Sonication enhances the stability of MnO2 nanoparticles on silk film template for enzyme mimic application

We have developed an in-situ method using sonication (3 mm probe sonicator, 30 W, 20 kHz) and auto-reduction (control) to study the mechanism of the formation of manganese dioxide (MnO₂) on a solid template (silk film), and its resulting enzymatic activity on tetramethylbenzidine (TMB) substrate. The fabrication of the silk film was first optimized for stability (no degradation) and optical transparency. A factorial approach was used to assess the effect of sonication time and the initial concentration of potassium permanganate (KMnO₄). The result indicated a significant correlation with a fraction of KMnO₄ consumed and MnO₂ formation. Further, we found that the optimal process conditions to obtain a stable silk film with highly catalytic MnO₂ nanoparticles (NPs) was 30 min of sonication in the presence of 0.5 mM of KMnO₄ at a temperature of 20–24 °C. Under the optimal condition, we monitored in-situ the formation of MnO₂ on the silk film, and after thorough rinsing, the in-situ catalysis of 0.8 mM of TMB substrate. For control, we used the auto-reduction of KMnO₄ onto the silk film after about 16 h. The result from single-wavelength analysis confirmed the different kinetics rates for the formation of MnO₂ via sonication and auto-reduction. The result from the multivariate component analysis indicated a three components route for sonication and auto-reduction to form MnO₂-Silk. Overall, we found that the smaller size, more mono-dispersed, and deeper buried MnO₂ NPs in silk film prepared by sonication, conferred a higher catalytic activity and stability to the hybrid material.     

Tailoring the size of ultrasound responsive lipid-shelled nanodroplets by varying production parameters and environmental conditions

Liquid perfluorocarbon nanodroplets (NDs) are an attractive alternative to microbubbles (MBs) for ultrasound-mediated therapeutic and diagnostic applications. ND size and size distribution have a strong influence on their behaviour in vivo, including extravasation efficiency, circulation time, and response to ultrasound stimulation. Thus, it is desirable to identify ways to tailor the ND size and size distribution during manufacturing. In this study phospholipid-coated NDs, comprising a perfluoro-n-pentane (PFP) core stabilised by a DSPC/PEG40s (1,2-distearoyl-sn-glycero-3-phosphocholine and polyoxyethylene(40)stearate, 9:1 molar ratio) shell, were produced in phosphate-buffered saline (PBS) by sonication. The effect of the following production-related parameters on ND size was investigated: PFP concentration, power and duration of sonication, and incorporation of a lipophilic fluorescent dye. ND stability was also assessed at both 4 °C and 37 °C. When a sonication pulse of 6 s and 15% duty cycle was employed, increasing the volumetric concentration of PFP from 5% to 15% v/v in PBS resulted in an increase in ND diameter from 215.8 ± 16.8 nm to 408.9 ± 171.2 nm. An increase in the intensity of sonication from 48 to 72 W (with 10% PFP v/v in PBS) led to a decrease in ND size from 354.6 ± 127.2 nm to 315.0 ± 100.5 nm. Increasing the sonication time from 20 s to 40 s (using a pulsed sonication with 30% duty cycle) did not result in a significant change in ND size (in the range 278–314 nm); however, when it was increased to 60 s, the average ND diameter reduced to 249.7 ± 9.7 nm, which also presented a significantly lower standard deviation compared to the other experimental conditions investigated (i.e., 9.7 nm vs. > 49.4 nm). The addition of the fluorescent dye DiI at different molar ratios did not affect the ND size distribution. NDs were stable at 4 °C for up to 6 days and at 37 °C for up to 110 min; however, some evidence of ND-to-MB phase transition was observed after 40 min at 37 °C. Finally, phase transition of NDs into MBs was demonstrated using a tissue-mimicking flow phantom under therapeutic ultrasound exposure conditions (ultrasound frequency: 0.5 MHz, acoustic pressure: 2–4 MPa, and pulse repetition frequency: 100 Hz).     

Electron paramagnetic resonance of sonicated powder suspensions in organic solvents

The chemical effects of the acoustic cavitation generated by ultrasound translates into the production of highly reactive radicals. Acoustic cavitation is widely explored in aqueous solutions but it remains poorly studied in organic liquids and in particular in liquid/solid media. However, several heterogeneous catalysis reactions take place in organic solvents.Thus, we sonicated trimethylene glycol and propylene glycol in the presence of silica particles (SiO₂) of different sizes (5–15 nm, 0.2–0.3 µm, 12–26 µm) and amounts (0.5 wt% and 3 wt%) at an ultrasound frequency of 20 kHz to quantify the radicals generated. The spin trap 5,5-dimethyl-1-pyrrolin–N-oxide (DMPO) was used to trap the generated radicals for study by electron paramagnetic resonance (EPR) spectroscopy. We identified the trapped radical as the hydroxyalkyl radical adduct of DMPO, and we quantified it using stable radical 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) as a quantitation standard. The concentration of DMPO spin adducts in solutions containing silica size 12–26 µm was higher than the solution without particles. The presence of these particles increased the concentration of the acoustically generated radicals by a factor of 1.5 (29 µM for 0.5 wt% of SiO₂ size 12–26 µm vs 19 µM for 0 wt%, after 60 min of sonication). Ultrasound produced fewest radicals in solutions with the smallest particles; the concentration of radical adducts was highest for SiO₂ particle size 12–26 µm at 0.5 wt% loading, reaching 29 µM after 60 min sonication. Ultrasound power of 50.6 W produced more radicals than 24.7 W (23 µM and 18 µM, respectively, at 30 min sonication). Increased temperature during sonication generated more radical adducts in the medium (26 µM at 75 °C and 18 µM at 61 °C after 30 min sonication). Acoustic cavitation, in the presence of silica, increased the production of radical species in the studied organic medium.     

Development of an empirical kinetic model for sonocatalytic process using neodymium doped zinc oxide nanoparticles

The degradation of Acid Blue 92 (AB92) solution was investigated using a sonocatalytic process with pure and neodymium (Nd)-doped ZnO nanoparticles. The nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). The 1% Nd-doped ZnO nanoparticles demonstrated the highest sonocatalytic activity for the treatment of AB92 (10 mg/L) with a degradation efficiency (DE%) of 86.20% compared to pure ZnO (62.92%) and sonication (45.73%) after 150 min. The results reveal that the sonocatalytic degradation followed pseudo-first order kinetics. An empirical kinetic model was developed using nonlinear regression analysis to estimate the pseudo-first-order rate constant (k_app) as a function of the operational parameters, including the initial dye concentration (5–25 mg/L), doped-catalyst dosage (0.25–1 g/L), ultrasonic power (150–400 W), and dopant content (1–6% mol). The results from the kinetic model were consistent with the experimental results (R² = 0.990). Moreover, DE% increases with addition of potassium periodate, peroxydisulfate, and hydrogen peroxide as radical enhancers by generating more free radicals. However, the addition of chloride, carbonate, sulfate, and t-butanol as radical scavengers declines DE%. Suitable reusability of the doped sonocatalyst was proven for several consecutive runs. Some of the produced intermediates were also detected by GC–MS analysis. The phytotoxicity test using Lemna minor (L. minor) plant confirmed the considerable toxicity removal of the AB92 solution after treatment process.     

Catalytic-oxidative/adsorptive denitrogenation of model hydrocarbon fuels under ultrasonic field using magnetic reduced graphene oxide-based phosphomolybdic acid (PMo-Fe3O4/rGO)

In this work, the effect of ultrasound irradiation on the catalytic oxidative/adsorptive denitrogenation (COADN) of model hydrocarbon fuels (composed of pyrrole or indole as an organonitrogen compounds dissolved in n-nonane) has been investigated using magnetic reduced graphene oxide supported with phosphomolybdic acid (PMo-Fe₃O₄/rGO) as a heterogeneous catalyst/adsorbent and hydrogen peroxide as an oxidant. The synthesized PMo-Fe₃O₄/rGO nanocomposite was characterized by XRD, FE-SEM, VSM and BET surface area analysis methods. Moreover, different experimental variables including catalyst dose, initial pyrrole/indole concentration, H₂O₂ to pyrrole/indole molar ratio, ultrasound power and sonication time have been studied on the COADN process. The regeneration/recyclability of PMo-Fe₃O₄/rGO catalyst was also examined. Experimental results revealed that, the ultrasound treatment significantly improved the adsorption process of organonitrogen compounds from model fuels (q_e increased by 50.3% for pyrrole and 18% for indole). Furthermore, high ultrasound-aided catalytic oxidative denitrogenation efficiency (85.6% for pyrrole and 90% for indole) has been attained under optimal conditions (ultrasonic power = 200 W, sonication time = 240 min, catalyst dose = 2 g/L, and H₂O₂:pyrrole/indole molar ratio = 5). The recyclability of catalyst displayed that the prepared catalyst can be reused five times without any significant reduction in its performance.     

Correlation between iodide dosimetry and terephthalic acid dosimetry to evaluate the reactive radical production due to the acoustic cavitation activity

Acoustic cavitation plays an important role in sonochemical processes and the rate of sonochemical reaction is influenced by sonication parameters. There are several methods to evaluate cavitation activity such as chemical dosimetry. In this study, to comparison between iodide dosimetry and terephthalic acid dosimetry, efficacy of sonication parameters in reactive radical production has been considered by iodide and terephthalic acid dosimetries. For this purpose, efficacy of different exposure parameters on cavitations production by 1 MHz ultrasound has been studied. The absorbance of KI dosimeter was measured by spectrophotometer and the fluorescence of terephthalic acid dosimeter was measured using spectrofluorometer after sonication. The result of experiments related to sonication time and intensity showed that with increasing time of sonication or intensity, the absorbance is increased. It has been shown that the absorbance for continuous mode is remarkably higher than for pulsing mode (p-value < 0.05). Also results show that with increasing the duty cycles of pulsed field, the inertial cavitation activity is increased. With compensation of sonication time or intensity in different duty cycles, no significant absorbance difference were observed unless 20% duty cycle. A significant correlation between the absorbance and fluorescence intensities (count) at different intensity (R = 0.971), different sonication time (R = 0.999) and different duty cycle (R = 0.967) were observed (p-value < 0.05). It is concluded that the sonication parameters having important influences on reactive radical production. These results suggest that there is a correlation between iodide dosimetry and terephthalic acid dosimetry to examine the acoustic cavitation activity in ultrasound field.     

High-efficiency degradation catalytic performance of a novel Angelica sinensis polysaccharide-silver nanomaterial for dyes by ultrasonic cavitation

Currently, the polluted wastewater discharged by industry accounts for the major part of polluted bodies of water. As one of the industrial wastewaters, dye wastewater is characterized by high toxicity, wide pollution, and difficulty in decolorization degradation. In this paper, a novel composite nanomaterial catalyst of silver was prepared by using Angelica sinensis polysaccharide (ASP) as a reducing and stabilizing agent. And the optimum reaction conditions explored are V_AgNO3 = 5 mL (300 mM) and v_ASP = 7% (w/v) for 6 h at 90 °C. In addition, the ASP-Ag nanocatalyst was characterized by several techniques. The results demonstrated that ASP-Ag nanoparticles were successfully synthesized. Degradation rate, which provides a numerical visualization of the percentage reduction in pollutant concentration. With the wrapping of ASP, the ultrasonic catalytic degradation rates of different organic dyes including rhodamine B (RB), methylene blue (MB), and methyl orange (MO) were from 88.2%, 88.7%, and 85.2% to 96.1%, 95.2% and 93.5% at room temperature, respectively. After the experiments, when c_dyes = 10 mg/L, the highest degradation rate can be observed under c_APS-AgNPs = 10 mg/L with the most powerful cavitation frequency f = 59 kHz. The effect of ultrasonic frequency on the acoustic pressure distribution in the reactor was investigated by using COMSOL Multiphysis^@ software to propose the mechanism of ultrasonic degradation and the mechanism was confirmed by OH radical trapping experiments. It indicates that OH produced by the ultrasonic cavitation effect plays a determinant role in the degradation. And then, the intermediate products of the dye degradation process were analyzed by gas chromatography and mass spectrometry (GC–MS), and the possible degradation processes of dyes were proposed. The resulting products of degradation are SO₄²⁻, NH₄⁺, NO₃⁻, N₂, CO₂ and H₂O. Finally, the recycling degradation experiments showed that catalyst maintains a high degradation rate within reusing 5 cycles. Thus, this catalyst is highly efficient and recyclable.     

Ultrasonic assisted-Fenton-like degradation of nitrobenzene at neutral pH using nanosized oxides of Fe and Cu

Ultrasonic-assisted heterogeneous Fenton reaction was used for degradation of nitrobenzene (NB) at neutral pH conditions. Nano-sized oxides of α-Fe₂O₃ and CuO were prepared, characterized and tested in degradation of NB (10 mg L⁻¹) under sonication of 20 kHz at 25 °C. Complete degradation of NB was effected at pH 7 in presence of 10 mM H₂O₂ after 10 min of sonication in presence of α-Fe₂O₃ (1.0 g L⁻¹), (k = 0.58 min⁻¹) and after 25 min in case of CuO (k = 0.126 min⁻¹). α-Fe₂O₃ showed also effective degradation under the conditions of 0.1 g L⁻¹ oxide and 5.0 mM of H₂O₂, even though with a lower rate constant (0.346 min⁻¹). Sonication plays a major role in enhancing the production of hydroxyl radicals in presence of solid oxides. Hydroxyl radicals-degradation pathway is suggested and adopted to explain the differences noted in rate constants recorded on using different oxides.     

The effect of low frequency ultrasound on the production and properties of nanocrystalline cellulose suspensions and films

Suspension of nanocrystalline cellulose (NCC) produced from bleached cotton by controlled sulphuric acid hydrolysis was treated with low frequency ultrasound at 20 kHz and 60% amplitude for 0, 1, 2, 5 and 10 min and the effects of sonication on the properties of both the cellulose nanocrystals and their aqueous suspensions were investigated. Furthermore, a series of nanocellulose films were manufactured from the suspensions that were sonicated for different periods of time and tested. Laser diffraction analysis and transmission electron microscopy proved that sonication not only disintegrated the large NCC aggregates (D_v50 14.7 μm) to individual nanowhiskers with an average length and width of 171 ± 57 and 17 ± 4 nm, respectively, but also degraded the nanocrystals and yielded shorter and thinner particles (118 ± 45 and 13 ± 3 nm, respectively) at 10-min sonication. The ultrasound-assisted disintegration to nano-sized cellulose whiskers decreased the optical haze of suspensions from 98.4% to 52.8% with increasing time from 0 to 10 min, respectively. Sonication of the suspensions significantly contributed to the preparation of films with low haze (high transparency) and excellent tensile properties. With the increasing duration of sonication, the haze decreased and the tensile strength rose gradually. Irrespectively of sonication, however, all films had an outstanding oxygen transmission rate in a range of 5.5–6.9 cm³/m² day, and a poor thermal stability.     

High-power sonication of soy proteins: Hydroxyl radicals and their effects on protein structure

High-power sonication (HPS) is shown to alter protein structure, thus, its functionality, via intermolecular interactions. This study evaluated the effects of HPS on molecular structure of soy proteins in aqueous medium. Free radicals generated during HPS were quantitated using the 5,5-dimethyl-l-pyrrolin N-oxide (DMPO) spin trap method. Electron paramagnetic resonance (EPR) was used to identify them as mostly hydroxyl radicals. The minimum saturation concentration of spin trap solution was determined to be 500 mM of DMPO in water, when exposed to 5 W/cm³ ultrasound power density (PD) for 10 min; subsequently, this concentration was used for quantitating radicals generated in protein samples. Five aqueous soy protein systems, namely, 5% soy protein isolate (SPI), 5% SPI without isoflavonoids (NO-ISO SPI), subunit solutions 1% glycinin (11S) and 1% β conglycinin (7S), and 10% soy flakes (w/v), were sonicated at 2.5 and 5 W/cm³ PDs. Only adducts of hydroxyl radicals (DMPO-OH) were detected in all of these aqueous systems. The highest concentration (3.68 µM) of DMPO-OH adduct was measured in 11S subunit solution at 5 W/cm³, whereas, the lowest (0.67 µM) was in soy flakes solution at 2.5 W/cm³. PD 5 W/cm³ generated higher concentration of radicals in 7S subunit solution, NO-ISO SPI, and soy flakes protein, compared to sonication at PD 2.5 W/cm³. No change in the protein electrophoretic patterns were observed due to HPS. However, some changes due to HPS were observed in the estimated secondary and tertiary structures, and the contents of free sulfhydryl groups and disulfide bonds in proteins.     

Synergistic effect of sonication on photocatalytic oxidation of pharmaceutical drug carbamazepine

Photocatalytic, sono-photocatalytic oxidation of pharmaceutical drug of carbamazepine was successfully carried out using Ag/AgCl supported BiVO₄ catalyst. For this purpose, firstly, photocatalytic oxidation was optimized by central composite design methodology and then synergistic effect of sonication was investigated. Low frequency (20 kHz) probe type and high frequency (850 kHz) plate type sonication at pulse and continuous mode were studied to degrade the carbamazepine (CBZ) containing wastewater. Pulse duties of 1:5 and 5:1 (on : off) were tested using the high frequency sonication system in the sono-photocatalytic oxidation of CBZ. The effects of frequency, power density measured from calorimetry by changing amplitudes were discussed in the sono-photocatalytic oxidation of CBZ. Complete carbamazepine removal was achieved at the optimum conditions of 5 ppm CBZ initial concentration with 1.5 g/L of catalysts loading and at an alkaline pH of 10 at the end of 4 h of photocatalytic reaction under visible LED light irradiation. Both low frequency and high frequency sonication systems caused an increase in photocatalytic efficiency in a shorter treatment time of 60 min. CBZ removal increased from 44% to 65.42% in low frequency sonication of 20 kHz at the amplitude of 20% (0.15 W/mL power density). In the case of high frequency ultrasonic system (850 kHz), CBZ removal increased significantly from 44% to 89.5 % at 75% amplitude (0.12 W/mL power density) within 60 min of reaction. Continuous mode sonication was observed to be more effective than that of pulse mode sonication not only for degradation efficiency and also for electrical energy consumption needed to degrade CBZ. Sono-catalytic oxidation was also conducted with simulated wastewater that contains SO₄^2-, CO₃^2–, NO^3–, Cl^- anions and natural organic component of fulvic acid. The CBZ degradation was inhibited slightly in the presence of NO₃^– and Cl^-, and fulvic acid, however, the existence of SO₄^2- and CO₃^2– increased the degradation degree of CBZ. Toxicity tests were performed to determine the toxicity of untreated CBZ, and treated CBZ by photocatalytic, and sono-photocatalytic oxidations.     

High-efficient liquid exfoliation of 2D metal-organic framework using deep-eutectic solvents

The exfoliation of bulk two-dimensional metal–organic framework (MOF) into few-layered nanosheets has attracted much attention recently. In this work, an environmental-friendly route has been developed for layered-MOF (MAMS-1) delamination using deep eutectic solvent (DES), which is more sustainable and efficient alternative than conventional organic solvents for MOF nanosheet preparation. Under sonication condition, DES as solvents, the highest exfoliation rate of MAMS-1 is up to 70% with two host layers via poly(vinylpyrrolidone) (PVP) surfactant-assisted method. The presence of tert-butyl exteriors and the atomically thickness endow the MOF nanosheets stable suspension for at least one month. Due to the 2D structure and excellent stability, MAMS-1 nanosheet (MAMS-1-NS) was chosen as a good candidate to encapsulate Eu³⁺ cations. The obtained Eu³⁺@MAMS-1-NS acts as a multi-responsive luminescent sensor through fluorescence quenching, and can specifically recognize Fe³⁺ (LOD = 0.40 μM, K_SV = 1.05 × 10⁵ M^−l), Hg²⁺ (LOD = 0.038 μM, K_SV = 5.78 × 10⁶ M^−l), Cr₂O₇²⁻ (LOD = 0.33 μM, K_SV = 1.55 × 10⁵ M^−l) and MnO₄⁻ (LOD = 0.088 μM, K_SV = 4.49 × 10⁵ M^−l). Compared with bulk Eu³⁺@MAMS-1, the sensitivity of Eu³⁺@MAMS-1-NS is greatly improved owing to its ultrathin nanosheet morphology and highly accessible active sites on the surface.     

Ultrasonic-assisted preparation of eucalyptus oil nanoemulsion: Process optimization,in vitro digestive stability,and anti-Escherichia coli activity

Eucalyptus oil (EO) is a natural and effective antimicrobial agent; however, it has disadvantages such as poor water solubility and instability. The aim of this study was to investigate the effect of process vessels and preparation process parameters on the particle size of the emulsion droplets using ultrasonic technique and response surface methodology to prepare eucalyptus oil nanoemulsion (EONE). The optimal sonication process parameters in conical centrifuge tubes were confirmed: sonication distance of 0.9 cm, sonication amplitude of 18%, and sonication time of 2 min. Under these conditions, the particle size of EONE was 18.96 ± 4.66 nm, the polydispersity index was 0.39 ± 0.09, and the zeta potential was −31.17 ± 2.15 mV. In addition, the changes in particle size, potential, micromorphology, and anti-Escherichia coli activity of EONE during digestion were investigated by in vitro simulated digestion. The emulsion was stable in simulated salivary fluid, tended to aggregate in simulated gastric fluid, and increased in particle size and potential value in simulated intestinal fluid. EONE showed higher anti-E. coli activity than EO by simulated digestion. These results provide a useful reference for the in vivo antimicrobial application of the essential oil.     

Sonochemical synthesis of nickel-manganous oxide nanocrumbs decorated partially reduced graphene oxide for efficient electrochemical reduction of metronidazole

In the present work, we report on the synthesis of crump-like nickel manganous oxide nanoparticles decorated partially reduced graphene oxide (NiMnO@pr-GO) nanocomposite through high-intensity ultrasonic bath sonication (ultrasonic frequency = 37 kHz and power = 150 W). The NiMnO@pr-GO nanocomposite modified glassy carbon electrode (GCE) was then employed for the electrochemical reduction of detrimental metronidazole (MNZ). The crystalline phase and formation of the NiMnO@pr-GO nanocomposites were confirmed by X-ray diffraction and other spectroscopic techniques. The cyclic voltammetry results demonstrate that this NiMnO@pr-GO nanocomposite modified GCE has a lower reduction potential and higher catalytic activity towards MNZ than do NiMnO and GO modified GCEs. Under optimized conditions, the fabricated NiMnO@pr-GO electrode can detect metronidazole over a wide linear range with a lower limit of detection of 90 nM. The sensitivity of the sensor was 1.22 µA µM^-1cm⁻² and was found to have excellent selectivity and durability for the detection of MNZ.     

Design of a new technique based on combination of ultrasound waves via magnetite solid phase and cloud point microextraction for determination of Cr(III) ions

In this work, we focused on development of a new techniques by coupling of ultrasound irradiation, cloud point method and magnetite solid phase microextraction for the extraction and preconcentration of Cr(III) ions from aqueous solutions. In order to reduce cost and improve practicability of proposed process a new efficient and regenerable magnetite sorbent (functionalized chitosan grafted-amino graphene oxide (GO) decorated by zinc ferrite nanoparticles (CS-GO-Zn: Fe₂O₄)) was synthesized through hydrothermal method and then characterized by FT-IR, FE-SEM, EDS and XRD analysis. Effect of initial sample volume and type, volume and concentration of eluent on the ER%_Cr(III) were investigated and optimized using one at a time method. Correlation between the main and interaction effects of other operational parameters such as Cr(III) ion concentration, CS-GO-Zn: Fe₂O₄ mass, sonication time, pH and solution temperature on the ER%_Cr(III) were investigated and optimized by central composite design coupled with desirability function approach. The results revealed that there were significant effects for most investigated terms on the ER%_Cr(III) and maximum ER% of 88.09% was obtained in desirability value of 1.0. This maximum efficiency was obtained at 0.035 µg/mL Cr(III) ion concentration, 40.16 °C temperature, 0.016 g of CS-GO-Zn: Fe₂O₄, pH 6.36 and 9.20 min sonication time. In addition, under the optimal conditions the linear range, limit of detection, enrichment factor and relative standard deviation were found to be 0.02–4.4 µg/mL, 0.002 µg/mL, 23.23 and 1.68% respectively. Finally, the method was successfully applied to the separation and preconcentration of Cr(III) ion from tap, river and mineral waters.     

Combining high intensity ultrasound and experimental design to improve carotenoid extraction efficiency from Buriti (Mauritia flexuosa)

Buriti (Mauritia flexuosa L.) is a significant source of carotenoids, but these compounds have been extracted using laborious and low-effective methods. The present work evaluated the high-intensity ultrasound combined with a chemometric approach to developing an optimal extraction method of carotenoids from buriti pulp. The multivariate optimization was carried out through two steps. First, a simplex-lattice mixture design was used to optimize the extractor solution finding higher extraction yield (903 ± 21 µg g⁻¹) with the acetone:ethanol (75/25) mixture. After, sample mass (80 mg) and sonication time (30 min) were optimized applying central composite design (CCD) which provided a 14% improvement in the extraction method yield. So, the total carotenoid content (TCC) with optimal extraction conditions was 1026 ± 13 µg g⁻¹ which is almost twice the yield of methods known in the literature for buriti. The RP-HPLC-DAD analysis revealed that the carotenoids are gently extracted and β-carotene is the major compound in the extracts. To confirm the accuracy, buriti samples spiked with β-carotene standard and the developed method showed recovery >84% and precision <6.5%. Furthermore, the optimized ultrasound-assisted extraction (UAE) method was applied to other samples (tomato, guava, carrot, mango, acerola, papaya, and pumpkin) and presented a yield to 5.5-fold higher when compared to the reported methods indicating high robustness. Based on results, the UAE method developed has demonstrated feasibility and reliability for the study of carotenoids in buriti pulp as well as in other plant matrices with high biological relevance.     

Sonochemical synthesis and anchoring of zinc oxide on hemin-mediated multiwalled carbon nanotubes-cellulose nanocomposite for ultra-sensitive biosensing of H2O2

In this work, the metal oxide and biopolymer nanocomposites on multiwalled carbon nanotubes (MWCNT) were prepared using a simple sonochemical method. The hexagonal nanorods of zinc oxide (ZnO NR) were synthesized by probe sonication (frequency = 20 kHz, amplitude = 50) method and were integrated on ultrasonically functionalized MWCNT-cellulose nanocrystals (MWCNT-CNC) for the first time. The stable hemin bio-composites also were prepared using the bath sonication (37 kHz of frequency, 150 W of power) method, and was used for the selective and ultrasensitive electrochemical detection of H₂O₂. The UV–Vis spectroscopy studies confirmed the presence of native hemin on MWCNT-CNC/ZnO NR nanocomposite. Cyclic voltammetry studies revealed that an enhanced redox electrochemical behaviour of hemin was observed on hemin immobilised MWCNT-CNC/ZnO NR nanocomposite than that of other hemin modified electrodes. Also, the MWCNT-CNC/ZnO NR/hemin modified SPCE showed 2.3 folds higher electrocatalytic activity with a lower reduction potential (−0.2 V) towards H₂O₂ than that of other investigated hemin modified electrodes including hemin/MWCNT and hemin/CNC-ZnO. The fabricated biosensor displayed a stable amperometric response (-0.2 V vs Ag/AgCl) in the linear concentration of H₂O₂ ranging up to 4183.3 µM with a lower detection limit of 4.0 nM.     

Fast femtosecond laser ablation for efficient cutting of sintered alumina substrates

Fast, accurate cutting of technical ceramics is a significant technological challenge because of these materials' typical high mechanical strength and thermal resistance. Femtosecond pulsed lasers offer significant promise for meeting this challenge. Femtosecond pulses can machine nearly any material with small kerf and little to no collateral damage to the surrounding material. The main drawback to femtosecond laser machining of ceramics is slow processing speed. In this work we report on the improvement of femtosecond laser cutting of sintered alumina substrates through optimisation of laser processing parameters. The femtosecond laser ablation thresholds for sintered alumina were measured using the diagonal scan method. Incubation effects were found to fit a defect accumulation model, with F_th,1=6.0 J/cm² (±0.3) and F_th,∞=2.5 J/cm² (±0.2). The focal length and depth, laser power, number of passes, and material translation speed were optimised for ablation speed and high quality. Optimal conditions of 500 mW power, 100 mm focal length, 2000 µm/s material translation speed, with 14 passes, produced complete cutting of the alumina substrate at an overall processing speed of 143 µm/s – more than 4 times faster than the maximum reported overall processing speed previously achieved by Wang et al. [1]. This process significantly increases processing speeds of alumina substrates, thereby reducing costs, making femtosecond laser machining a more viable option for industrial users.     

Resistant starch type 2 from lotus stem: Ultrasonic effect on physical and nutraceutical properties

Resistant starch type 2 (RS) was isolated from lotus stem using enzymatic digestion method. The isolated RS was subjected to ultrasonication (US) at different sonication power (100–400 W). The US treated and untreated RS samples were characterized using dynamic light scattering (DLS), scanning electron microscopy (SEM), light microscopy and Fourier transform infrared spectroscopy (FT-IR). DLS revealed that particle size of RS decreased from 12.80 µm to 413.19 nm and zeta potential increased from −12.34 mV to −26.09 mV with the increase in sonication power. SEM revealed smaller, disintegrated and irregular shaped RS particles after ultrasonication. FT-IR showed the decreased the band intensity at 995 cm⁻¹ and 1047 cm⁻¹ signifying that US treatment decreased the crystallinity of RS and increased its amorphous character. The bile acid binding, anti-oxidant and pancreatic lipase inhibition activity of samples also increased significantly (p < 0.05) with the increase in sonication power. Increase in US power however increased the values of hydrolysis from 23.11 ± 1.09 to 36.06 ± 0.13% and gylcemic index from 52.39 ± 0.38 to 59.50 ± 0.11. Overall, the non-thermal process of ultrasonic treatment can be used to change the structural, morphological and nutraceutical profile of lotus stem resistant starch which can have great food and pharamaceutical applications.     

Interaction of dioxouranium(VI) ion with EDTA at different ionic strengths

The formation of complex species of dioxouranium(VI) ion with EDTA was studied in the pH range of 1–3.5 and at 25 °C using a combination of potentiometric and spectrophotometric techniques. Results showed evidence for formation of the following species: [UO₂H₄EDTA]²⁺, [UO₂H₃EDTA]⁺, and [UO₂H₂EDTA]. Investigations were performed in sodium perchlorate as background electrolyte at 0.1, 0.3, 0.5, 0.7, and 1.0 mol dm^? 3. The parameters based on the formation constants were calculated, and the dependences of protonation and the stability constants on ionic strength are described. The dependence on ionic strength of the formation constants was analyzed using the specific ion interaction theory (SIT) model. The stability constant values at infinite dilution, obtained using SIT model, are log β°₁₄₁ = 6.77, log β°₁₃₁ = 5.99 and log β°₁₂₁ = 9.29, where indexes for the overall stability constant, β_pqr, refer to the equilibrium pUO₂²⁺ + qH⁺ + rL^4? ? M_pH_qL_r^{(2p + q ? 4r)}. The specific interaction coefficients are also reported.