The present study utilized Analytical Quality by Design (AQbD) approach to develop a stability-indicating high-performance liquid chromatography (HPLC) method for estimating evogliptin tartrate using design expert software. The key parameters were methodically optimized, contours were plotted, and stability was evaluated using various forced degradation conditions. Using an Agilent HPLC system with a photo diode array (PDA) detector along with Fortis C18 column (250 × 4.6 mm, 5 μm) effectively separated the drug from its degradants. The mobile phase used was methanol: water (pH adjusted to 3.0, 76:24; v/v) at 0.8 mL/min flow rate. Evogliptin was eluted at 2.98 min, at a detection wavelength of 267 nm. The proposed method was found to be specific, precise, linear and robust. The drug was sensitive to acidic, basic, oxidative, thermal, and photodegradation resolving six degradation products. Thus, the developed AQbD-based stability-indicating HPLC method is applicable in analyzing evogliptin in bulk, tablet dosage form and stability samples.

In this study, Ag2CrO4@NiFe-LDH nanoparticles were synthesized by hydrothermal method for photocatalytic degradation of Alizarin Red (AR) dye. Three composites with different molar percentages were prepared, among which 50%Ag2CrO4@50%NiFe-LDH composite was the best sample with a removal rate of 97.1% in AR degradation. Also, the properties, structure, and characteristics of pure Ag2CrO4 and NiFe-LDH and their composites were determined by XRD, FESEM, FTIR, EDX mapping, and UV-visible analyses. It was found that Ag2CrO4@NiFe-LDH composites with the formation of heterogeneous structure of Z-scheme, in addition to increasing the active sites and increasing the specific surface, decrease the recombination rate of pure Ag2CrO4 and NiFe-LDH. Also, the Box-Behnken design technique, which is one of the most common designs used in response surface methodology, was used to optimize the operating conditions and investigate the effect of 4 independent parameters: catalyst amount, solution concentration, pH, and light intensity. The importance of independent parameters and their interactions were determined by ANOVA. By means of numerical optimization, the optimal values of the selected parameters equal to 1.34 g/L of catalyst, concentration of 16.45 mg/L, pH = 10.74, and light intensity of 15.53 W were obtained as optimal conditions with a desirability coefficient of 1.00 and an absorption value of 89.34%. The closeness of adjusted R2 (0.9838) and predicted R2 (0.9507) values show that this model can be successfully used for prediction.

The present paper is a comprehensive study on the optimization of ultrasonic assisted extraction and characterization of valued components from the newly developed garlic cultivar NARC-G1. The response surface methodology was employed to optimize the extraction time, solvent-to-solid ratio and extraction temperature, for optimal total phenolic contents (TPC), DPPH radical scavenging activity, α-amylase inhibition, and α-glucosidase inhibition. Under the optimized conditions (23 min extraction time, 60 °C temperature, and 39 : 1 solvent-to-solute ratio) the optimal TPC (13.76 mg GAE/g), DPPH radical scavenging activity (62.76 %), α-amylase inhibition (71.43 %), and α-glucosidase inhibition (79.43 %) were obtained. Significant correlations were observed between actual values and predicted values for the selected responses. Gas chromatography-mass spectrometry (GC-MS), revealed 26 high-value bioactives, with diallyl disulphide being the most abundant (16.22 %), followed by 2,3-dihydro-3,5-dihydroxy-6-methyl, 4H-pyran-4-one and 5-Hydroxymethylfurfural. Additionally, in silico investigation indicated that stigmasterol, arbutin, squalene, α-tocopherol and linoleic acid were responsible for antihyperglycemic potential. Moreover, antimicrobial activity revealed that S. mutans (19.25±1.98 mm) and L. monocytogenes (19.34±2.04 mm) were the most sensitive, while P. aeruginosa was the least sensitive bacterial strains against the optimized NARC-G1 garlic extract. This research effectively explains the optimal recovery of high-valued components from NARC-G1 and may contribute to nutra-pharmaceutical and functional food developments.

BACKGROUND: The recovery process for bioactives from discarded by-products of the winemaking industry is of great value considering both environmental and economic aspects.
OBJECTIVE: The goal of this study is to investigate the extraction of phenolic antioxidants from grape (Vitis vinifera) seeds by means of carboxylic acid-based deep eutectic solvents (DESs) in order to propose an environmentally friendly method based on a multivariate optimization approach.
METHODS: Carboxylic acid-based DESs were designed with several molar ratios (1/1, 1/2, and 2/1). Two polyols (glycerol and ethylene glycol) were used as hydrogen bond donors, while formic acid, acetic acid, and propionic acid were selected as hydrogen bond acceptors. The process parameters (water content, extraction time, and solid mass) were analyzed to optimize the process through Box-Behnken design with response surface method, after determination of the best combination for the highest total phenolic content (TPC) and the antioxidant activity yields.
RESULTS: The maximum TPC yield (153.17 ± 0.003 mg-GAE/g-GS) and antioxidant activity yield (82.26 ± 0.004 mg-GAE/g-GS) were achieved by 50% water addition into the DES (ethylene glycol/acetic acid, 1/1), 85 sec extraction time, and 0.1 g grape seed.

ABSTARCTAim: Development and evaluation of aqueous core nanocapsules (ACNs) of BCS-II-class drug like resveratrol (RSV) and pterostilbene (PTE) for prostate cancer. Materials & methods: Identify synergistic effects of molar ratios of RSV and PTE against PC-3 cell. Selected ratio of drugs was added to ACNs by double-emulsification-method using Box-Behnken design. Further, assessed for physicochemical characterization, release kinetics, compatibility, in vitro cytotoxicity, in vivo pharmacokinetic and biodistribution studies. Results: Selected 1:1 ratio of RSV and PTE had greatest synergy potential have smaller particle-size (128.1 ± 3.21 nm), zeta-potential (-22.12 ± 0.2 mV), 0.53 PDI, improved encapsulation (87% for RSV, 72% for PTE), stable, no systemic toxicity, high biodistributed/accumulated in prostate cells. Conclusion: ACNs exhibited high t1/2 (12.42 ± 1.92 hs) and 8.20 ± 8.21 hs Mean Residence Time and lower clearance, proving the high effectiveness for prostate cancer.
[Box: see text].

Acid mine drainage (AMD) is one of the main environmental problems associated with mining activity, whether the mine is operational or abandoned. In this work, several precipitates from this mine drainage generated by the oxidation of sulfide minerals, when exposed to weathering, were used as adsorbents. Such AMD precipitates from abandoned Portuguese mines (AGO, AGO-1, CF, and V9) were compared with two raw materials from Morocco (ClayMA and pyrophyllite) in terms of their efficiency in wastewater treatment. Different analytical techniques, such as XRD diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), N2 adsorption isotherms, and Scanning Electron Microscopy (SEM) with Energy Dispersive X-ray (EDX) were used to characterize these natural materials. The adsorption properties were studied by optimizing different experimental factors, such as type of adsorbent, adsorbent mass, and dye concentration by the Box-Behnken Design model, using methylene blue (MB) and crystal violet (CV) compounds as organic pollutants. The obtained kinetic data were examined using the pseudo-first and pseudo-second order equations, and the equilibrium adsorption data were studied using the Freundlich and Langmuir models. The adsorption behavior of the different adsorbents was perfectly fitted by the pseudo-second order kinetic model and the Langmuir isotherm. The most efficient adsorbent for both dyes was AGO-1 due to the presence of the cellulose molecules, with qm equal to 40.5 and 16.0 mg/g for CV and MB, respectively. This study confirms the possibility of employing AMD precipitates to adsorb organic pollutants in water, providing valuable information for developing future affordable solutions to reduce the wastes associated with mining activity.

Cellulose and lignin, sourced from biomass, hold potential for innovative bioprocesses and biomaterials. However, traditional fractionation and purification methods often rely on harmful chemicals and high temperatures, making these processes both hazardous and costly. This study introduces a sustainable approach for fractionating acacia wood, focusing on both cellulose and lignin extraction using a deep eutectic solvent (DES) composed of choline chloride (ChCl) and levulinic acid (LA). A design of experiment was employed for the optimization of the most relevant fractionation parameters: time and temperature. In the case of the lignin, both parameters were found to be significant variables in the fractionation process (p-values of 0.0128 and 0.0319 for time and temperature, respectively), with a positive influence. Likewise, in the cellulose case, time and temperature also demonstrated a positive effect, with p-values of 0.0103 and 0.028, respectively. An optimization study was finally conducted to determine the maximum fractionation yield of lignin and cellulose. The optimized conditions were found to be 15% (w/v) of the wood sample in 1:3 ChCl:LA under a treatment temperature of 160 °C for 8 h. The developed method was validated through repeatability and intermediate precision studies, which yielded a coefficient of variation lower than 5%. The recovery and reuse of DES were successfully evaluated, revealing remarkable fractionation yields even after five cycles. This work demonstrates the feasibility of selectively extracting lignin and cellulose from woody biomass using a sustainable solvent, thus paving the way for valorization of invasive species biomass.

This study aimed to develop a fast procedure for caffeine extraction from roasted coffee beans. The microwave-assisted extraction was carried out in the microwave oven with an operating frequency of 2450 MHz. The response surface methodology based on a Box-Behnken design was used to model and optimize the extraction process. Among the analyzed extraction parameters (factors), the influence of extraction time (2-6 min), liquid-to-solid ratio (5-15 mL/g), and microwave power (336-595 W) were considered, while the yield of extracted caffeine was observed as the response of the system. Water was used as the solvent of choice for the extraction of caffeine. The optimum conditions were as follows: extraction time, 2 min; liquid-to-solid ratio, 15 mL/g; and microwave power, 500 W. In this optimized condition, the expected extraction yield of caffeine was 1.01 g/100 g dry weight (value confirmed by experimental assays). The total energy consumed of 1.7 kWh/100 g of purified caffeine indicated a more energy-efficient procedure by about 1200-15,000 times than the reported procedures. This study showed that caffeine can be quantitatively extracted from roasted coffee beans through a green approach and that the isolated caffeine has a high purity degree, which was confirmed by the UHPLC-ESI-MS/MS method. With this quality, isolated caffeine could be further used as an active ingredient in the food industry, while for pharmaceutical purposes, it must be further purified.

Additive manufacturing (AM), particularly fused filament fabrication (FFF), has gained significant attention for its design flexibility and cost-effectiveness. This study focuses on optimizing FFF parameters that employ response surface methodology (RSM) to enhance the flexural performance of polyethylene terephthalate glycol (PETG) parts. Three essential parameters-layer height, print speed, and nozzle temperature-were varied, and their effects on flexural strength, flexural modulus, flexural toughness for ultimate strength, flexural toughness at 5% strain, and strain at ultimate strength were evaluated. Based on a Box-Behnken design, the experiments revealed significant effects of these parameters on the mechanical responses. The analysis of variance (ANOVA) indicates that layer height predominantly affects flexural modulus and toughness, while nozzle temperature significantly impacts flexural strength. The RSM models exhibited high accuracy, with R2 values exceeding 99%. Optimal parameter combinations yield remarkable improvements: flexural strength reached 39.55 MPa, flexural modulus peaked at 1344.60 MPa, flexural toughness for ultimate strength reached 218.22 J/mm3, flexural toughness at 5% strain reached 381.47 J/mm3, and strain at ultimate strength reached 3.50%. Validation experiments confirm the effectiveness of the optimization, with errors below 3.17%.

The presence of heavy metals and pollutant dyes can have detrimental effects on aquatic ecosystems and compromise aquatic aesthetics. This study investigates the use of unprocessed waste gem meerschaum powder as a new adsorbent in the removal of both Cu(II) and methylene blue (MB) from aqueous solutions to reduce water pollution. The structure of the waste powder was characterized by FT-IR, XRD, SEM and BET methods. Optimization of Cu(II) and MB dye removal was carried out using design of experiment technique. Under optimum conditions, remarkable removal efficiencies of 95.5% (± 3.7) for Cu(II) and 97.8% (± 0.4) for MB were achieved. The removal of Cu(II) followed the Freundlich isotherm model, while the removal of MB dye adhered to the Langmuir isotherm model. Both adsorption processes obeyed the pseudo-second-order kinetic model and occurred spontaneously. This innovative approach offers a promising solution to water pollution by highlighting the importance of sustainable and cost-effective waste use.