Reduced graphene oxide (rGO) is widely utilised to develop various types of biosensors; however, producing self-assembled rGO nanoflake networks through single-droplet drop-casting remains inconsistent. In the present work, we systematically used three different methods to prepare rGO suspensions in order to produce large scale self-assembled rGO nanoflake networks through single-droplet drop-casting. The rGO suspensions were prepared using only deionised water with no added any chemicals/organic solvents, which we considered to be a low-cost method. Subsequently, the most effective preparation method was used to deposit rGO nanoflakes onto commercial gold interdigitated microelectrodes (Au-IDE) to examine their electrical performance. Assessment of the yields, developed methods, surface morphologies, spectroscopy and structural analyses of the as-prepared rGO nanoflakes were conducted. The results revealed that method-3 (involving sonication, centrifugation and post-sonication) produced large self-assembled rGO nanoflake networks with strong adhesion to glass substrates. Furthermore, the as-prepared rGO/Au-IDE modified sensors showed excellent electron mobility where the electrical conductivity was enhanced approximately ~ 1000 fold compared to the bare devices. The present work provided new insights for depositing large self-assembled interconnected rGO nanoflake networks through single-droplet drop-casting which will be beneficial for biosensor development and other downstream applications.
In this study, a simple sugaring-out supported by liquid biphasic flotation technique combined with ultrasonication was introduced for the extraction of proteins from microalgae. Sugaring-out as a phase separation method is novel and has been used in the extraction of metal ions, biomolecules and drugs. But, its functioning in protein separation from microalgae is still unknown. In this work, the feasibility of sugaring-out coupled with ultrasound for the extraction of protein was investigated. Primary studies were carried out to examine the effect of sonication on the microalgae cell as well as the separation efficiency of the integrated method. Effect of various operating parameters such as the concentration of microalgae biomass, the location of sonication probe, sonication time, ultrasonic pulse mode (includes varying ON and OFF duration of sonication), concentration of glucose, types of sugar, concentration of acetonitrile and the flow rate in the flotation system for achieving a higher separation efficiency and yield of protein were assessed. Besides, a large-scale study of the integration method was conducted to verify the consistency of the followed technique. A maximum efficiency (86.38%) and yield (93.33%) were attained at the following optimized conditions: 0.6% biomass concentration, 200 g/L of glucose concentration, 100% acetonitrile concentration with 5 min of 5 s ON/10 s OFF pulse mode and at a flow rate of 100 cc/min. The results obtained for large scale were 85.25% and 92.24% for efficiency and yield respectively. The proposed liquid biphasic flotation assisted with ultrasound for protein separation employing sugaring-out demonstrates a high production and separation efficiency and is a cost-effective solution. More importantly, this method provides the possibility of extending its application for the extraction of other important biomolecules.
The present study was conducted to examine the effects of sonication treatments (time intervals of 0, 15, 30, 45 and 60 min.) on phenolics and other antioxidant compounds in starfruits extracted in methanol and water. Overall, methanolic extracts exhibited significantly higher extractability, percentage inhibition of DPPH radicals, ferric reducing antioxidant property (FRAP) value, antioxidant capacity, flavonoids, total phenolics and tannins (p
In this study, the synthesis of Fe3O4@GO@g-C3N4 ternary nanocomposite for enhanced photocatalytic degradation of phenol has been investigated. The surface modification of Fe3O4 was performed through layer-by-layer electrostatic deposition meanwhile the heterojunction structure of ternary nanocomposite was obtained through sonicated assisted hydrothermal method. The photocatalysts were characterized for their crystallinity, surface morphology, chemical functionalities, and band gap energy. The Fe3O4@GO@g-C3N4 ternary nanocomposite achieved phenol degradation of ∼97%, which was significantly higher than that of Fe3O4@GO (∼75%) and Fe3O4 (∼62%). The enhanced photoactivity was due to the efficient charge carrier separation and desired band structure. The photocatalytic performance was further enhanced with the addition of hydrogen peroxide, in which phenol degradation up to 100% was achieved in 2 h irradiation time. The findings revealed that operating parameters have significant influences on the photocatalytic activities. It was found that lower phenol concentration promoted higher activity. In this study, 0.3 g of Fe3O4@GO@g-C3N4 was found to be the optimized photocatalyst for phenol degradation. At the optimized condition, the reaction rate constant was reported as 6.96 × 10-3 min-1. The ternary photocatalyst showed excellent recyclability in three consecutive cycles, which confirmed the stability of this ternary nanocomposite for degradation applications.
This study aimed to determine the total phenolics and antioxidant capacity of defatted dabai parts based on liquid extraction and optimized using response surface methodology (RSM). A two-level factorial design was applied to determine the effect of two independent variables (extraction time: X1 and % methanol: X2) on three response variables (total phenolic content: Y1, total flavonoid/anthocyanin content: Y2 and Trolox equivalent antioxidant capacity: Y3). The optimum conditions for extraction time and percent methanol were 36 min or 1 min and 62.25% or 53% for the defatted dabai pulp or peel, respectively. The RSM optimized extraction was compared with sonication-assisted extraction. Optimization results showed that defatted dabai parts had high total phenolic content and antioxidant capacity. Sonication-assisted extraction utilized the optimized extraction conditions had further increased the total phenolic content and antioxidant capacity of defatted dabai peel, but not in the pulp. Therefore, optimization of different extraction methods for the defatted fruit parts is recommended for future studies.
In this study, graphene oxide (Go) filled epoxy nanocomposites were prepared using hot pressed method. The GO was produced using modified Hummers' method. The produced GO at different compositions (0.1, 0.3 and 0.5 wt%) were mixed with epoxy before the addition of hardener using ultra-sonication. The produced epoxy nanocomposites were characterized in terms of mechanical and thermal properties. The mechanical properties of the nanocomposites were significantly enhanced by the addition of GO. About 50% of increment in the flexural strength of the composite sample filled with 03 wt% of GO as compared to the neat epoxy sample. However, only slight improvement in the impact strength of the composite were obtained by adding 0.1 wt% of GO.
In this present study, microalgal phycobiliproteins were isolated and purified via potential biphasic processing technique for pharmaceutical as well as food applications. The algal pre-treatment techniques were studied to enhance the yield of microalgal phycobiliproteins from the biomass. The proposed methods were optimised to obtain the best recovery yield of phycobiliproteins that can be isolated from the biomass. The phycobiliproteins were further purified using liquid biphasic system. The results showed that microalgal phycobiliproteins of high purity and yield was achieved using sonication treatment (20% power, 50% duty cycle and 7 min of irradiation time) with the biphasic system, where the purification fold of 6.17 and recovery yield of 94.89% was achieved. This work will provide insights towards the effective downstream processing of biomolecules from microalgae.
The aim of this work was to study the ultrasonication-assisted Liquid Tri-phasic Flotation (LTF) System to obtain lipid and protein from microalgae Chlorella sorokiniana in a single step as a novel process. In the current study, biorefinery of Chlorella sorokiniana was performed using LTF system in a single step. The highest protein recovery of 97.43 ± 1.67% and lipid recovery of 69.50 ± 0.54% were obtained. The corresponding parameters were microalgae biomass loading of 0.5 w/v%, ammonium sulphate concentration of 40 w/v%, volume ratio of 1:1.5 (salt:alcohol), ultrasonication pulse mode of 20 s ON/20 s OFF at 20% amplitude for 5 mins, flotation air flowrate of 100 mL/min. Additionally, recycling of alcohol phase to study the circular nature of proposed biorefinery was investigated. The proposed LTF system for extraction of proteins and lipid reduces the number of operation units required in this biorefinery approach.
The aim of this study was to determine the best parameter for extracting phenolic-enriched kenaf (Hibiscus cannabinus L.) seeds by a pulsed ultrasonic-assisted extraction. The antioxidant activities of ultrasonic-assisted kenaf seed extracts (KSE) were determined by a 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging capacity assay, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) radical scavenging assay, β -carotene bleaching inhibition assay, and ferric reducing antioxidant power (FRAP) assay. Total phenolic content (TPC) and total flavonoid content (TFC) evaluations were carried out to determine the phenolic and flavonoid contents in KSE. The KSE from the best extraction parameter was then subjected to high performance liquid chromatography (HPLC) to quantify the phenolic compounds. The optimised extraction condition employed 80% ethanol for 15 min, with the highest values determined for the DPPH, ABTS, and FRAP assay. KSE contained mainly tannic acid (2302.20 mg/100 g extract) and sinapic acid (1198.22 mg/100 g extract), which can be used as alternative antioxidants in the food industry.
Palm oil mill effluent (POME) is a highly contaminating wastewater due to its high chemical oxygen demand (COD) and biochemical oxygen demand (BOD). Conventional treatment methods require longer residence time (10-15 days) and higher operating cost. Owing to this, finding a suitable and efficient method for the treatment of POME is crucial. In this investigation, ultrasound cavitation technology has been used as an alternative technique to treat POME. Cavitation is the phenomenon of formation, growth and collapse of bubbles in a liquid. The end process of collapse leads to intense conditions of temperature and pressure and shock waves which assist various physical and chemical transformations. Two different ultrasound systems i.e. ultrasonic bath (37 kHz) and a hexagonal triple frequency ultrasonic reactor (28, 40 and 70 kHz) of 15 L have been used. The results showed a fluctuating COD pattern (in between 45,000 and 60,000 mg/L) while using ultrasound bath alone, whereas a non-fluctuating COD pattern with a final COD of 27,000 mg/L was achieved when hydrogen peroxide was introduced. Similarly for the triple frequency ultrasound reactor, coupling all the three frequencies resulted into a final COD of 41,300 mg/L compared to any other individual or combination of two frequencies. With the possibility of larger and continuous ultrasonic cavitational reactors, it is believed that this could be a promising and a fruitful green process engineering technique for the treatment of POME.
Ultrasonic treatment is an emerging food processing technology that has growing interest among health-conscious consumers. Freshly squeezed Chokanan mango juice was thermally treated (at 90 °C for 30 and 60s) and sonicated (for 15, 30 and 60 min at 25 °C, 40 kHz frequency, 130 W) to compare the effect on microbial inactivation, physicochemical properties, antioxidant activities and other quality parameters. After sonication and thermal treatment, no significant changes occurred in pH, total soluble solids and titratable acidity. Sonication for 15 and 30 min showed significant improvement in selected quality parameters except color and ascorbic acid content, when compared to freshly squeezed juice (control). A significant increase in extractability of carotenoids (4-9%) and polyphenols (30-35%) was observed for juice subjected to ultrasonic treatment for 15 and 30 min, when compared to the control. In addition, enhancement of radical scavenging activity and reducing power was observed in all sonicated juice samples regardless of treatment time. Thermal and ultrasonic treatment exhibited significant reduction in microbial count of the juice. The results obtained support the use of sonication to improve the quality of Chokanan mango juice along with safety standard as an alternative to thermal treatment.
In the present investigation, the operating efficiency of a bench-top air-driven microfluidizer has been compared to that of a bench-top high power ultrasound horn in the production of pharmaceutical grade nanoemulsions using aspirin as a model drug. The influence of important process variables as well as the pre-homogenization and drug loading on the resultant mean droplet diameter and size distribution of emulsion droplets was studied in an oil-in-water nanoemulsion incorporated with a model drug aspirin. Results obtained show that both the emulsification methods were capable of producing very fine nanoemulsions containing aspirin with the minimum droplet size ranging from 150 to 170 nm. In case of using the microfluidizer, it has been observed that the size of the emulsion droplets obtained was almost independent of the applied microfluidization pressure (200-600 bar) and the number of passes (up to 10 passes) while the pre-homogenization and drug loading had a marginal effect in increasing the droplet size. Whereas, in the case of ultrasound emulsification, the droplet size was generally decreased with an increase in sonication amplitude (50-70%) and period of sonication but the resultant emulsion was found to be dependent on the pre-homogenization and drug loading. The STEM microscopic observations illustrated that the optimized formulations obtained using ultrasound cavitation technique are comparable to microfluidized emulsions. These comparative results demonstrated that ultrasound cavitation is a relatively energy-efficient yet promising method of pharmaceutical nanoemulsions as compared to microfluidizer although the means used to generate the nanoemulsions are different.
Freshly squeezed kasturi lime fruit juice was sonicated (for 0, 30 and 60min at 20°C, 25kHz frequency) to evaluate its impact on selected physico-chemical and antioxidant properties, such as pH, °Brix, titratable acidity, Hunter color values (L(∗), a(∗), b(∗)), ascorbic acid, DPPH radical scavenging activity, total phenolics, antioxidant capacity, flavonoids and flavonols. Additionally, the effect of sonication treatments on the microbial load (TPC, yeast and mold) were also evaluated. Sonication of juice samples for 60min showed enhancement in most of the bioactive compounds compared to samples treated for 30min and control samples (untreated). Significant reductions in the microbial load corresponding to sonication time were also recorded. Results of the present study indicate that sonication may be employed as a suitable technique for kasturi lime juice processing, where antioxidant and other bioactive compound retention or enhancement is desired, along with the achievement of safety and quality standards.
5-Hydroxymethylfurfural (HMF) has been identified as a promising biomass-derived platform chemical. In this study, one pot production of HMF was studied in ionic liquid (IL) under probe sonication technique. Compared with the conventional heating technique, the use of probe ultrasonic irradiation reduced the reaction time from hours to minutes. Glucose, cellulose and local bamboo, treated with ultrasonic, produced HMF in the yields of 43%, 31% and 13% respectively, within less than 10min. The influence of various parameters such as acoustic power, reaction time, catalysts and glucose loading were studied. About 40% HMF yield at glucose conversion above 90% could be obtained with 2% of catalyst in 3min. Negligible amount of soluble by-product was detected, and humin formation could be controlled by adjusting the different process parameters. Upon extraction of HMF, the mixture of ionic liquid and catalyst could be reused and exhibited no significant reduction of HMF yield over five successive runs. The purity of regenerated [C4C1im]Cl and HMF was confirmed by NMR spectroscopy, indicating neither changes in the chemical structure nor presence of any major contaminants during the conversion under ultrasonic treatment. 13C NMR suggests that [C4C1im]Cl/CrCl3 catalyses mutarotation of α-glucopyranose to β-glucopyranose leading to isomerization and finally conversion to HMF. The experimental results demonstrate that the use of probe sonication technique for conversion to HMF provides a positive process benefit.
In this work, sonication (20-kHz) was conducted to assist the biosorption of phenolics from blueberry pomace extracts by brewery waste yeast biomass. The adsorption capacity of yeast increased markedly under ultrasonic fields. After sonication at 394.2 W/L and 40 °C for 120 min, the adsorption capacity was increased by 62.7% compared with that under reciprocating shaking. An artificial neural network was used to model and visualize the effects of different parameters on yeast biosorption capacity. Both biosorption time and acoustic energy density had positive influences on yeast biosorption capacity, whereas no clear influence of temperature on biosorption process was observed. Regarding the mechanism of ultrasound-enhanced biosorption process, the amino and carboxyl groups in yeast were considered to be associated with the yeast biosorption property. Meanwhile, ultrasound promoted the decline of the structure order of yeast cells induced by phenolic uptake. The interactions between yeast cells and phenolics were also affected by the structures of phenolics. Moreover, the mass transfer process was simulated by a surface diffusional model considering the ultrasound-induced yeast cell disruption. The modeling results showed that the external mass transfer coefficient in liquid phase and the surface diffusion coefficient under sonication at 394.2 W/L and 40 °C were 128.5% and 74.3% higher than that under reciprocating shaking, respectively.
O/W nanoemulsions are isotropic colloidal systems constituted of oil droplets dispersed in continuous aqueous media and stabilised by surfactant molecules. Nanoemulsions hold applications in more widespread technological domains, more crucially in the pharmaceutical industry. Innovative nanoemulsion-based drug delivery system has been suggested as a powerful alternative strategy through the useful means of encapsulating, protecting, and delivering the poorly water-soluble bioactive components. Consequently, there is a need to generate an emulsion with small and consistent droplets. Diverse studies acknowledged that ultrasonic cavitation is a feasible and energy-efficient method in making pharmaceutical-grade nanoemulsions. This method offers more notable improvements in terms of stability with a lower Ostwald ripening rate. Meanwhile, a microstructured reactor, for instance, microchannel, has further been realised as an innovative technology that facilitates combinatorial approaches with the acceleration of reaction, analysis, and measurement. The recent breakthrough that has been achieved is the controlled generation of fine and monodispersed multiple emulsions through microstructured reactors. The small inner dimensions of microchannel display properties such as short diffusion paths and high specific interfacial areas, which increase the mass and heat transfer rates. Hence, the combination of ultrasonic cavitation with microstructures (microchannel) provides process intensification of creating a smaller monodispersed nanoemulsion system. This investigation is vital as it will then facilitate the creation of new nanoemulsion based drug delivery system continuously. Following this, the fabrication of microchannel and setup of its combination with ultrasound was conducted in the generation of O/W nanoemulsion, as well as optimisation to analyse the effect of varied operating parameters on the mean droplet diameter and dispersity of the nanoemulsion generated, besides monitoring the stability of the nanoemulsion. Scanning transmission electron microscopy (STEM) images were also carried out for the droplet size measurements. In short, the outcomes of this study are encouraging, which necessitates further investigations to be carried out to advance a better understanding of coupling microchannel with ultrasound to produce pharmaceutical-grade nanoemulsions.
Phenolic acids of oak gall were extracted using ultrasonic-probe assisted extraction (UPAE) method in the presence of ionic liquid. It was compared with classical ultrasonic-bath assisted extraction (CUBAE) and conventional aqueous extraction (CAE) method, with and without the presence of ionic liquid. Remarkably, the UPAE method yielded two-fold higher extraction yield with the presence of ionic liquid, resulting 481.04 mg/g for gallic acids (GA) and 2287.90 mg/g for tannic acids (TA), while a decreased value of 130.36 mg/g for GA and 1556.26 mg/g for TA were resulted with the absence of ionic liquid. Intensification process resulted the highest yield of 497.34 mg/g and 2430.48 mg/g for GA and TA, respectively, extracted at temperature 50 °C with sonication intensity of 8.66 W/cm2 and 10% duty cycle, diluted in ionic liquid, 1-Butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, [Bmim][Tf2N] at concentration of 0.10 M with sample-to-solvent ratio 1:10 for 8 h. Peleg's model successfully predicted the UPAE process confirming that extraction capacity is the controlling factor in extracting phenolic acids. Hence, it can be concluded that UPAE method and ionic liquid have synergistic effect as it effectively enhanced the extraction efficiency to increase the bioactive constituents yield.
Recently, chitin and chitosan are widely investigated for food preservation and active packaging applications. Chemical, as well as biological methods, are usually adopted for the production of these biopolymers. In this study, modification to a chemical method of chitin synthesis from shrimp shells has been proposed through the application of high-frequency ultrasound. The impact of sonication time on the deproteinization step of chitin and chitosan preparation was examined. The chemical identities of chitin and chitosan were verified using infrared spectroscopy. The influence of ultrasound on the deacetylation degree, molecular weight and particle size of the biopolymer products was analysed. The microscopic characteristics, crystallinity and the colour characteristics of the as-obtained biopolymers were investigated. Application of ultrasound for the production of biopolymers reduced the protein content as well as the particle size of chitin. Chitosan of high deacetylation degree and medium molecular weight was produced through ultrasound assistance. Finally, the as-derived chitosan was applied for beef preservation. High values of luminosity, chromatid and chrome were noted for the beef samples preserved using chitosan films, which were obtained by employing biopolymer subjected to sonication for 15, 25 and 40 min. Notably; these characteristics were maintained even after ten days of packaging. The molecular weight of these samples are 73.61 KDa, 86.82 KDa and 55.66 KDa, while the deacetylation degree are 80.60%, 92.86% and 94.03%, respectively; in the same order, the particle size of chitosan are 35.70 μm, 25.51 μm and 20.10 μm.
Hybridisation plays a significant role in the evolution and diversification of plants. Hybridisation among Nepenthes species is extensive, either naturally or man-made. To investigate the effects of hybridisation on the chemical compositions, we carried out metabolomics study on pitcher tissue of Nepenthes ampullaria, Nepenthes rafflesiana and their hybrid, Nepenthes × hookeriana. Pitcher samples were harvested and extracted in methanol:chloroform:water via sonication-assisted extraction before analysed using LC-TOF-MS. MS data were analysed using XCMS online version 2.2.5. This is the first MS data report towards the profiling, identification and comprehensive comparison of metabolites present in Nepenthes species.