Min Sonication Time Research Articles

Ultrasonic assisted extraction of water-soluble vitamins from minor components of bee pollen with deep eutectic solvents (DESs) as green solvent

In this study, different deep eutectic solvents (DESs) were used for vitamin extraction from bee pollen. The DES combination with the highest total amount of individual vitamins was choline chloride: ethylene glycol (molar ratio 1:2). The response surface method was then used to optimize the extraction conditions. The independent variables used for optimization were ultrasonic power, time, and temperature, while the dependent variables were the total individual amino acids, total individual phenolic compounds, and total individual vitamin contents. Spectrophotometric analyses and antimicrobial activity were also determined in the extracts. In addition, AGREEprep, ComplexGAPI and BAGI tools were used to evaluate the greenness of the method. The results obtained with DES were compared with water, ethanol, and methanol extracts, which were considered control groups. As a result of optimization, the optimum conditions were found to be 75 % for ultrasonic power, 71.5 min for sonication time, and 40 °C for ultrasonic bath temperature. The model’s composite desirability value (d) was found to be 0.81. The predicted value and the experimental values were close to each other. Furthermore, the most dominant vitamin in DES extracts was ascorbic acid, the most dominant amino acid was proline, and the most dominant phenolic compound was myricetin. The amounts of these compounds were higher than those obtained from water, ethanol, and methanol extracts. The spectrophotometric analysis results obtained higher yields with DES compared to the control groups. Antimicrobial activity analysis showed that pollen extracts prepared using choline chloride: ethylene glycol had a weak inhibitory effect for Gram-positive and Gram-negative bacteria but not yeast-like fungal strains. In conclusion, DES has been successfully used to extract vitamins and other bioactive compounds from bee pollen. The results obtained showed that DESs can be an alternative to organic solvents for the extraction of vitamins, which are among the minor components of bee pollen. Besides, the potential of the application different DESs for more efficient extraction of vitamins and components with important pharmaceutical properties from bee pollen needs to be evaluated in detail.

Application of ZnS:Ni Loaded on Sponge‐Activated Carbon as an Efficient Adsorbent for Dye Removal

AbstractIn the present work, a ZnS:Ni loaded on sponge‐activated carbon (SAC) was synthesized and applied as an effective adsorbent to remove bromophenol blue (BPB) dye from aqueous solutions. Various techniques such as Fourier‐transform infrared, X‐ray diffraction, transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), and Brunauer‐Emmett‐Teller (BET) were used to characterize ZnS:Ni–SAC. The effective parameters such as BPB concentration, amount of ZnS:Ni–SAC, ultrasonic time, and pH of the aqueous solution were investigated and optimized by response surface methodology. To investigate the accuracy and reliability of the proposed method, the analysis of variance was used based on p‐values and F‐test. The optimal values of the parameters were obtained using the desirability function, and they were as follows: 15 mg L−1 BPB concentration, 20 min sonication time, 18 mg of ZnS:Ni–SAC, and pH = 7. To evaluate the adsorption mechanism and calculation of maximum adsorption capacity, different adsorption isotherms were studied, and according to the obtained results, the Langmuir isotherm model showed the highest compatibility due to its higher R2 (0.997). Also, the proposed adsorbent represented good adsorption capacity (125 mg g−1). Moreover, kinetic studies proved the applicability of the pseudo‐second‐order model (R2 = 0.986) compared to other models. The achieved results confirmed the applicability of ZnS:Ni–SAC as a versatile adsorbent for the removal of BPB.

Modelling and optimization of fabrication parameters for multi-walled carbon nanotubes-filled GFRP composites using RSM and Rao-1 algorithm

This study presents an optimized approach for fabricating multi-walled carbon nanotubes (MWCNTs) filled glass fibre reinforced polymers (GFRP) composites using hybrid optimization approach. The experimental runs performed as per Box-Behnken design of response surface methodology (RSM) by considering three fabrication parameters: MWCNT loading, sonication time (ST), and oven curing temperature (OCT), and the output response, ultimate tensile strength (UTS) is noted. Analysis of variance (ANOVA) is employed to ascertain the significance of the effects that each factor has on UTS and found fabrication variables, OCT, and combined effects of ST and OCT are most significant. Other variables, direct effects of MWCNT loading, interaction effects of all three combinations have influence on UTS. Mathematical modeling is postulated using RSM from which contour plots are drawn to illustrate both direct and interactive effects and reveal fabrication parameters have detrimental effects on UTS. The mathematical equation of UTS is then solved by Rao-1 optimization algorithm and obtained condition is: 1.0% of MWCNT loading, 97.5 min of sonication time, and 76 °C of oven curing temperature and corresponding UTS of 624 MPa. SEM analysis has also been performed to verify the distribution of MWCNTs in the GFRP and observed uniform dispersion of MWCNTs in the developed composite. A confirmatory test validates the predicted optimal fabrication condition derived from the RSM combined with Rao-1 algorithm, ensuring that the methodology has ability to enhance the UTS of MWCNTs-embedded GFRP composites.

Synthesis of magnetic layered double hydroxide (Fe3O4@CuCr-LDH) decorated with ZIF-8 for efficient sonocatalytic degradation of tetracycline

A series of Fe3O4@CuCr-LDH hybrids decorated with different amount of ZIF-8 (FLZ, 10–40 wt%) was prepared using simple methods and characterized with different techniques. The activity of the synthesized nanocomposites was investigated in the sonocatalytic degradation of tetracycline (TC) antibiotic from wastewater. When the content of ZIF-8 in the nanocomposite structure was 20 wt%, the FLZ-20 sonocatalyst exhibited the high performance in the sonocatalytic removal of TC. At optimum conditions (0.7 g/L catalyst dosage, pH of 7, 50 mg/L initial concentration of antibiotic, and 15 min sonication time) of the sonocatalytic removal of TC approached to 91.4% under ultrasonic irradiation (USI) using FLZ-20. This efficiency was much higher than those of obtained results by Fe3O4@CuCr-LDH and pristine ZIF-8. The formed ●OH and ●O2− exhibited the major roles in the sonocatalytic TC degradation process. The excellent performance of FLZ-20 can be attributed to the heterojunctions created between composite components, which could improve the electron transfer ability and effectively separate e−/h+ pairs. In addition, FLZ-20 showed the superior reusability and stability during three successive recycling. Moreover, the facile magnetically separation of the sonocatalyst from the aqueous solution was another outstanding feature, which prevents the formation of secondary pollutants. It can be concluded that the fabrication of heterojunctions is an efficient procedure to promote the sonocatalytic acting of the catalyst.

Green Synthesis of Selenium Nanoparticles using Green Coffee Beans: An Optimization Study.

In this study, ultrasonication extraction of some bioactive compounds from green coffee beans was optimized with the response surface method using Box-Behnken experimental design. The best condition was selected as 90.90 W ultrasonic power, 33.63 min sonication time and 30 % solid concentration. The responses obtained under optimum conditions had TPC, DPPH and CUPRAC values identified as 6603.33±2025.94 ppm GAE, 9638.31±372.17 ppm TE and 98.83 mmol, respectively. Microwave-assisted selenium nanoparticle production was carried out using the extract obtained under optimized conditions. The produced selenium nanoparticles showed absorbance between 350-400 nm. The surface morphology and size of the nanoparticles were determined by transmission electron microscopy (TEM) and spherical nanoparticles of about 100 nm were produced. Functional groups affecting the reduction were determined by FTIR analysis. In addition, the produced selenium nanoparticles had amorphous (non-uniform) structure and could maintain their stability at high temperatures.

Optimization of Ultrasound-Assisted Protein Extraction from Watermelon Seeds: Taguchi Approach

Nowadays, there has been a growing interest in finding alternative protein sources for both the food industry and nutritional purposes. Protein experts have recently focused on investigating watermelon seeds, which are not only a food processing waste but also contain high-quality proteins. Therefore, this study aimed to achieve maximum protein extraction from watermelon seeds using an ultrasound-assisted extraction process. The study investigated the effects of pH (A; 7─11), sonication temperature (B; 30─60 °C), and sonication time (C; 5─15 min) on protein recovery to develop a Taguchi model. Through optimization, the optimal conditions for maximum protein recovery (85.81%) within the range of process variables were found to be 11 pH, 45 °C sonication temperature, and 10 min sonication time (A3B2C2). An analysis of variance (ANOVA) revealed that pH and sonication temperature significantly influenced the protein extraction process (P

Skin hydration modulatory activities of Ficus deltoidea extract

Ficus deltoidea was known for its potent antioxidant, anti–melanogenic and photoprotective skin barrier activities. These properties are contributed by its biomarkers which are vitexin and isovitexin. This study aims to optimize the yield of methanolic extraction of Ficus deltoidea leaves (EFD) and evaluate their effects on skin barrier function and hydration. For optimization, Box–Behnken design was utilized to investigate the effects of methanol concentration, sonication time, and solvent–to–sample ratio on the yields of vitexin and isovitexin in EFD. The optimal yields obtained were 32.29 mg/g for vitexin and 35.87 mg/g for isovitexin. The optimum extraction conditions were 77.66% methanol concentration, 20.03 min sonication time, and 19.88 mL/g solvent–to–sample ratio. The quantitative real-time polymerase chain reaction was utilized to measure variant marker genes of transglutaminase-1, caspase 14, ceramide synthase 3, involucrin, and filaggrin of EFD-induced keratinocyte differentiation by in vitro study. Exposure to EFD has elevated the mRNA levels of all tested marker genes by 0.7–9.2 folds. Then, in vivo efficacy study was conducted on 20 female subjects for 14 days to evaluate skin biophysical assessment of hydration. EFD topical formulation treatment successfully increased skin hydration on day 7 (43.74%) and day 14 (47.23%). In silico study by molecular docking was performed to identify intermolecular binding interactions of vitexin and isovitexin with the interested proteins of tested marker genes. The result of molecular docking to the interested proteins revealed a similar trend with real-time PCR data. In conclusion, EFD potentially enhanced the skin barrier function and hydration of human skin cells.

DES-based microwave- and ultrasound-assisted extraction of natural products from Rumex hastatus as per response surface methodology

Rumex hastatus D. Don is a medicinal wild herb that abundantly grows in many parts of the world. The current work explores the extraction of its polyphenolic and antioxidant compounds using glycerol-choline chloride deep eutectic solvent and two modern techniques, ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE). The optimization was done as per the response surface methodology. Six responses were studied including total phenolic content (TPC), total flavonoid content (TFC), total condensed tannin content (TCT), ferrous iron-chelating (FIC) activity, DPPH radical scavenging activity (RSA), and ferric reducing antioxidant potential (FRAP). The optimal factors for MAE were 10 s extraction time, 229.40 W power, 40 mL/g SSR (solvent-to-solid ratio) and 60 % DES concentration with the predicted TPC, TFC, TCT, FIC, RSA and FRAP as 64.46 mg GAE/g PM, 155.78 mg RE/g PM, 129.73 mg CE/g PM, 51.46 mg EDTAE/g PM, 235.84 mg AAE/g PM and 129.14 mg AAE/g PM, respectively. For UAE, the predicted optimal factors were 24.30 min sonication time, 47 °C extraction temperature, 40 mL/g SSR and 60 % DES concentration with the predicted TPC, TFC, TCT, FIA, RSA, and FRAP as 56.54 mg GAE/g PM, 148.24 mg RE/g PM, 155.60 mg CE/g PM, 57.83 mg EDTAE/g PM, 240.56 mg AAE/g PM and 111.71 mg AAE/g PM, respectively. Both the models were strongly supported by the validation study with minimal % errors; 2.53–6.38 % for MAE and 1.14–5.30 % for UAE. MAE was more efficient than UAE in terms of time input and recovery of total polyphenols. Therefore, the method based on DES-MAE can safely be recommended for use on an industrial level for obtaining bioactives from R. hastatus.

Extraction of dietary fiber and encapsulated phytochemical enriched functional pasta from Bottle gourd (Lagenaria siceraria) peel waste

Bottle gourd (Lagenaria siceraria) peels are treated as an agro-waste material and are generally discarded. Dietary fiber and phytochemicals from this agro-waste material can serve as important functional ingredients. The aim of this study was to utilize bottle gourd peels for extraction of dietary fiber and phytochemicals and use them as functional ingredients in the preparing pasta. Dietary fiber was extracted using alkaline extraction (AEDF), ultrasound-assisted alkaline extraction (UAEDF) and enzymatic extraction (EADF). The optimised conditions for extraction using ultrasound-assisted alkaline extraction were 1: 60 solute to solvent ratio, 40 min sonication time, and 40 % ultrasonic amplitude. The physicochemical and functional properties of extracted dietary fiber, results showed that dietary fiber from ultrasound-assisted alkaline extraction gave a better result for thermal, oil and water holding properties. Phytochemicals were extracted and identified using RP-HPLC followed by encapsulation using 2 % sodium alginate solution as the wall material. Functional pasta was prepared by incorporation of extracted dietary fiber and encapsulated phytochemicals in 5 different formulations of durum wheat semolina (g), extracted DF (g) and phytochemical beads (mg). The results of the study revealed that bottle gourd peel could be used as an inexpensive source of dietary fiber and phytochemicals to prepare functional foods.

Optimization of Bromocriptine-Mesylate-Loaded Polycaprolactone Nanoparticles Coated with Chitosan for Nose-to-Brain Delivery: In Vitro and In Vivo Studies.

Bromocriptine mesylate (BM), primarily ergocryptine, is a dopamine agonist derived from ergot alkaloids. This study aimed to formulate chitosan (CS)-coated poly ε-caprolactone nanoparticles (PCL NPs) loaded with BM for direct targeting to the brain via the nasal route. PCL NPs were optimized using response surface methodology and a Box-Behnken factorial design. Independent formulation parameters for nanoparticle attributes, including PCL payload (A), D-α-tocopherol polyethylene glycol 1000 succinate (TPGS) concentration (B), and sonication time (C), were investigated. The dependent variables were nanoparticle size (Y1), zeta potential (Y2), entrapment efficiency (EE; Y3), and drug release rate (Y4). The optimal formulation for BM-PCL NPs was determined to be 50 mg PCL load, 0.0865% TPGS concentration, and 8 min sonication time, resulting in nanoparticles with a size of 296 ± 2.9 nm having a zeta potential of -16.2 ± 3.8 mV, an EE of 90.7 ± 1.9%, and a zero-order release rate of 2.6 ± 1.3%/min. The optimized BM-PCL NPs were then coated with CS at varying concentrations (0.25, 0.5, and 1%) to enhance their effect. The CS-PCL NPs exhibited different particle sizes and zeta potentials depending on the CS concentration used. The highest EE (88%) and drug load (DL; 5.5%) were observed for the optimized BM-CS-PCL NPs coated with 0.25% CS. The BM-CS-PCL NPs displayed a biphasic release pattern, with an initial rapid drug release lasting for 2 h, followed by a sustained release for up to 48 h. The 0.25% CS-coated BM-CS-PCL NPs showed a high level of permeation across the goat nasal mucosa, with reasonable mucoadhesive strength. These findings suggested that the optimized 0.25% CS-coated BM-CS-PCL NPs hold promise for successful nasal delivery, thereby improving the therapeutic efficacy of BM.

Formulation and Characterization of Ursodeoxycholic Acid Nanosuspension Based on Bottom-Up Technology and Box-Behnken Design Optimization.

Ursodeoxycholic acid (UDCA) is a therapeutic agent used for the treatment of cholestatic hepatobiliary diseases in pediatric patients. It is a bile acid that presents high lipophilicity, and it belongs to Class II of the Biopharmaceutical Classification System (BCS), which exhibits low water solubility and high intestinal permeability, which leads to poor oral absorption. The objective of this work was to design and optimize UDCA nanosuspensions by means of the precipitation-ultrasonication method to improve the solubility, dissolution, and oral bioavailability of UDCA. A three-level, three-factor Box-Behnken design was used to optimize formulation variables and obtain uniform, small-particle-size UDCA nanosuspensions. The independent variables were: stabilizer percentage (X1), amplitude (X2), and sonication time (X3), and the dependent variable was the particle size (Y1). In the precipitation-ultrasonication method, UDCA was dissolved in acetone:PEG 400 (1:1 v/v) and quickly incorporated into the antisolvent (pre-cooled aqueous dispersion of HPMC E-15 0.3%), by means of intense sonication at 50 W for 5 min, controlling temperature through an ice water bath. The lyophilization efficacy was evaluated by means of a cryoprotective efficacy test, working with 10% maltose at -80 °C. The nanosuspensions were characterized by dynamic light scattering (DLS), X-ray diffraction, and scanning electron microscopy (SEM). The physicochemical stability was determined at 25 °C and 4 °C at 7, 14, 30, and 60 days, and the UDCA content was analyzed via HPLC-UV. An in vitro dissolution assay and an oral bioavailability study were performed in male Wistar rats. A significant impact was achieved in the optimized nanosuspension with 0.3% (stabilizer), 50 W (amplitude), and 5 min (sonication time), with a particle size of 352.4 nm, PDI of 0.11, and zeta potential of -4.30 mV. It presented adequate physicochemical stability throughout the study and the UDCA content was between 90% and 110%. In total, 86% of UDCA was dissolved in the in vitro dissolution test. The relative oral bioavailability was similar without significant statistical differences when comparing the lyophilized nanosuspension and the commercial tablet, the latter presenting a more erratic behavior. The pharmacokinetic parameters of the nanosuspension and the commercial tablet were Tmax (1.0 ± 0.9 h vs. 2.0 ± 0.8 h, respectively), Cmax (0.558 ± 0.118 vs. 0.366 ± 0.113 µM, respectively), ΔCmax (0.309 ± 0.099 vs. 0.232 ± 0.056, respectively), AUC (4.326 ± 0.471 vs. 2.188 ± 0.353 µg/mL.h, respectively, p < 0.02), and IAUC0-24h (2.261 ± 0.187 µg/mL.h vs. 1.924 ± 0.440 µg/mL.h, respectively). The developed nanosuspension presents an appropriate dosage and administration for pediatric patients. On the other hand, it exhibits an adequate absorption and UDCA oral bioavailability.

Comparing the effects of irradiation and ultrasound on enrofloxacin, oxytetracycline, and sulfadiazine residues in chicken meat

PurposeThis research aims to evaluate and compare the effects of irradiation and ultrasound treatments on residual amount of three widely detected antibiotics in chicken meat, in addition to colorimetry and weight loss investigation. MethodsBroiler chickens were administered with three common antibiotics including enrofloxacin, oxytetracycline, and sulfadiazine and slaughtered at the age of 42 days. Chicken breast meat containing antibiotic residues was separately treated by gamma irradiation (at doses of 3, 5, and 7 kGy) and ultrasound at 240 W and 40 kHz (for 2, 5, and 10 min) to assess the effects of the treatments on reduction of antibiotic residues using HPLC technique. Moreover, the impact of treatments on weight loss and color changes were evaluated. ResultsThe results showed that both treatments significantly reduced the antibiotic residues; however, irradiation at higher doses and ultrasound at longer durations were more effective. The highest reduction of antibiotic residue was obtained at 7 kGy radiation dose and 10 min sonication time which was assigned to enrofloxacin (86.1%) followed by oxytetracycline (85%) and sulfadiazine (70.3%). Irradiation increased the L* (lightness) value and decreased the a* (redness) and b* (yellowness) values in chicken, but ultrasound had mostly no significant effect on the L* and a* values. Furthermore, both irradiation and ultrasound caused weight loss in the samples, but in the irradiated samples it was more than the sonicated ones. ConclusionsGenerally, using ultrasound for 10 min can be recommended as a better method to reduce the antibiotic residues in chicken.

Response surface methodology optimization extraction of aloins from Aloe vera leaf skin by ultrasonic horn sonicator and cytotoxicity evaluation

Aloe vera leaf skin (AVLS) is a major byproduct of plant gel treatment and a promising source of bioactive compounds. The present study aims at intensifying the extraction of AVLS using an ultrasound-assisted technique. Central composite design (CCD) protocol as a subset of Response Surface Methodology (RSM) was employed to investigate the interaction of process variables on the amount of aloin A and aloin B extraction from AVLS. The optimum extraction conditions of 30 min sonication time, EtOH 80%, and 65% sonication power were obtained corresponding to maximize extraction of aloin A (4.33 mg.g−1), and aloin B (4.46 mg.g−1), and the extraction yield was 9.43%. It was revealed that the amounts of aloin A and aloin B increased as the extraction yield decreased. To evaluate the cytotoxic effect of the extract on cancer cells MTT assay was performed on A549 cells (a human lung cancer cell line). Our preliminary results indicated that the AVLS extract could inhibit the proliferation of A549 cells (IC50 =166 µg.mL−1). Moreover, compared with conventional methods, ultrasound radiation made effective cracks in the surface structures of the leaf skin. The results of the present study may have contributed to the development of extraction methods with probe-sonic applicable to extract of aloin A and B.

Complete removal of CO at ambient conditions using copper manganese oxide (CuMnOx) catalysts synthesised via co-precipitation with ultrasonic irradiation

This present work investigates the novel method of synthesising copper manganese oxide (Hopcalite) catalysts with a Cu:Mn ratio of 1:2 by using a facile ultrasound-assisted co-precipitation synthesis technique. The CuMnOx catalysts were synthesised using an ultrasonic bath or an ultrasonic probe with varying ultrasonic powers. The catalysts were further characterised and evaluated for the oxidation of carbon monoxide (CO). Characterisation results revealed that samples prepared using the ultrasonic method exhibited enhanced physical properties, such as highly dispersed particles with a larger surface area and pore size. Besides, the presence of mixed copper and manganese oxide phases was detected, which provided synergistic interactions to facilitate and enhance CO oxidation. The amorphicity and reducibility of the catalysts were also improved, thus indicating the presence of more active sites. Furthermore, the catalyst prepared using the ultrasonic probe at a power of 23.3 W with a 15 min sonication time was found to be the most active, with the capability of oxidising CO to CO2 to completion (100 %) at ambient conditions. It also possessed high catalytic stability, in which catalytic activity was not compromised for as long as 200 min. On the whole, this work has ascertained that by incorporating a simple ultrasonic irradiation step into the synthesis procedure of copper manganese oxide catalysts, the overall performance of the catalyst can be greatly improved compared to those already found in the literature, which demonstrates the potential application of this new method on a wider, commercial scale for carbon monoxide removal.

Impact of different drying techniques on grapefruit peels and subsequent optimization of ultrasonic extraction conditions for bioactive compounds

AbstractThis research aims to investigate the effect of different drying methods on the phytochemical compounds of grapefruit peels and the subsequent optimization of ultrasonicated assisted extraction conditions for bioactive compounds. Based on the maximum retention of phenolic compounds and naringin content, the hot air‐drying approach was selected for optimization of extraction process. The Box–Behnken design was used for ultrasonic‐assisted extraction (UAE) of bioactive compounds from hot air‐dried peel powder. Three factors such as solvent concentration (SC), ultrasonic amplitude (UA), and sonication time (ST) were considered for optimize the extraction condition based on total phenolic content (TPC), total flavonoid content (TFC), naringin content, and total antioxidant activities (TAA). UV‐spectrophotometric and HPLC was used for the determination in this study. The results revealed that UA and ST had significant effects on all the extraction responses. Based on the numerical optimization, the optimum extraction condition was found to be 48% (v/v) ethanol concentration, 40% ultrasonic amplitude, and 13 min sonication time. The respective optimum phytochemicals and antioxidant activity responses were obtained as TPC (78.5 mg GAE/g dw), TFC (53.5 mg naringin/g dw), naringin content (40.8 mg/g dw), and total antioxidant activities by DPPH assay (25.5 mM Trolox/g dw), ABTS*+ assay (4050 mM Trolox/100 g dw) and FRAP assay (17.45 Fe [II]/g dw).Practical ApplicationsFruit peels are a rich and valuable bioactive residue obtained from the various juice and beverage processing industries. Grapefruit peels are an abundant source of antioxidants and bioflavonoids such as naringin and hesperidin, which have huge potential as a functional ingredients. The optimum extraction condition obtained by this UAE technique has higher levels of polyphenolic compounds and flavonoids, particularly naringin, which shows a wide range of applications in the pharmaceutical sector and might be a way towards its effective sources of utilization in functional foods.

Incorporation of graphene oxide to metal‐free phthalocyanine through hydrogen bonding for optoelectronic applications: An experimental and computational study

AbstractThis paper focuses on incorporation of graphene oxide (GO) to metal‐free phthalocyanine (MPc) through only hydrogen bonding and π‐π stacking. Briefly, Pc‐GO composites at various concentrations were prepared by self‐assembly method. The processing time was kept below 10 min to avoid covalent attachment and we aimed at answering the research question of what will happen if the conjugation is realized only through hydrogen bonding under extremely limited processing times. The as‐prepared MPc‐GO composites were characterized by Fourier transform infrared (FT‐IR), UV‐Vis, scanning electron microscope (SEM), and fluorescence analysis. We report that the interaction between MPc and GO could immediately be initiated upon mixing of corresponding solutions. Also, complete conjugation by hydrogen bonding and π‐π stacking could be reached even only in 5 min of sonication time. In addition, it was also determined that the prepared MPc‐GO composites are stable at room conditions and during dilution. Finally, the optoelectronic properties of MPc and MPc‐GO composites were also investigated experimentally and theoretically. Both experimental and theoretical results suggest that MPc‐GO composites exhibit improved optoelectronic properties as compared to MPc, even though the conjugation of GO to MPc was only via hydrogen bonding without covalent attachment.

Andrographolide nanophytosomes exhibit enhanced cellular delivery and pro-apoptotic activities in HepG2 liver cancer cells

Andrographolide (AG), a major active constituent of Andrographis paniculata, is known to hinder proliferation of several types of cancer cells. However, its poor solubility and cellular permeability restrict its use in clinical applications. In this study, AG-loaded phytosomes (AG-PTMs) were formulated and optimized with respect to particle size using l-α-phosphatidylcholine (PC):AG ratio and sonication time (ST) as independent variables. The optimized formula was prepared at 1:2.7 for AG:PC molar ratio and 4.9 min for ST and exhibited a particle size of 243.7 ± 7.3 nm, polydispersity index (PDI) of 0.310 and entrapment efficiency of 72.20 ± 4.53. Also, the prepared formula showed a slow release of AG over 24-h period. The antiproliferative activity of AG-PTMs was investigated against the liver cancer cell line HepG2. AG-PTMs significantly repressed the growth of HepG2 cells with an IC50 value of 4.02 ± 0.14 µM. AG uptake by HepG2 cells was significantly enhanced in incubations containing the optimized formula. AG-PTMs also caused G2-M cell cycle phase arrest and increased the fraction of apoptotic cells in pre-G1 phase. These effects were associated with induction of oxidative stress and mitochondrial dysfunction. In addition, AG-PTMs significantly upregulated mRNA expression of BAX and downregulated that of BCL2. Furthermore, AG-PTMs significantly enhanced the concentration of caspase-3 in comparison to raw AG. These data indicate that the phytosomal delivery of AG significantly inhibited HepG2 cell proliferation through enhanced cellular uptake, arresting cell cycle at the G2-M phase and inducing mitochondrial-dependent apoptosis.

Optimization of thiamine chitosan nanoemulsion production using sonication treatment

The production of thiamine chitosan nanoemulsion via sonication treatment has been optimized using response surface methodology (RSM). This study examines the effect of sonication treatment on thiamine chitosan formulation and variations in time, amplitude, and surfactant concentration to distinguish optimum production conditions. Chitosan thiamine nanoemulsion was prepared using the central composite design (CCD) with 3 independent variables (time, amplitude, and surfactant concentration), which generated 20 experimental points. The optimum condition was determined by analyzing the response variable, which, in this study, is viscosity. The analysis was carried out using the Minitab 18 software. The sample as formulated using the optimum conditions derived were then tested for particle size using a Particle Size Analyzer (PSA). The results showed that the 3-factorial design and response surface methodology could determine the optimum conditions for the formulation process of chitosan thiamine nanoemulsion. The optimum viscosity of the thiamine chitosan nanoemulsion determined was 10.5 mPa s which was obtained with 55.2 min sonication time, Tween 80 surfactant concentration of 3.4%, and amplitude of 56.8 m. The chitosan thiamine nanoemulsion produced with these conditions had a particle size of 20.1 nm and a polydispersity index of 0.446, which indicated that it was stable and homogeneous.

Optimization of ultrasonic-assisted osmotic dehydration as a pretreatment for microwave drying of beetroot (Beta vulgaris).

The aim of this study was to optimize drying conditions during ultrasonic-assisted osmotic dehydration and subsequent microwave drying of red beetroot using the Box-Behnken design. For this purpose, ultrasonic-assisted osmotic dehydration was performed at different ultrasonic powers (50, 75, and 100 W), sonication times (20, 40, and 60 min), and salt concentrations (0%, 15%, and 30%). The subsequent drying procedures were conducted with 231, 518, and 805 W microwave power. The best condition was selected as 5.15% salt concentration, 20 min sonication time, 50 W ultrasonic power, and 716.45 W microwave power. The responses obtained under optimum conditions were determined as 68.06%, 9.54 mg GAE/g dm, 28.23, 42.66, and 3.08 for DPPH• % inhibition, total phenolic content, L*, a*, and b* values, respectively. While favorable impacts on color were detected for the applied pretreatments, the DPPH• scavenging activities of the dried beetroot were determined to be more significant after ultrasonic-assisted osmotic dehydration. Furthermore, the drying kinetics of beetroot were evaluated according to the Midilli et al. model. When the fit to the model was investigated, it was compatible at R2 > 0.90 level. As a result, the ultrasonic-assisted osmotic dehydration pretreatment performed before the microwave drying method preserved the quality characteristics of beetroot samples and was successfully applied.

Optimization of Influential Parameters for the Degradation of Metronidazole Contained in Aquaculture Effluent via Sonocatalytic Process: Kinetics and Mechanism

This study examined the synthesis of a viable catalyst for the degradation of metronidazole contained in aquaculture effluent. Zinc oxide nanoparticles (n-ZnO) were synthesized via the precipitation method and calcined at 500oC in a muffle furnace to enhance the degradability properties. The morphology showed a hexagonal structure with an average particle size of 71.48 nm and the elemental composition showed a higher weight percent of 59.15% for zinc and 21.65% for oxygen. The FTIR confirms the vibrational characteristic mode of the Zn-O band at 427.21cm-1. The XRD showed a good crystallinity and the BET surface area was 8.58 m2.g-1 which showed that the n-ZnO possesses more active sites that can remove pollutants from wastewater. However, no studies have been done on the removal of MNZ in aquaculture effluent. The kinetics followed pseudo-second-order kinetics and the Langmuir-Hinshelwood model best fit the degradation process with R2, Kc, and KLH values of 0.96781, 1.486 × 10-1 mg. Lmin-1) and 8.790 × 10-2 (L.mg-1). Under the influential parameters, the percentage COD removal achieved for MNZ in aquaculture effluent was 62.6%, 89.8%, and 98.5% of MNZ at 20% ultrasonic amplitude, 5 mL 2% H2O2 and 0.02g n-ZnO within 60 min sonication time for US only, US/n-ZnO and US/n-ZnO/H2O2 systems. Hence, MNZ contained in aquaculture effluent can best be degraded with the synergetic effect of the US/n-ZnO/ H2O2 system.