Process optimization and stability of D-limonene-in-water nanoemulsions prepared by ultrasonic emulsification using response surface methodology

d-limonene in water nanoemulsion was prepared by ultrasonic emulsification using mixed surfactants of sorbitane trioleate and polyoxyethylene (20) oleyl ether. Investigation using response surface methodology revealed that 10% d-limonene nanoemulsions formed at S₀ ratio (d-limonene concentration to mixed surfactant concentration) 0.6-0.7 and applied power 18 W for 120 s had droplet size below 100 nm. The zeta potential of the nanoemulsion was approximately −20 mV at original pH 6.4, closed to zero around pH 4.0, and around −30 mV at pH 12.0. The main destabilization mechanism of the systems is Ostwald ripening. The ripening rate at 25 °C (0.39 m³ s⁻¹ × 10²⁹) was lower than that at 4 °C (1.44 m³ s⁻¹ × 10²⁹), which was in agreement with the Lifshitz-Slezov-Wagner (LSW) theory. Despite of Ostwald ripening, the droplet size of d-limonene nanoemulsion remained stable after 8 weeks of storage.     

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.     

Modification in structural,physicochemical, functional,and in vitro digestive properties of kiwi starch by high-power ultrasound treatment

Kiwi starch (KS) is a fruit-derived starch; in order to improve its processing performance and increase its added value, it is necessary to modify KS to enhance the positive attributes and to enlarge its application. In this study, KS was modified by high-power ultrasound treatment (HUT) to reveal the relationship between the structure and function of KS with different treatment powers (0, 200, 400, and 600 W) and different treatment times (0, 10, 20, and 30 min). The results showed that HUT destroyed the granular morphology of KS, formed holes and cracks on the surface, and reduced the particle size and the short-range molecular order of KS. After different HUTs, the apparent amylose content (AAC), swelling power (SP), water solubility index (WSI), viscosity and setback value (SB) of KS were significantly increased, while the gelatinization temperature was significantly decreased. In addition, HUT significantly reduced the content of rapidly digestible starch (RDS) and slowly digestible starch (SDS), while it significantly enhanced the content of resistant starch (RS) (64.08–72.73%). In a word, HUT as a novel physical modification method for KS, enlarged its application, and fulfilled different demands of a starch-based product, which introduces another possibility for kiwi fruit further processing.     

Preparation and characterization of type 3 resistant starch by ultrasound-assisted autoclave gelatinization and its effect on steamed bread quality

In this study, we aimed to establish an innovative and efficient preparation method of potato resistant starch (PRS). To achieve this, we prepared type 3 resistant starch (RS3) from native potato starch (PS) using an ultrasonic method combined with autoclave gelatinization and optimized by the response surface method to study the structure and properties of potato RS3 (PRS3) and its effect on the quality of steamed bread. Under optimal treatment conditions, the PRS3 content increased from 7.5% to 15.9%. Compared with PS, the B-type crystal structure of PRS3 was destroyed, and the content of hydroxyl groups was increased, but no new chemical groups were introduced. PRS3 had a rougher surface and a lower crystallinity, gelatinization temperature, viscosity, setback value, and breakdown value. The low content (5%) of PRS3 had a stable viscosity and was easily degraded by bacteria, which can improve the quality of steamed bread to a certain extent. When the PRS3 content was over 10%, it competed with the gluten protein to absorb water, which reduced the contents of β-turn and α-helix in the dough, increased the contents of β-fold, and weakened the structure of the gluten network. It also decreased the specific volume and elasticity of the steamed bread and increased the spreading rate, hardness, and chewiness. Steamed bread prepared with a flour mixture containing 5% PRS3 was similar to the presidential acceptance of control flour. In this study, a new sustainable and efficient PRS3 preparation method was established, which has certain guiding significance for the processing of Functional steamed bread with high-resistant starch.     

Preparation and characterization of highly lipophilic modified potato starch by ultrasound and freeze-thaw treatments

In order to explore the potential application of combined physical treatment in producing highly lipophilic modified starch, the effects of ultrasound combined with freeze-thaw treatment on the microstructure and physicochemical properties of potato starch were investigated. The samples treated by combined treatment had the roughest structure and the oil adsorptive capacity value increased from 59.62% (native starch, NS) to 80.2% (7 cycles of ultrasound-freeze-thaw treatment starch, 7UT-FTS). Compared to NS, the crystalline type and chemical groups of modified starches did not change, but the relative crystallinity, enthalpy change, and paste viscosity decreased to varying degrees, while the gelatinization temperature increased. The digestibility of raw modified starch was higher than that of NS, but this phenomenon disappeared after gelatinization. 7UT-FTS showed better resist-digestibility than NS after encapsulating oil. Hence, this would be an efficient and environmentally friendly way to produce modified starch with safety, highly lipophilic and heat resistance.     

Modulating the in vitro digestibility of chemically modified starch ingredient by a non-thermal processing technology of ultrasonic treatment

Chemically modified starch (RS4) was commercially available as a food ingredient, however, there was a lack of knowledge on how ultrasonic treatment (non-thermal technology) modulated the enzymatic resistance of RS4. In this study, structural change of RS4 during ultrasonic treatment and its resulting digestibility was investigated. Results from scanning electron microscopy, particle size analysis, chemical composition analysis, X-ray diffraction, differential scanning calorimetry, and Fourier transform infrared spectroscopy showed that ultrasonic treatment remained the granule morphology, increased the apparent amylose content, reduced the particle size, destroyed the crystalline structure, decreased the helical orders, but enhanced the short-range molecular orders of ultrasonic-processed RS4. In vitro digestibility analysis showed that the total content of rapidly digestible starch and slowly digestible starch was increased, whereas the content of resistant starch was decreased. Overall, ultrasonic treatment substantially reduced the enzymatic resistance of RS4, indicating that RS4 was not stability against the non-thermal processing technology of ultrasonic treatment.     

Physicochemical,structural, and digestive properties of pea starch obtained via ultrasonic-assisted alkali extraction

As a new and clean extraction technology, ultrasonic extraction has been demonstrated with great potential in the preparation of modified starch. In order to increase its added value, it is necessary to modify pea starch to enlarge its application. In this study, the efficiency of combining ultrasonic with alkali in the extraction of pea starch was evaluated and compared to conventional alkali extraction. Ultrasonic-assisted alkali extraction conditions were optimized using single-factor experiments and response surface methodology. The results revealed that maximum yield of pea starch (54.43 %) was achieved using ultrasound-assisted alkali extraction under the following conditions: sodium hydroxide solution with a concentration of 0.33 %, solid/alkali solution ratio of 1:6 (w/v), ultrasonic power of 240 W, temperature of 42 °C, and extraction time of 22 min. The ultrasound-assisted alkali extraction yielded 13.72 % greater pea starch than conventional alkali extraction. On the other hand, morphological, structural, and physicochemical properties of the obtained starch isolates were evaluated. The ultrasound-assisted alkali extraction resulted in pea starch with greater amylose content, water-solubility, swelling power, and viscosity compared with conventional alkali extraction. Furthermore, ultrasonication influenced the morphological properties of pea starch granules, while the molecular structure and crystal type were not affected. Moreover, the ultrasonic-assisted extraction produced starch with a slightly greater resistant starch content. Therefore, ultrasonic-assisted extraction can be suggested as a potential method for extracting pea starch with improved functional properties.     

Structural and physicochemical characterization of modified starch from arrowhead tuber (Sagittaria sagittifolia L.) using tri-frequency power ultrasound

Sagittaria sagittifolia L. is a well-known plant, belongs to the Alismataceae family. Sonication can improve the functional properties of starch; hence, the aim of this study was to develop ultrasonically modified arrowhead starch (UMAS) using a sophisticated and eco-friendly tri-frequency power ultrasound (20/40/60 kHz) method at 300, 600, and 900 W for 15 and 30 min. Significant (p < 0.05) increases in swelling power, solubility, and water and oil holding capacities were achieved. FTIR spectroscopy corroborated the ordered, amorphous, and hydrated crystals of the sonicated samples. Increases in sonication frequency and power led to significant (p < 0.05) increases in onset gelatinization temperatures. Scanning electron microscopic analysis of sonicated samples showed superficial cracks and roughness on starch granules appeared in a sonication power-dependent manner compared with that of untreated sample. Overall, the ultrasonically-treated samples showed improved physicochemical properties, which could be useful for industrial applications.     

Process optimization and characterization of arachidonic acid oil degumming using ultrasound-assisted enzymatic method

Ultrasound assisted enzymatic method was applied to the degumming of arachidonic acid (ARA) oil produced by Mortierella alpina. The conditions of degumming process were optimized by response surface methodology with Box- Behnken design. A dephosphorization rate of 98.82% was achieved under optimum conditions of a 500 U/kg of Phospholipase A₁ (PLA₁) dosage, 2.8 mL/100 g of water volume, 120 min of ultrasonic time, and 135 W of ultrasonic power. The phosphorus content of ultrasonic assisted enzymatic degumming oil (UAEDO) was 4.79 mg/kg, which was significantly lower than that of enzymatic degumming oil (EDO, 17.98 mg/kg). Crude Oil (CO), EDO and UAEDO revealed the similar fatty acid compositions, and ARA was dominated (50.97 ~ 52.40%). The oxidation stability of UAEDO was equivalent to EDO and weaker than CO, while UAEDO presented the strongest thermal stability, followed by EDO and CO. Furthermore, aldehydes, acids and alcohols were identified the main volatile flavor components for the three oils. The proportions of major contributing components such as hexanal, nonanal, (E)-2-nonanal, (E, E)-2,4-decadienal, (E)-2-nonenal and aldehydes in UAEDO and EDO were all lower than CO. Overall, Ultrasound assisted enzymatic degumming proved to be an efficient and superior method for degumming of ARA oil.     

Ferulic acid loaded pickering emulsions stabilized by resistant starch nanoparticles using ultrasonication: Characterization,in vitro release and nutraceutical potential

The use of starch based nanoparticles have gained momentum in stabilizing pickering emulsions for it’s numerous advantages. In present study resistant starch (RS) was isolated from lotus stem using enzymatic digestion and subjected to nanoprecipitation and ultrasonication to yield resistant starch nanoparticles (RSN). RSN of varying concentrations (2%, 10% and 20%) were used to stabilize the flax seed-oil water mixture to form pickering emulsions. The emulsions were used to nanoencapsulate ferulic acid (FA) – a well known bioactive via ultrasonication. The emulsions were lyophilized to form FA loaded lyophilized pickering emulsion (FA-LPE). The FA-LPE (2%, 10 % and 20%) were characterized using dynamic light scattering (DLS), light microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM) and attenuated total reflectance fourier transform infra-spectroscopy (ATR-FTIR). AFM showed FA-LPE as spherical droplets embedded in the matrix with maximum peak height of 8.47 nm and maximum pit height of 1.69 nm. SEM presented FA-LPE as an irregular and continuous surface having multiple folds and holes. The ATR-FTIR spectra of all the samples displayed peaks of C = C aromatic rings of FA at 1600 cm⁻¹ and 1439 cm⁻¹, signifying successful encapsulation. In vitro release assay displayed more controlled release of FA from FA-LPE (20%). Bioactivity of FA-LPE was evaluated in terms of anti-cancer, anti-diabetic, angiotensin converting enzyme (ACE) inhibition and prevention against oxidative damage under simulated gastro-intestinal conditions (SGID). The bioactivity of FA-LPE (20%) was significantly higher than FA-LPE (2%) and FA-LPE (10%). Key findings reveal that pickering emulsions can prevent FA under harsh SGID conditions and provide an approach to facilitate the design of pickering emulsions with high stability for nutraceutical delivery in food and supplement products.     

Ultrasonic-assisted binding of canistel (Lucuma nervosa A.DC) seed starch with quercetin

In order to provide a reference for improving the physicochemical properties of starch, the study of starch polyphenol complex interaction has aroused considerable interest. As a common method of starch modification, ultrasound can make starch granules have voids and cracks, and make starch and polyphenols combine more closely. In this research, canistel seed starch was modified by ultrasonic treatment alone or combined with quercetin. The molecular structure, particle characteristics and properties of starch were evaluated. With the increase of ultrasonic temperature, the particle size of the dextrinized starch granules increased, but the addition of quercetin could protect the destruction of starch granule size by ultrasonic; X-ray diffraction and infrared spectra indicated that quercetin was bound to the surface of canistel seed starch through hydrogen bonding, and the complex and the original starch had the same crystal structure and increased crystallinity; by molecular simulation, quercetin bound inside the starch molecular helix preserved the crystalline helical configuration of starch to some extent and inhibited the complete unhelicalization of starch molecules. Meanwhile, hydrogen bonding was the main driving force for the binding of starch molecules to quercetin, and van der Waals interactions also promoted the binding of both. In the physicochemical properties, as the temperature increased after the combination of ultrasonic modified starch combined with quercetin, the solubility, swelling force and apparent viscosity of the compound increased significantly, and it has higher stability and shear resistance.     

The effect of surface modification on the properties of sisal fiber and improvement of interfacial adhesion in sisal/starch composites induced by starch nanocrystals

A facile approach was utilized to introduce starch nanocrystals (SNCs) onto sisal fiber (SF) to improve the interfacial adhesion between SF and starch. For this, fibers were treated with alkali and then subjected to cold plasma treatment to increase the accessibility with SNCs, which was confirmed through X-ray photoelectron spectroscopy (XPS). It was found that due to the influence of cold plasma treatment, new functional groups were introduced onto SF. The surface characteristics of SF were examined by Fourier transform infrared spectroscopy (FTIR) and Scanning electron microscopy (SEM). The observed results suggested that SNCs were successfully distributed onto SF. Tensile strength and interfacial shear strength of fibers treated under different conditions were calculated and compared through a two-parameter Weibull model. The highest interfacial shear strength of 3.05 MPa was obtained by Alkali-300 W-SNCs, which indicated an increase of 80.6% than untreated SF. It has also been proved that the starch nanocrystals produced hydrogen bonding and physical interlocking between sisal fiber and starch. Notably, the outcome of this investigation indicates that SNCs may be applied for the fabrication of high performance, environmentally friendly sisal/starch composites for a range of technological applications.     

Sonodynamic inactivation of methicillin-resistant Staphylococcus aureus in planktonic condition by curcumin under ultrasound sonication

Methicillin-Resistant Staphylococcus aureus (MRSA) is an important cause of difficult-to-treat infections. The present study aims to investigate sonodynamic inactivation of MRSA in planktonic condition using curcumin under ultrasound sonication. Dark toxicity of curcumin to MRSA was investigated to choose the concentration range of curcumin used in the study. The uptake of curcumin in MRSA was observed before ultrasound sonication. After sonication colony forming units (CFUs) and bacterial viability were investigated using fluorescence assay. Additionally, chromosomal DNA fragmentation was also analyzed. Curcumin showed no dark toxicity to MRSA in the concentration range of ?500 μM. The maximum uptake of curcumin in MRSA occurred in 50 min after curcumin incubation. Counting of CFUs showed that curcumin had significantly sonodynamic killing effect on MRSA in a curcumin dose-dependent manner, and 5-log reduction in CFU was observed after curcumin treatment (40 μM) at room temperature in the dark for 50 min followed by exposure to ultrasound with intensity of 1.56 W/cm² for 5 min. The ratio of green-fluorescent intensity to red-fluorescent intensity was obviously decreased after curcumin treatment under ultrasound sonication. No significant change in chromosomal DNA was found in the cultured MRSA after the combined treatment of curcumin and ultrasound. These results demonstrated that sonodynamic action of curcumin had significant inactivation of MRSA in planktonic condition.     

Activation of microbubbles by low-intensity pulsed ultrasound enhances the cytotoxicity of curcumin involving apoptosis induction and cell motility inhibition in human breast cancer MDA-MB-231 cells

Ultrasound and microbubbles-mediated drug delivery has become a promising strategy to promote drug delivery and its therapeutic efficacy. The aim of this research was to assess the effects of microbubbles (MBs)-combined low-intensity pulsed ultrasound (LPUS) on the delivery and cytotoxicity of curcumin (Cur) to human breast cancer MDA-MB-231 cells. Under the experimental condition, MBs raised the level of acoustic cavitation and enhanced plasma membrane permeability; and cellular uptake of Cur was notably improved by LPUS–MBs treatment, aggravating Cur-induced MDA-MB-231 cells death. The combined treatment markedly caused more obvious changes of cell morphology, F-actin cytoskeleton damage and cell migration inhibition. Our results demonstrated that combination of MBs and LPUS may be an efficient strategy for improving anti-tumor effect of Cur, suggesting a potential effective method for antineoplastic therapy.     

Ultrasound-assisted solution crystallization of fotagliptin benzoate: Process intensification and crystal product optimization

The ultrasound-assisted crystallization process has promising potentials for improving process efficiency and modifying crystalline product properties. In this work, the crystallization process of fotagliptin benzoate methanol solvate (FBMS) was investigated to improve powder properties and downstream desolvation/drying performance. The direct cooling/antisolvent crystallization process was conducted and then optimized with the assistance of ultrasonic irradiation and seeding strategy. Direct cooling/antisolvent crystallization and seeding crystallization processes resulted in needle-like crystals which are undesirable for downstream processing. In contrast, the ultrasound-assisted crystallization process produced rod-like crystals and reduced the crystal size to facilitate the desolvation of FBMS. The metastable zone width (MSZW), induction time, crystal size, morphology, and process yield were studied comprehensively. The results showed that both the seeding and ultrasound-assisted crystallization process (without seeds) can improve the process yield and the ultrasound could effectively reduce the crystal size, narrow the MSZW, and shorten the induction time. Through comparing the drying dynamics of the FBMS, the small rod-shaped crystals with a mean size of 9.6 μm produced by ultrasonic irradiation can be completely desolvated within 20 h, while the desolvation time of long needle crystals with an average size of about 157 μm obtained by direct cooling/antisolvent crystallization and seeding crystallization processes is more than 80 h. Thus the crystal size and morphology were found to be the key factors affecting the desolvation kinetics and the smaller size produced by using ultrasound can benefit the intensification of the drying process. Overall, the ultrasound-assisted crystallization showed a full improvement including crystal properties and process efficiency during the preparation of fotagliptin benzoate desolvated crystals.     

Mapping of the cationic starch adsorbed on pulp fibers by ToF-SIMS

Cationic starch (CS) is routinely used in the papermaking process to improve the dry strength or printability of paper. The effectiveness depends on the distribution of the starch on the pulp fiber, and in this study, time-of-flight secondary ion mass spectrometry was used to investigate this distribution. The characteristic peak at 58m/z was applied to map the CS. Based on the imaging analysis of the handsheets with the CS as an internal additive, the distribution of CS became more uniform with decreasing freeness. The amount of adsorbed CS increased with increasing fiber length and was lower on vessels than on other fibers. These results were related to fibrillation. From the analysis of handsheets with CS as an external additive, the penetration depth of the starch into base paper increased with decreases in the sizing degree of the base paper.     

Effect of ultrasound on keratin valorization from chicken feather waste: Process optimization and keratin characterization

Chicken feather (CF) has been deemed as one of the main poultry byproducts with a large amount produced globally. However, the robust chemical nature of chicken feathers has been limiting in its wide-scale utilization and valorization. The study proposed a strategy of keratin regeneration from chicken feather combining ultrasound and Cysteine (Cys)-reduction for keratin regeneration. First, the ultrasonic effect on feather degradation and keratin properties was systematically explored based on Cys-reduction. Results showed that the feather dissolution was significantly improved by increasing both ultrasonic time and power, and the former had a greater impact on keratin yield. However, the treatment time over 4 h led to a decrease of keratin yield, producing more soluble peptides, > 9.7 % of which were < 0.5 kDa. Meanwhile, prolonging time decreased the thermal stability with weight loss at a lower temperature and amino acids content (e.g., Ser, Pro and Gly) of keratin. Conversely, no remarkable damage in chemical structure and thermal stability of regenerated keratin was observed by only increasing ultrasonic power, while the keratin solubility was notably promoted and reached 745.72 mg·g⁻¹ in NaOH (0.1 M) solution (400 W, 4 h). The regenerated keratin under optimal conditions (130 W, 2.7 h, and 15 % of Cys) possessed better solubility while without obvious damage in chemical structure, thermal stability, and amino acids composition. The study illustrated that ultrasound physically improved CF degradation and keratin solubility without nature damage and provided an alternative for keratin regeneration involving no toxic reagent, probably holding promise in the utilization and valorization of feather waste.     

Nanoemulsification of soybean oil using ultrasonic microreactor: Process optimization,scale-up and numbering-up in series

Ultrasonically-induced nanoemulsions have been widely investigated for the development of functional food, cosmetics, and pharmaceuticals due to ideal droplet sizes (DS), low polydispersity index (PDI), and superior physical stability. However, a series of frequently-used ultrasonic set-ups mainly suffered from a low ultrasonic energy efficiency caused by the large acoustic impedance and energy consumption, subordinately confronted with a low throughput, complicated fabrication with complex structure and weak ultrasonic cavitation. Herein, we employed a typical ultrasonic microreactor (USMR) that ensured the high-efficient energy input and generated intense cavitation behavior for efficient breakage of droplets and continuous production of unified oil-in-water (O/W) nanoemulsions in a single cycle and without any pre-emulsification treatment. The emulsification was optimized by tuning the formula indexes, technological parameters, and numerical analysis using Response Surface Methodology (RSM), followed by a comparison with the emulsification by a traditional ultrasonic probe. The USMR exhibited superior emulsification efficiency and easy scale-up with remarkable uniformity by series mode. In addition, concurrent and uniform nanoemulsions with high throughput could also be achieved by a larger USMR with high ultrasonic power. Based on RSM analysis, uniform DS and PDI of 96.4 nm and 0.195 were observed under the optimal conditions, respectively, well consistent with the predicted values. Impressively, the optimal nanoemulsions have a uniform spherical morphology and exhibited superior stability, which held well in 45 days at 4℃ and 25℃. The results in the present work may provide a typical paradigm for the preparation of functional nanomaterials based on the novel and efficient emulsification tools.     

Investigation of zinc powder modified by ultrasonic impregnation of rare earth lanthanum

Different lanthanum conversion films coated directly on zinc particles are prepared by ultrasonic impregnation with the variable concentration of lanthanum nitrate solution and the adjusted ultrasonic time to modify zinc powder, and the characterization as well as electrochemical behavior of zinc are analyzed using scanning electron microscopy, energy dispersion spectrometry, potentiodynamic polarization, cyclic voltammetry. The lanthanum conversion films are found to enhance the property of corrosion resistance, suppress the dendritic growth and reduce the capacity loss for zinc electrode made of such modified zinc powder. Furthermore, the particle size of zinc powder immersed in lanthanum nitrate solution becomes thin and slim under the effect of ultrasound, which is beneficial to improve the electrochemical reaction activity of zinc powder at the assurance of high corrosion resistance for zinc electrode.     

正交试验法优选都梁凝胶贴剂的提取工艺

采用超声法优选都梁凝胶贴剂中白芷、川芎药对的最佳提取工艺.按照L9（34）正交试验设计,以欧前胡素、阿魏酸的转移率及干浸膏得率为综合评价指标,用高效液相色谱法进行含量测定.结果表明,都梁凝胶贴剂中白芷、川芎药对的最佳超声提取工艺为：8倍量的80％乙醇提取2次,每次超声40min;此时浸膏中欧前胡素的平均含量为0.1379％,阿魏酸的平均含量为0.1410％.本实验所建立的高效液相色谱法的准确度、精密度与重现性良好;提取工艺简便,合理.