Polyphenolic compounds with biological activity in guabiroba fruits (Campomanesia xanthocarpa Berg.) by comprehensive two-dimensional liquid chromatography.

This study aimed to evaluate the polyphenolic composition along with the biological activity of guabiroba (Campomanesia xanthocarpa Berg.) fruits using comprehensive two-dimensional liquid chromatography (LC × LC). A simplex centroid design comprising three solvents (methanol, 2% acetic acid, and acetonitrile) was used to optimize the extraction mixture for polyphenols from ripe and unripe guabiroba fruits. A quantitative LC × LC platform was proposed to characterize the guabiroba extracts using a RP-Amide column and a C18 column in the first and second dimensions, respectively. Antidiabetic properties, using in vitro enzyme assay models and in vivo antioxidant activity with the eukaryote model Saccharomyces cerevisiae, was measured. Total phenolics compounds were more efficiently extracted with 2% acetic acid solution and acetonitrile (50:50, v/v). A total of 37 different compounds were identified and quantified using the proposed LC × LC method (linearity ranging from 0.9990 to 0.9994, intra- and interday precision from 0.40 to 10.57% and, accuracy from 81.89 to 108.98%). Significant differences were observed between ripe and unripe guabiroba fruits, especially for the compounds geraldone and methyl galangin isomer. Guabiroba fruits showed significant antidiabetic and antioxidant properties and may be potentially adopted as part of dietary strategies in the management of early stages of type 2 diabetes and associated complications.

Statistical mixture design investigation for extraction and quantitation of aporphine alkaloids from the leaves of Unonopsis duckei R.E. Fr. by HPLC-MS/MS.

INTRODUCTION: Alkaloids-derived drugs are a billionaire world-market and several phytochemical investigations aim the identification of new sources and/or structures. Thus, improving the way of extracting and methods to quantify them are of utmost importance. OBJECTIVE: To quantify isoquinoline-derived alkaloids in Unonopsis duckei R.E. Fr. through a new validated high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) method in combination with a statistical mixture design that aimed a proper direct extraction of these compounds from leaves. METHODOLOGY: Extracts were obtained with acetone, methanol, chloroform, and n-hexane in different combinations and proportions. Chemometrics were applied in order to compare peak areas, and therefore evaluate synergism and antagonism effects between the solvents. After selection of extraction solvent, the quantification was validated and applied in the best solvent combination to quantify the main alkaloids in U. duckei. RESULTS: Chemometrics indicated a synergistic effect between chloroform and methanol solvents, thus improving alkaloid extraction and extract yield. Analytes were quantified in a 15-min method, with limits of detection (LODs) between 0.5 and 5.2 ng/mL and limits of quantification (LOQs) between 1.6 and 17.2 ng/mL. The accuracy ranged between 80 and 120%. Coefficients of variation were lower than 17.42% at all concentrations. Concentrations of the alkaloids in U. duckei varied from 6.79 to 131.10 µg/g of dried leaf and glaziovine was found to be the main compound. CONCLUSION: The integration of simplex centroid model and quantification by HPLC-MS/MS is promising. Statistical optimisation of the alkaloid extraction and application of selective, sensitive and robust HPLC-MS/MS method will contribute to quality control applications in phytotherapeutic medicines.

Application of multi-block analysis and mixture design with process variable for development of chocolate cake containing yacon (Smallanthus sonchifolius) and maca (Lepidium meyenii).

BACKGROUND: In this study, a chocolate cake formulation was developed with partial substitution of wheat flour by yacon and maca flour. A simplex-centroid design was applied to determine the proportions of the three flours, and the amount of water was included as a process variable at three distinct levels. According to the overall acceptability of the cakes, the tasters were separated into two groups using k-means. RESULTS: After segmentation, regression models were constructed for overall acceptability of each group; R2adjusted values of 92.5% for group 1 and 98.9% for group 2 were obtained. Using the sequential simplex method an optimized formulation was determined for group 1 (0.49 kgwheat kg-1total flour , 0.37 kgyacon kg-1total flour , 0.14 kgmaca kg-1total flour and 140.0 mL of water) and another for group 2 (0.35 kgwheat kg-1total flour , 0.65 kgyacon kg-1total flour and 120.0 mL of water). In addition to these formulations, a third formulation was proposed with a greater maca proportion (0.32 kgmaca kg-1total flour ), which does not significantly alter the overall acceptability of both groups. The three optimized formulations and two control formulations were evaluated through free-choice profiling. The data were evaluated using the multi-block method common components and specific weights analysis (CCSWA). CONCLUSION: It was observed that a greater proportion of maca intensified brownness and burnt aroma and taste, whereas a larger proportion of yacon produced a better appearance, softness, sweetness and chocolate flavor. © 2017 Society of Chemical Industry.

Advances in the Production of Sustainable Bacterial Nanocellulose from Banana Leaves.

Interest in bacterial nanocellulose (BNC) has grown due to its purity, mechanical properties, and biological compatibility. To address the need for alternative carbon sources in the industrial production of BNC, this study focuses on banana leaves, discarded during harvesting, as a valuable source. Banana midrib juice, rich in nutrients and reducing sugars, is identified as a potential carbon source. An optimal culture medium was designed using a simplex-centroid mixing design and evaluated in a 10 L bioreactor. Techniques such as Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), X-ray diffraction (XRD), and thermogravimetric analysis (TGA) were used to characterize the structural, thermal, and morphological properties of BNC. Banana midrib juice exhibited specific properties, such as pH (5.64), reducing sugars (15.97 g/L), Trolox (45.07 µM), °Brix (4.00), and antioxidant activity (71% DPPH). The model achieved a 99.97% R-adjusted yield of 6.82 g BNC/L. Physicochemical analyses revealed distinctive attributes associated with BNC. This approach optimizes BNC production and emphasizes the banana midrib as a circular solution for BNC production, promoting sustainability in banana farming and contributing to the sustainable development goals.

Optimized Solvents for the Maceration of Phenolic Antioxidants from Curcuma xanthorrhiza Rhizome using a Simplex Centroid Design.

Background: Curcuma xanthorrhiza Roxb., from the Zingiberaceae family, is a famous plant native to Indonesia that is highly effective in treating diseases due to the various chemical compounds it contains. Objective: This study aims to optimize the extraction process for the phenolic content, with its antioxidant activity, from the rhizome of C. xanthorrhiza using different solvent (water, acetone, methanol, and ethanol) systems based on the simplex centroid design using the Design Expert 13.0 program. Methods and Material: Total phenolic content (TPC) was analyzed by colorimetry using Follin-Ciocalteu, while the antioxidant activity was measured based on 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging and ferric reducing antioxidant power (FRAP) using a spectrophotometer. Results: To measure TPC and DPPH, a special cubic model was used; to measure FRAP, a linear model was utilized. Each model demonstrated a good match with the R2 values for TPC (0.9808), DPPH (0.9583), and FRAP (0.7872). The combination of a mixture of water (0.409), acetone (0.307), and methanol (0.284) with a desirability level of 0.723, resulted in a TPC of 34.112 mg gallic acid equivalent (GAE)/g dry weight (DW), DPPH of 26.533 µmol Trolox equivalent (TE)/g DW, and FRAP of 92.353 µmol TE/g DW. This showed a high extraction efficiency which was optimal. Conclusions: The best condition to extract the rhizomes of C. xanthorrhiza was a ternary combination of solvents including water, acetone, and methanol in the proportions of 0.409, 0.307, and 0.284, respectively, with a desirability level of 0.723.

Methylphenidate Fast Dissolving Films: Development, Optimization Using Simplex Centroid Design and In Vitro Characterization.

Objectives: The focus of this study was to design and optimize methylphenidate hydrochloride mouth dissolving film (MDF) that can be beneficial in an acute condition of attention deficit hyperactivity disorder (ADHD) and narcolepsy. Materials and Methods: Solvent casting method was used for the preparation of this film. Optimization of the effect of independent variables such as the number of polymers and active pharmaceutical ingredients [hydroxypropyl methyl cellulose (HPMC) E5, HPMC E15, and maltodextrin], % of drug release, disintegration time, and tensile strength of the film done using simplex centroid design. Complex formation of the film was tested using fourier-transform infrared spectroscopy and differential scanning calorimetry study. The multiple regression analysis was obtained from equations of the results that adequately describe influence of the independent variables on the selected responses. Polynomial regression analysis, contour plots, and 3-D surface plots were used to relate dependent and independent variables. Results: Experimental results indicated that different polymer amounts had complex effects on % drug release from the film, disintegration time as well as the tensile strength of the film. The observed responses were in near alignment with expected values calculated from the developed regression equations as shown by percentage relative error. Final formulation showed more than 95% drug release within 2 min and was shown to disintegrate within a minute that had good tensile strength. Conclusion: These findings suggest that MDF containing methylphenidate hydrochloride is likely to become a choice of methylphenidate hydrochloride preparations for treatment in ADHD and narcolepsy conditions.

Influence of organic acids on pentlandite bioleaching by Acidithiobacillus ferrooxidans LR.

Bioleaching is a bio-hydrometallurgical process of solubilizing metals from low-grade sulfide ores by microbial action employing chemolithoautotrophic microorganisms capable of promoting redox reactions. Organic acids have been applied in bioleaching once can act in two different ways; providing hydrogen ions for mineral acidolysis and complexing metals due to their chelating capacity. This study investigates the synergy of different organic acids (acetic, ascorbic, citric, lactic, and oxalic) and Acidithiobacillus ferrooxidans LR pentlandite bioleaching. The addition of oxalic acid had a positive effect on the Ni extraction during pentlandite biological-chemical leaching after 15 days, and the yields observed were 45.6% (26.5 mg Ni/g ore). The yields for Co extraction were meager, and Co extraction values were found to only 2.8% (1.6 mg Co/g ore) in the presence of citric acid. A design of experiments with mixtures was used to evaluate the interaction of organic acids in bioleaching. According to simplex-centroid experiments, only citric acid presented a statistically significant effect and has contributed in a synergistic form in pentlandite biological-chemical leaching in the presence of A. ferrooxidans. This study provides a new synergistic bioleaching system to improve Ni and Co extraction from sulfide ores.

Combination of Catechin, Epicatechin, and Rutin: Optimization of a novel complete antidiabetic formulation using a mixture design approach.

Nowadays, synthetic chemical antidiabetic drugs, besides their therapeutic effects, present adverse effects that could be hard to handle over time. In the last decade, studies reported new alternative molecules with more health benefits and less adverse effects. The goal of this study is to optimize a new antidiabetic formulation using plant flavonoids: Catechin, Epicatechin, and Rutin. They are also a powerful antioxidant and anti-inflammatory molecules. A mixture design experiment will optimize their combination to obtain a new, safe multi-targets antidiabetic formulation making it a powerful combination for the management of diabetes and its complications. To study the variation of blood glucose level in response to the treatment over the time we performed an Oral Glucose Tolerance Test. The blood glucose level variations recorded as responses for the mixture design experiment. We used the molecules at a dose of 10 mg/kg. According to the software analysis, the prediction profiler showed us the optimum combination, and the result was a binary combination between Rutin and Epicatechin (25% and 75%, respectively). This combination prevented hyperglycemia and hypoglycemia, along with the best area under the curve, and after that, we validated it through a repeated oral administration on alloxan-induced diabetic mice for 28 d. Rutin, Catechin, and Epicatechin exhibit a potent antihyperglycemic activity, their synergistic combination validates a new formulation that could be a real candidate to conventional drugs.

Effects of adding spices with antioxidants compounds in red ale style craft beer: A simplex-centroid mixture design approach.

The growing demand for authentic products that provide sensory characteristics combined with health benefits has been the focus of current studies. This study developed a Red Ale style craft beer with spices such as turmeric (T), black pepper (P) and aroma hops (H), used isolated or in mixtures. A mixture design was employed to evaluate the total phenolic compounds and the antioxidant activity in the green and aged beers formulations. The spice extracts influenced the product's shelf-life. The addition of spices into the beers did not affect the physicochemical parameters that classify the Red Ale style, according to the hierarchical cluster analysis, except for aroma hops. A multiresponse optimization approach simultaneously maximized the antioxidant activity and the phenolic compounds in beers. The ideal formulation obtained for green beers was 25% T and 37.5% P and H; for aged beers, the formulation was 50% T, 20% P and 30% H.

Recent Applications of Mixture Designs in Beverages, Foods, and Pharmaceutical Health: A Systematic Review and Meta-Analysis.

Design of Experiments (DoE) is a statistical tool used to plan and optimize experiments and is seen as a quality technology to achieve products excellence. Among the experimental designs (EDs), the mixture designs (MDs) stand out, being widely applied to improve conditions for processing, developing, or formulating novel products. This review aims to provide useful updated information on the capacity and diversity of MDs applications for the industry and scientific community in the areas of food, beverage, and pharmaceutical health. Recent works were selected following the Preferred Reporting Items for Systematic Review and Meta-Analyses statement (PRISMA) flow diagram. Data analysis was performed by self-organizing map (SOM) to check and understand which fields of application/countries/continents are using MDs. Overall, the SOM indicated that Brazil presented the largest number of works using MDs. Among the continents, America and Asia showed a predominance in applications with the same amount of work. Comparing the MDs application areas, the analysis indicated that works are prevalent in food and beverage science in the American continent, while in Asia, health science prevails. MDs were more used to develop functional/nutraceutical products and the formulation of drugs for several diseases. However, we briefly describe some promising research fields in that MDs can still be employed.