increased the susceptibility of the substrates to enzymatic digestibility. Ultimately, CWGP might be a prospective candidate for the pretreatment process of enzyme-based lignocellulosic biorefineries., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

With the increasing awareness on the toxicity of several synthetic dyes, demand for pigments from natural sources, such as microbial carotenoids, has gained interest as a promising safe alternative colour additive. In this study, a surface response methodology based on the Doehlert distribution for two factors [% of glucose in a mixture of glucose + fructose (10 g/L total sugars), and sulfate concentration] was used towards the optimal carotenoids production by Gordonia alkanivorans strain 1B in the presence of light (400 lx). Time influence on pigment production by this bacterium was also evaluated, as well as the cell viability profile during longer incubation periods at optimal conditions. Indeed, the highest carotenoid production (2596-3100 μg/g DCW ) was obtained when strain 1B was cultivated in the optimal conditions: glucose 10 g/L and sulfate ≥ 22 mg/L, in the presence of light for 19 days at 30 °C, 150 rpm. Flow cytometry showed that the highest production was somehow related with the cellular stress. These results highlight the great potential of strain 1B as a new hyperpigment producer to be exploited towards several applications.

Bisphenol A (BPA) is an emerging contaminant of water resources that disrupts endocrine function. Attempts are continuing to develop cost-effective methods to remove BPA from water environments. The aim of this study was to prepare and characterize polysulfone/graphene oxide nano-composite membranes for removal of BPA from water. Three membranes were synthetized using phase inversion method: polysulfone membrane as PSF and two polysulfone/graphene oxide nano-composite membranes with graphene oxide (GO) weight ratios of 0.4 and 1.0% as PSF/GO 0.4% and PSF/GO 1.0%, respectively. The membrane characteristics including morphology, surface roughness, pore size, zeta potential and presence of functional groups were determined using field emission scanning electron microscopy, atomic force microscopy, streaming potential, and attenuated total reflectance Fourier transform infrared spectroscopy techniques. Inclusion of GO remarkably increased permeate flux of the membranes, so that pure water flux of PSF, PSF/GO 0.4% and PSF/GO 1.0% at operating pressure of 2 bar was determined 226, 449 and 512 L/m 2  h, respectively. The membrane PSF/GO 0.4% with the most negative zeta potential (-10.46 mV) and the highest BPA removal efficiency was determined as the optimal membrane. The optimum conditions of input pressure, operating time, initial concentration of BPA, and pH for BPA removal efficiency by PSF/GO 0.4% were determined using surface response methodology to be 1.02 bar, 10.6 min, 7.5 mg/L, and 5.5, respectively. By optimizing the conditions of operating parameters, experimental BPA removal efficiency by PSF/GO 0.4% reached to as high as 93%., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Although Azospirillum strains used in commercial inoculant formulations presents diazotrophic activity, it has been reported that their ability to produce phytohormones plays a pivotal role in plant growth-promotion, leading to a general recommendation of its use in association with regular N-fertilizer doses. In addition, a high variability in the effectiveness of Azospirillum inoculants is still reported under field conditions, contributing to the adoption of the inoculation technology as an additional management practice rather than its use as an alternative practice to the use of chemical inputs in agriculture. To investigate whether the content of stress-resistance biopolymers would improve the viability and performance of Azospirillum inoculants when used as substitute of N-fertilizers, biomass of A. brasilense strain Ab-V5 enriched in exopolysaccharides (EPS) and polyhydroxybutirate (PHB) was produced using a new culture medium developed by factorial mixture design, and the effectiveness of resulting inoculants was evaluated under field conditions. The culture medium formulation extended the log phase of A. brasilense cultures, which presented higher cell counts and increased EPS and PHB contents than observed in the cultures grown in the OAB medium used as control. An inoculation trial with maize conducted under greenhouse conditions and using the biopolymers-enriched Ab-V5 cells demonstrated the importance of EPS and PHB to the long term bacterial viability in soil and to the effectiveness of inoculation. The effectiveness of liquid and peat inoculants prepared with Ab-V5 cells enriched with EPS and PHB was also evaluated under field conditions, using maize as target crop along different seasons, with the inoculants applied directly over seeds or at topdressing under limiting levels of N-fertilization. No additive effect on yield resulted from inoculation under high N fertilizer input, while inoculated plants grown under 80% reduction in N fertilizer showed yields at levels compared to fully fertilized plants, regardless the inoculation method. The presented data highlights the feasibility to partially substitute the N-fertilizer demand in non-legume crops using high-quality inoculant formulations, prepared with diazotrophic bacteria enriched with stress-resistance biopolymers that confer increased viability an effectiveness to the bacterial cells.

Sodium hydroxide pretreatment of sugarcane bagasse under vacuum conditions was established and evaluated in this study. Compared to pretreatment under conventional moderate pressure conditions, only half of the total phenolic compounds and less than half of the formic acid were produced under vacuum conditions, while the yield of total fermentable sugar was significantly increased by 31.38%. The pretreatment parameters: NaOH concentration, pretreatment time, and pretreatment temperature, were optimized using response surface methodology based on the response values of the total fermentable sugar yield (TFSY) and the total fermentable sugar concentration (TFSC), respectively. Under the optimal conditions, the TFSY of 0.5146g/g and the TFSC of 17.37g/L were achieved, respectively. By adjusting the ratio of cellulases to xylanase, the TFSY reached a maximum of 0.5213g/g when the ratio was 1:1, while the maximum TFSC of 17.71g/L was achieved when the ratio was 1:4., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Microencapsulation techniques have been intensively explored by many research sectors such as pharmaceutical and food industries. Microencapsulation allows to protect the active ingredient from the external environment, mask undesired flavours, a possible controlled release of compounds among others. The purpose of this review is to provide a background of design of experiments in microencapsulation research context. Optimization processes are required for an accurate research in these fields and therefore, the right implementation of micro-sized techniques at industrial scale. This article critically reviews the use of the response surface methodologies in pharmaceutical and food microencapsulation research areas. A survey of optimization procedures in the literature, in the last few years is also presented., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Aim: A micellar liquid chromatographic method to determine several anticancer drugs (pazopanib, dabrafenib and regorafenib) in plasma was developed and validated by the guidelines of the EMA., Experimental: Plasma samples were directly injected, after a 1/5-dilution in a micellar solution. The drugs were resolved in <18 min using a C18 column. The mobile phase was an aqueous solution of 0.12 M SDS - 2% 1-pentanol, buffered at pH 7. The detection was performed by absorbance at 260 nm., Results: The values of the main validation parameters were: LOD (0.1-1 mg/l), calibration range (0.2-2 to 80 mg/l), accuracy (-12.5 to +11.7%) and precision (<11.9%)., Conclusion: The procedure was conducted by minimum cost, effort, manipulation, time and quantity of hazardous chemicals. The method was useful to determine the drugs at their respective target concentrations, and was found useful for clinical analysis.

Optimization of microwave-assisted extraction (MAE) of water-soluble pectin (WSP) from Opuntia ficus indica cladodes was performed using Response Surface Methodology. The effect of extraction time (X 1 ), microwave power (X 2 ), pH (X 3 ) and solid-to-liquid ratio (X 4 ) on the extraction yield was examined. The optimum conditions of MAE were as follows: X 1 =2.15min; X 2 =517W; X 3 =2.26 and X 4 =2g/30.6mL. The maximum obtained yield of pectin extraction was 12.57%. Total carbohydrate content of WSP is about 95.5% including 34.4% of Galacturonic acid. Pectin-related proteins represent only the 0.66% of WSP mass. HPSEC and light scattering analyses reveal that WSP is mostly constituted of high molecular pectin and FTIR measurements show that the microwave treatment does not alter the chemical structure of WSP, in which Galacturonic acid content and yield are 34.4% and 4.33%, respectively. Overall, application of MAE can give rise to high quality pectin., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Background: Abstract: The objective of the present work was to prepare and optimize the loteprednoletabonate (LE) loaded poly (D,L-lactide co-glycolide) (PLGA) polymer based nanoparticle carrier. The review on recent patents (US9006241, US20130224302A1, US2012/0028947A1) assisted in the selection of drug and polymer for designing nanoparticles for ocular delivery applications., Methods: The nanoparticles were prepared by solvent evaporation followed by high speed homogenization. Biodegradable polymer PLGA (50:50) grade was utilized to develop various formulations with different drug:polymer ratio. A Box-Behnken design with 33 factorial design was selected for the present study and 17 runs were carried out in totality. The influence of various process variables (viz., polymer concentration, homogenization speed and sonication time) on the characteristics of nanoparticles including the in vitro drug release profile were studied., Results: The nanoparticulate formulations were evaluated for mean spherical diameter, polydispersity index (PDI), zeta potential, surface morphology, drug entrapment and in-vitro drug release profile. The entrapment efficiency, drug loading and mean particle size were found to be 96.31±1.68 %, 35.46±0.35 % and 167.6±2.1 nm respectively., Conclusion: The investigated process and formulation variables were found to have significant effect on the particle size, drug loading (DL), entrapment efficiency (EE), and in vitro drug release profile. A biphasic in vitro drug release profile was apparent from the optimized nanoparticles (NPs) for 24 hours., (Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.)

Purpose: This work examines the relevance of viral activity in the optimization of spray drying process parameters for the development of thermally stable vaccine powders. In some instances, the actual active pharmaceutical ingredient (API) is not included in the process optimization as it is deemed too costly to use until the final selection of operating conditions, however, that approach is inappropriate for highly labile biopharmaceutics. We investigate the effects of spray drying parameters on i) yield, ii) particle size and iii) viral vector activity of a mannitol/dextran encapsulated recombinant human type 5 adenoviral vector vaccine, to demonstrate the effects and magnitude of each effect on the three responses, and further show that the API must be included earlier in the optimization., Methods: A design of experiments approach was used with response surface methodology (RSM) to optimize parameters including inlet temperature, spray gas flow rate, liquid feed rate and solute concentration in the feed., Results: In general, good conditions for maintaining viral activity led to reduced yield and fewer particles of the desired size. Within the range of parameters tested, the yield varied from 50 to 90%, the percentage of ideally size particles was 10-50%, and the viral vector titre loss was 0.25-4.0 log loss., Conclusions: RSM indicates that the most significant spray drying parameters are the inlet temperature and spray gas flow rate. It was not possible to optimize all three output variables with one set of parameters, indicating that there will only be one dominant criteria for processing which in the case of viral vaccines will likely be viral vector activity.

The evolution of zinc oxide nanostructures grown on graphene by alcohol-assisted ultrasonic spray pyrolysis was investigated. The evolution of structures is strongly depended on pyrolysis parameters, i.e., precursor molarity, precursor flow rate, precursor injection/deposition time, and substrate temperature. Field-effect scanning electron microscope analysis, energy dispersive X-ray spectroscopy, X-ray diffraction, and transmission electron microscopy were used to investigate the properties of the synthesized nanostructures and to provide evidence for the structural changes according to the changes in the pyrolysis parameters. The optimum parameters to achieve maximum density and well-defined hexagonally shaped nanorods were a precursor molarity of 0.2 M, an injection flow rate of 6 ml/min, an injection time of 10 min, and a substrate temperature of 250-355 °C. Based on the experimental results, the response surface methodology (RSM) was used to model and optimize the independent pyrolysis parameters using the Box-Behnken design. Here, the responses, i.e., the nanostructure density, size, and shape factor, are evaluated. All of the computations were performed using the Design-Expert software package. Analysis of variance (ANOVA) was used to evaluate the results of the model and to determine the significant values for the independent pyrolysis parameters. The evolution of zinc oxide (ZnO) structures are well explained by the developed modelling which confirms that RSM is a reliable tool for the modelling and optimization of the pyrolysis parameters and prediction of nanostructure sizes and shapes.

An efficient generic static headspace gas chromatography (HSGC) method was developed, optimized and validated for the routine determination of several residual solvents (RS) in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO) was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chromatograph from Agilent Model 6890 equipped with flame ionization detector (FID) and a DB-624 (30 m×0.53 mm i.d., 3.00 µm film thickness) column was used. The inlet split ratio was 5:1. The influencing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT), the final temperature (FT) of the oven and the carrier gas flow rate (F) were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were 30 °C for IT, 158 °C for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents through a comprehensive validation according to the ICH guidelines.

The objective of this present investigation was to develop and formulate floating sustained release matrix tablets of s (-) atenolol, by using different polymer combinations and filler, to optimize by using surface response methodology for different drug release variables and to evaluate the drug release pattern of the optimized product. Floating sustained release matrix tablets of various combinations were prepared with cellulose-based polymers: Hydroxypropyl methylcellulose, sodium bicarbonate as a gas generating agent, polyvinyl pyrrolidone as a binder and lactose monohydrate as filler. The 3(2) full factorial design was employed to investigate the effect of formulation variables on different properties of tablets applicable to floating lag time, buoyancy time, % drug release in 1 and 6 h (D1 h,D6 h) and time required to 90% drug release (t90%). Significance of result was analyzed using analysis of non variance and P < 0.05 was considered statistically significant. S (-) atenolol floating sustained release matrix tablets followed the Higuchi drug release kinetics that indicates the release of drug follows anomalous (non-Fickian) diffusion mechanism. The developed floating sustained release matrix tablet of improved efficacy can perform therapeutically better than a conventional tablet.

Background: The extraction method of bioactive compounds is an important step in the manufacturing of herbal medicines, because secondary metabolites with therapeutic potential are usually found in small quantities in plant materials., Objective: Due the potential of Apeiba tibourbou Aubl, this study aimed to evaluate the impact of the extraction method on the quality of herbal extract and optimize the extraction of fatty acid, rosmarinic (Ra) and caffeic (Ca) acid from A. tibourbou., Materials and Methods: Determinations of residual moisture (Rm), proteins (Pt), lipids (Lp), total fiber (Tf), and carbohydrate (Cy) were performed in triplicate samples according assessment of antioxidant capacity. Extraction of fatty acids was carried out by two different methods: (i) By shoxlet and (ii) bligh and dyer. The optimized conditions were determined by surface response methodology (RSM), and the criterion of desirability was the maximum extraction of Ra and Ca., Results: The method of bligh and dyer was able to extraction more total Lp than the shoxlet. However, the extraction of fatty acid was different for the two methods. The optimized conditions to extract RA and Ca was calculated by RSM, 42°C, 30% (alcohol degree) and 24 min, this conditions maximize simultaneously the extraction of Ca (0, 04%) and Ry (1.89)., Conclusion: It was observed that the extraction method alters the chemical composition of extract, and it is possible to extract Ca and Ra from A. tibourbou's leaves using ultrasound-assisted extraction.