Production of Kudzu Starch Gels with Superior Mechanical and Rheological Properties through Submerged Ethanol Exposure and Implications for In Vitro Digestion.

Producing starch gels with superior mechanical attributes remains a challenging pursuit. This research sought to develop a simple method using ethanol exposure to produce robust starch gels. The gels' mechanical properties, rheology, structural characteristics, and digestion were assessed through textural, rheological, structural, and in vitro digestion analyses. Our investigation revealed an improvement in the gel's strength from 62.22 to178.82 g. The thermal transitions were accelerated when ethanol was elevated. The exposure to ethanol resulted in a reduction in syneresis from 11% to 9.5% over a period of 6 h, with noticeable changes in size and color. Rheologically, the dominating storage modulus and tan delta (<0.55) emphasized the gel's improved elasticity. X-ray analysis showed stable B- and V-type patterns after ethanol exposure, with relative crystallinity increasing to 7.9%. Digestibility revealed an ethanol-induced resistance, with resistant starch increasing from 1.87 to 8.73%. In general, the exposure to ethanol played a crucial role in enhancing the mechanical characteristics of kudzu starch gels while simultaneously preserving higher levels of resistant starch fractions. These findings have wide-ranging implications in the fields of confectioneries, desserts, beverages, and pharmaceuticals, underscoring the extensive academic and industrial importance of this study.

Starches modification with rose polyphenols under multi-frequency power ultrasonic fields: Effect on physicochemical properties and digestion behavior.

As the main source of energy for human beings, starch is widely present in people's daily diet. However, due to its high content of rapidly digestive starch, it can cause a rapid increase in blood glucose after consumption, which is harmful to the human body. In the current study, the complexes made from edible rose polyphenols (ERPs) and three starches (corn, potato and pea) with different typical crystalline were prepared separately by multi-frequency power ultrasound (MFPU). The MFPU includes single-frequency modes of 40, 60 kHz and dual-frequency of 40 and 60 kHz in sequential and simultaneous mode. The results of the amount of complexes showed that ultrasound could promote the formation of polyphenol-starch complexes for all the three starches and the amount of ERPs in complexes depended on the ultrasonic parameters including treatment power, time and frequency. Infrared spectroscopy and X-ray diffraction indicated that ERPs with or without ultrasound could interact with the three starches through non-covalent bonds to form non-V-type complexes. Scanning electron microscopy showed that the shape of starches changed obviously from round/oval to angular and the surface of the starches were no longer smooth and appeared obvious pits, indicating that the ultrasonic field destroyed the structure of starches. In addition, compared to the control group, the in vitro digestibility study with 40/60 kHz sonication revealed that ultrasonic treatment greatly improved the digestive properties of the polyphenol-starch complexes by significantly increasing the content of resistant starch (20.31%, 17.27% and 14.98%) in the three starches. Furthermore, the viscosity properties of the three starches were all decreased after ERPs addition and the effect was enhanced by ultrasound both for single- and dual-frequency. In conclusion, ultrasound can be used as an effective method for preparing ERPs-starch complexes to develop high value-added products and low glycemic index (GI) foods.

Individual and synergistic effect of multi-frequency ultrasound and electro-infrared pretreatments on polyphenol accumulation and drying characteristics of edible roses.

The freeze-dried (FD) edible roses with high content of bioactive substances and superior flavor have been favored by consumers. Nevertheless, the development of freeze-dried rose industry has been plagued by a long drying time and low efficiency. This study investigated the effects of ultrasonic pretreatment (UP) in multi-frequency modes and electro-infrared pretreatment (EIP) prior to FD on polyphenol accumulation and drying characteristics of roses. The mechanism was explored by the changes in microstructure, equivalent circuit parameters, and phenol identifications of rose. The results showed that the FD time of roses decreased by 26 % after ultrasonic-infrared sequential synergistic pretreatment (UP + EIP) due to the damage of cell membrane permeability from UP. The quality attributes of UP + EIP products including color, phenols, and antioxidant activity (DPPH and ABTS radical scavenging rates) remarkably improved. UP + EIP significantly (p < 0.05) increased the content of polyphenols, namely quercetin-3ß-d-glucoside, phlorizin, procyanidin B2, gallicacid, and rutin in the FD roses quantified by ultra-high performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-qTOF-MS/MS). Therefore, UP + EIP is an effective pretreatment method for shortening FD time and producing high-quality FD rose products with enhanced polyphenol content.

Effect of Multi-Mode Thermosonication on the Microbial Inhibition and Quality Retention of Strawberry Clear Juice during Storage at Varied Temperatures.

Strawberry juice, which is rich in nutrients and charming flavor, is favored by consumers. To explore whether multi-mode thermosonication (MTS) can ensure the quality stability of strawberry clear juice (SCJ) during storage, the effects of microbial inhibition, enzyme activity, and physicochemical properties of SCJ pretreated by MTS were evaluated during storage at 4, 25, and 37 °C in comparison with thermal pretreatment (TP) at 90 °C for 1 min. The MTS, including dual-frequency energy-gathered ultrasound pretreatment (DEUP) and flat sweep-frequency dispersive ultrasound pretreatment (FSDUP), were conducted at 60 °C for 5 and 15 min, respectively. Results showed that the total phenols, flavonoids, anthocyanins, ascorbic acid, and DPPH free radical scavenging ability of SCJ decreased during the storage period. The control sample of SCJ was able to sage for only 7 days at 4 °C based on the microbiological quality, while the FSDUP and DEUP group extended the storage period up to 21 and 14 days, respectively. The polyphenol oxidase in SCJ pretreated by MTS did not reactivate during the storage period. The MTS remarkably (p < 0.05) reduced the color deterioration, browning degree, and nutrient degradation during the storage period. Moreover, the FSDUP group exhibited the maximum shelf life with a minimum loss of quality, demonstrating that it was the most suitable processing method for obtaining high-quality SCJ. It can be concluded that the MTS has the potential to inhibit enzymatic browning, inactivating microorganisms, preserve original quality attributes, and prolong the shelf life of SCJ.

Multi-frequency power ultrasound as a novel approach improves intermediate-wave infrared drying process and quality attributes of pineapple slices.

This study evaluated the effect of mono-frequency ultrasound (MFU, 20 kHz), dual-frequency ultrasound (DFU, 20/40 kHz), and tri-frequency ultrasound (TFU, 20/40/60 kHz) on mass transfer, drying kinetics, and quality properties of infrared-dried pineapple slices. Pretreatments were conducted in distilled water (US), 35 °Brix sucrose solution (US-OD), and 75% (v/v) ethanol solution (US-ET). Results indicated that ultrasound pretreatments modified the microstructure of slices and shortened drying times. Compared to the control group, ultrasound application reduced drying time by 19.01-28.8% for US, 15.33-24.41% for US-OD, and 38.88-42.76% for US-ET. Tri-frequency ultrasound provoked the largest reductions, which exhibited time reductions of 6.36-11.20% and better product quality compared to MFU. Pretreatments increased color changes and loss of bioactive compounds compared to the control but improved the flavor profile and enzyme inactivation. Among pretreated sample groups, US-OD slices had lower browning and rehydration abilities, higher hardness values, and better retention of nutrients and bioactive compounds. Therefore, the combination of TFU and osmotic dehydration could simultaneously improve ultrasound efficacy, reduce drying time, and produce quality products.

Selection of drying techniques for Pingyin rose on the basis of physicochemical properties and volatile compounds retention.

Awareness of edible rose being beneficial for health has attracted researchers in exploring different rose products. The study aimed to investigate effects of vacuum freeze drying (VFD), hot air drying (HAD), heat pump drying (HPD), relative humidity drying (RHD) and catalytic infrared drying (CID) on the physicochemical properties, and volatile organic compounds (VOCs) of Pingyin roses. Results showed that the VFD roses had significantly (p < 0.05) bright color, complete tissue cells, low shrinkage, and good plasma membrane permeability. CID roses showed the highest total phenols content (164.09 ± 0.88 mg/g) and the strongest antioxidant activity. Besides, the odor is the most crucial indicator for dried roses. VFD can well prevent the odor from diminishing/destroying and preserve the natural smell of rose. Thermal drying including HAD, HPD, RHD, and CID, could cause significant losses of VOCs. Consequently, the findings can provide the scientific basis for future large-scale production of dried rose products.

The temperature induced disruption process of amylopectin under ultrasonic treatments.

In this study, amylopectin was ultrasonicated at different temperatures to explore its disruption process. Results showed a significant decrease in amylopectin Mw after ultrasonic treatments and a retarded effect was detected with the increase of temperatures. The amylopectin disruption process fitted to the second order kinetic model (1/Mwt - 1/Mw0 = kt) and its disruption rate coefficient decreased from 2.203 × 10-8 to 0.986 × 10-8 mol/g min as the temperatures increased from 20 to 80 °C. This was ascribed to the higher vapour pressure and the lower viscosity of the solution at higher temperatures. Ultrasound induced break points preferentially occurred to B3 chains of amylopectin at higher temperatures which contributed to an increase of A chains, which because that amylopectin would be more extended at higher temperatures. The activation energy of amylopectin disruption was negative (-11.6 KJ/mol), which indicated that its scission process by ultrasound was essentially a mechanical action.

Recent development in high quality drying of fruits and vegetables assisted by ultrasound: A review.

The preservation of agri-products with a high moisture content like fruits and vegetables is challenging. Traditional dehydration techniques (sun drying and hot air drying) were used to limit food degradations and extend shelf life. However, few issues have been raised regarding the long processing time during the dehydration process causing the pronounced oxidation of nutrients and significant energy losses. Recent studies emphasize different process intensification methods, such as ultrasound (US), to rapidly and economically obtain quality dehydrated food to tackle quality deteriorating issues. The current work provides a comprehensive state-of-art of the drying of fruits and vegetables using ultrasound as an improvement technique for quality retention. The review will first provide a global knowledge of ultrasound in the drying field with a special focus on the equipment as well as mechanisms involved when US is used as a pretreatment or simultaneously during various drying processes. Discussion on the efficiency of each ultrasonic device and its potential use in industry is also provided along the way. The second part will cover a critical report and analysis of recent studies highlighting the effects of the two ultrasound application modes in the drying field (pretreatment and combined with the drying process) on the quality of fruits and vegetables. Overall, applying ultrasound to assist the dehydration of fruits and vegetables is a promising way to reduce drying time and obtain nutritious dehydrated products. This non-thermal technology alleviates the oxidation of nutrients, thus offering a favorable perspective to increase the marketability of finished products as public awareness of food quality is surging.

Effects of flat sweep frequency and pulsed ultrasound on the activity, conformation and microstructure of mushroom polyphenol oxidase.

The effects of thermal processing (TP) and flat sweep frequency and pulsed ultrasound (FSFPU) treatment with different frequency modes on the activity, conformation and physicochemical properties of mushroom polyphenol oxidase (PPO) were investigated. The results showed that the relative enzymatic activity of PPO gradually decreased with increasing temperature and duration, and thermosonication decreased the PPO activity to a greater extent compared with thermal processing. FSFPU treatment with dual-frequency of 22/40 kHz mode showed the most significant effect. Circular dichroism (CD) showed that the content of α-helix and ß-turn dropped, while that of ß-sheet and random coil raised after FSFPU treatment. The intensity of endogenous fluorescence decreased, indicating that PPO protein unfolded and the tertiary structure was destroyed. The amount of free sulfhydryl, protein aggregation index, and turbidity all rose. Moreover, FSFPU treatment led to the aggregation of protein from the analysis of atomic force microscope (AFM). Conclusively, FSFPU can be used as an effective method to inhibit the activity of endogenous enzymes in food.

One-step preparation of hydrogel based on different molecular weights of chitosan with citric acid.

BACKGROUND: Chitosan-based hydrogels have been prepared previously by a two-step protocol in which chitosan was first dissolved in dilute acetic acid and then crosslinked by glutaraldehyde or genipin. This was a time-consuming method, which had the disadvantages of high costs and biological safety problems. RESULTS: Scanning electron microscopy (SEM) results verified the successful preparation of hydrogels based on high, medium, and low molecular-weight chitosan (HCS, MCS, and LCS), respectively. The hydrogels prepared with HCS, MCS, and LCS were formed through the accumulation of different-sized crystals. The framework density of the hydrogel was enhanced by an increase in the chitosan molecular weight and exhibited a crack pore pattern composed of flake particles. Medium molecular-weight chitosan-based hydrogel exhibited the highest specific surface area and total pore volume, with values of 3.81 m2 g-1 and 0.0109 cm3 g-1 , respectively. The water absorption rate of the chitosan based hydrogels was influenced by its molecular weights at the sequence of LCS > HCS > MCS, while the maximum compression stress was affected at the sequence of HCS > MCS > LCS. The network structure was enhanced with an increase in the chitosan molecular weight and reached maximum stress levels of 4.50, 1.50 and 0.75 MPa for HCS-, MCS-, and LCS-based hydrogels, respectively. CONCLUSION: Citric acid was shown to be an effective dissolving and crosslinking agent in the preparation of MCS- and HCS-based hydrogels. The physiochemical properties of the hydrogels were enhanced as the molecular weight of the chitosan increased. © 2021 Society of Chemical Industry.

Effect of multi-mode dual-frequency ultrasound pretreatment on the vacuum freeze-drying process and quality attributes of the strawberry slices.

The effects of osmotic pretreatment assisted by ultrasound in different frequency modes before vacuum freeze-drying (VFD) on moisture migration and quality characteristics of strawberry slices were investigated. The frequency modes are single-frequency modes under 20, 40 kHz (SM-20, SM-40), and dual-frequency under 20/40 kHz including sequential mode (SeDM) and simultaneous mode (SiDM). The quality characteristics of dried strawberry products including rehydration, hardness, color, flavor, total anthocyanins, total phenols, vitamin C content, and active antioxidant components (DPPH and -OH) were determined. Results showed that drying time of the strawberry slices irradiated by ultrasound was reduced by 15.25%-50.00%, compared to the control samples. Besides, dual-frequency ultrasound shortened the drying time more than single-frequency ultrasound. The drying time of SeDM was the shortest. In addition to vitamin C content, the quality characteristics including rehydration, hardness, color, flavor, total anthocyanins, total phenols, and antioxidant activity of dried strawberry products pretreated by SeDM were significantly (p < 0.05) better than those of control and other pretreated samples. It can be concluded that the SeDM was an effective pretreatment method to produce high-quality vacuum freeze-dried strawberry products.

Effect of multi-frequency power ultrasound (MFPU) treatment on enzyme hydrolysis of casein.

Effect of multi-frequency power ultrasound (MFPU) pretreatments on the degree of hydrolysis (DH) and mechanism of casein during alcalase enzymolysis was investigated. Results showed that MFPU pretreatment in tri-frequency 20/40/60 kHz mode significantly (p < 0.05) improved the DH value of casein. Variation of intrinsic fluorescence spectrum indicated the unfolding and degradation of casein occurred after MFPU pretreatment. Fourier transform infrared spectra showed that α-helix and ß-sheet content of MFPU pretreated casein decreased, while ß-turn and random coil content increased. Surface topography and nanostructures of caseins were found modified after MFPU pretreatments by the analysis of scanning electron microscopy (SEM) and atomic force microscopy (AFM). The SEM analysis also indicated that the enzymolysis residues of casein pretreated by MFPU were smaller than untreated samples. In conclusion, the MFPU can be used as an efficient pretreatment method to promote the enzymolysis of casein.

The ex-situ and in-situ ultrasonic assisted oxidation of corn starch: A comparative study.

The objective of this study was to evaluate the differences in ex-situ (starch treated by ultrasonication and oxidation sequentially, U-OS) and in-situ (starch treated by ultrasonication and oxidation simultaneously, UOS) ultrasonic assisted oxidation process of corn starch, which were studied in contrast to the traditional oxidized starches (OS). Fourier-transform infrared spectra confirmed the successful oxidation of all modified starches samples. In comparison to the OS, the carboxyl contents of U-OS and UOS increased by 56% and 112%, respectively. The same increase trend was also found for the carbonyl contents. The significance raise was attributed to the great increase of pores and specific surface areas in the starch granule after ultrasonic irradiation which promoted the penetration of the sodium hypochlorite into the starch granules with higher chances for chemical reactions. SEM and pore size distribution characterizations further verified this result. However, the method of in-situ ultrasonic assisted oxidation can simultaneously accelerate the increase of pores and the penetration process. Consequently, the starches with higher oxidation degree can be more efficiently prepared by the strategy of in-situ ultrasonic assisted oxidation.

Structural changes of chemically modified rice starch by one-step reactive extrusion.

Structural changes of chemically modified rice starch (CMRS) by one-step reactive extrusion (REX) via esterification, acetylation, hydroxypropylation, and cross-linking or dual-modification (hydroxypropylation-cross-linking and acetylation-cross-linking) were investigated. REX treatments exhibited a significant effect on the structure of rice starch granules, resulting in the destruction of the starch crystalline structure and formation of new crystalline complexes. The original A-type crystalline structure was transformed to VH-type after REX treatments, which were further confirmed by DSC experiments since a new endotherm at 100-122 °C was detected. Due to the susceptibility differences in shear-induced breakdown of amylopectin and amylose, the molecular degradation was heterogeneous and retarded by esterification but enhanced by cross-linking. Morphology analysis showed that the original starch granular structure was lost and replaced with a rougher and more irregular structure. In consequence, REX process exerted significant influences on rice starch granules which enhanced its resistance to enzyme hydrolysis.

Disruption and molecule degradation of waxy maize starch granules during high pressure homogenization process.

The mechanism underlying the fragmentation of waxy maize starch (WMS) granules during high-pressure homogenization (HPH) was studied and the results were interpreted in terms of granular and molecular aspects. The diameter of disrupted starch granules decreased exponentially with increasing HPH pressure, but decreased linearly with increasing of HPH cycles. Scanning electron microscopy revealed a cone-like inside-out disruption pattern through the channels that resulted in separation of blocklets fragments or starch fragments. The Mw of amylopectin was reduced by ∼half following treatment at 150MPa with two cycles, or at 100MPa for eight cycles, and the decrease was in accordance with the disruption of starch granules. This indicated that amylopectin was "protected" by blocklets, and the disruption of WMS granules mainly occurred close to the linkage among blocklets. Increasing the HPH pressure appeared to be more effective for breaking starch granules than increasing the number of HPH cycles.

Low frequency ultrasound pretreatment of carrot slices: Effect on the moisture migration and quality attributes by intermediate-wave infrared radiation drying.

The effect of low frequency ultrasound (LFU) pretreatment prior to intermediate-wave infrared radiation (IW-IR) drying on water migration and quality attributes of carrot slices was investigated in this study. Results showed that the vacuole water of LFU pretreated carrot samples decreased, while the cytoplasm and intercellular space water increased by low-field nuclear magnetic resonance analysis. In addition, LFU pretreatment caused the disruption of cell structures and formation of micro-channels, resulting in significant (p<0.05) decrease of drying time required. The IW-IR dried carrot slices with LFU pretreatment showed higher ß-carotene content and rehydration ratio in comparison with control samples. The color parameters of ultrasound pretreated dried carrot slices after dehydration were closer to the raw carrot samples. The results of electronic nose showed that the aromatic and volatile organic compounds of dried carrot increased by sonicated pretreatment, while the nitrogen oxides decreased, indicating that LFU can improve the flavor of dried carrot slices.

Effect of reaction solvents on the multi-scale structure of potato starch during acid treatment.

Potato starch was treated with 0.36% HCl in ethanol and water for various time periods, and its structural changes were evaluated and compared in this study. Acid-ethanol treated starch (AET-s) had relatively low average molecular weight (Mw) and z-average radius of gyration (Rg), and its solubility was higher than that of the counterpart acid-water treated starch (AWT-s). The granular appearance and differential scanning calorimetry (DSC) profile demonstrated that acid in ethanol and in water exhibited different attack pathways on the granules. No significant difference in crystallinity was observed for AET-s; however, the ratio of absorbance 1022/995cm-1 and the peak intensity detected by small-angle X-ray scattering (SAXS) were increased with increasing treatment time. These results suggested that ethanol-acid treatment simultaneously attacked on the amorphous and crystalline regions, and the degradation extent on crystalline regions caused by ethanol-acid treatment was higher than that observed by acid-water treatment.

Synthesis, characterization and hydrophobicity of silylated starch nanocrystal.

Starch nanocrystal (SNC) was silylated by hexadecyltrimethoxysilane (HDS) aiming to improve its hydrophobicity. HDS was firstly hydrolyzed in ethanol/water and then adsorbed onto SNC through hydrogen bonds, finally the long chain hydrocarbon was covalently linked to the surface of SNC through SiOC bonds which formed via the condensation reaction between hydroxyl and silanol groups. Due to the multilayer coverage of the hydrolyzed HDS, the long chain hydrocarbon crystalized on the surface of SNC and superimposed over the original A-type starch diffraction pattern. Both the hydrophobicity and hydrophobic stability were increased with the increase of the applied HDS. The contact angle of modified SNC increased from 43° to 119° as the applied HDS increased from 0% to 0.3% (v/v). The modification significantly improved its dispersibility in non-polar solvents and a homogenous suspension could be formed in acetone and n-hexane.

Thermal degradation behavior of hypochlorite-oxidized starch nanocrystals under different oxidized levels.

The thermal degradation behavior of hypochlorite-oxidized starch nanocrystals (OSNCs) was evaluated in this study. Carbonyl and carboxyl groups in OSNCs increased from 0.006 and 0.091mmol/g to 0.033 and 0.129mmol/g, respectively, as the active chlorine concentration increased from 1% to 4% (w/w). Compared with starch nanocrystals (SNCs), the initial degradation temperature of OSNCs with 4% oxidization decreased from 273°C to 253°C. Two degradation processes were detected using differential thermal analysis. The activation energy of the low-temperature process increased with increasing oxidization level because of removal of sulfate esters and reduction of the decomposition products of H2O during oxidation. With increasing temperature, the H2O generating from decarboxylation and decomposition of the carboxyl groups may catalyze SNCs depolymerization, leading to decrease in the activation energy of the high-temperature process. OSNCs (4% oxidized level) can be used in dry process below 253°C to avoid degradation.

Preparation and characterization of carboxymethyl starch microgel with different crosslinking densities.

Microgels synthesized with different crosslinking densities were characterized by Fourier transform infrared (FT-IR) spectroscopy, thermogravimetry analysis (TGA), swelling, and rheological analyses. The lysozyme uptake capacity of these microgels was evaluated through the effects of lysozyme concentration, pH, and ionic strength. The microgel particle size mostly ranged within 25µm to 45µm. FT-IR analysis results suggested that sodium trimetaphosphate reacted with the hydroxyl groups of carboxymethyl starch (CMS), thereby forming ester linkages. TGA data indicated that crosslinking increased the thermal stability of CMS. Swelling degree increased with increasing pH before pH 5, and then remained almost constant. However, swelling degree decreased with increasing ionic strength and crosslinking density. The microgels behaved as viscoelastic solids because the storage modulus was higher than the loss modulus over the entire frequency range of dispersions with polymer concentrations of 3% (W/W) at 25°C. The data for the uptake of lysozyme by microgels demonstrated that the protein uptake increased with increasing pH and lysozyme concentration, as well as with decreasing ionic strength and crosslinking density. The lysozyme-microgels complex was identified by CLSM, and the distribution of lysozyme in microgels with low crosslinking density was rather homogeneous.