Crystalline Type Research Articles

Significant fluorescence from pulsed laser ablated silver-copper nanocomposites

Diverse biocompatible nanomaterials with improved physiochemical characteristics became demanding for biomedicines. Thus, new types of crystalline and spherical silver-copper nanocomposites (AgCuNCs) with prominent fluorescence (FL) and localized surface plasmon resonance (LSPR) absorption were made using pulse laser ablation in liquid (PLAL) method. The structure, morphology, and FL properties of these NCs were customized via the laser fluence (LF) adjustments. Nanocomposite made at LF of 14.15 ± 0.4 J cm−2 displayed uniform particle size distribution (mean diameter of 7.22 ± 1.31 nm) with a high FL quantum yield of 0.061. Exciton-like energy states and size-enabled electronic transitions shown by these proposed plasmonic NCs were asserted to be beneficial for biomedical applications especially in improved FL-based drug formulation.

Spectroscopic characterization, DFT modeling and antimicrobial studies of some novel nanoparticles mixed ligand complexes of NS bidentate ligand in presence of 2,2′-bipyridine

Cr(III), Fe(III), Co(II), Ni(II), Cu(II), and Zn(II) interacted with 1-[4-(4-methoxyphenyl)-6-methyl-2-thioxo-1,2,3,4-tetrahydropyrimidin-5-yl]ethanone (L) to form six mixed ligand metal complexes in existence of 2,2′-bipyridine (Bipy).The produced compounds were described utilizing elemental analyses, FT-IR, UV–vis., 1H NMR spectra, thermal analyses (TG-DTG and DTA), X-ray powder diffraction method (XRD), molar conductance and magnetic moment. The IR showed that L bonded with metal ions as bidentate ligand through nitrogen and sulfur atoms, while, Bipy coordinated across nitrogen atoms. According to the molar conductance measurements the complexes are electrolytes. For all complexes the octahedral geometry were supported by employing the magnetic moments and electronic spectra. The degradation pathways for L, Bipy and their complexes utilizing TG and DTG were determined and thermodynamic parameter (Ea, ΔH*, ΔS* and ΔG*) were computed utilizing Horowitz-Metzger (HM) and Coats-Redfern (CR). The average crystalline size (D) and type of each molecule were evaluated using the XRD analysis (crystalline or amorphous). In order to recognize the optimal molecular geometry for the compounds, density functional theory (DFT) simulations were performed. Regarding L, which has σ value of 17.544 eV, all investigated complexes with σ values ranging from 21.053 to 95.238 eV are regarded as soft. Numerous bacterial and fungal strains were used as test subjects for the compound's biological activities. The data show that the current complexes are highly effective and could serve as superior bactericides.

Study on the effect of different concentrations of choline glycine ionic liquid-water mixtures on debranched starch butyrylation reaction

In this study, the effect of choline glycine ionic liquids on the butyrylation of starch was investigated by the butyrylation of debranched cornstarch in different concentrations of choline glycine ionic liquid-water mixtures (choline glycine ionic liquids to water in mass ratios of 0:10, 4:6, 5:5, 6:4, 7:3, 8:2 and 10:0). The butyryl characteristic peaks in 1H NMR and FTIR of the butyrylated samples indicated the success of butyrylation modification. 1H NMR calculations showed that the most effective mass ratio of choline glycine ionic liquids to water (6:4) increased the butyryl substitution degree from 0.13 to 0.42. X-ray diffraction results showed that the crystalline type of the starch modified in the choline glycine ionic liquid-water mixtures changed from B-type to a mixture of V-type and B-type isomers. The butyrylated starch modified in the ionic liquid increased its own content of resistant starch from 25.42 % to 46.09 %. This study highlights the effect of different concentrations of choline glycine ionic liquid-water mixtures on the promotion of starch butyrylation reactions.

Engineering β-ketoamine covalent organic frameworks for photocatalytic overall water splitting

Covalent organic frameworks (COFs) are an emerging type of crystalline and porous photocatalysts for hydrogen evolution, however, the overall water splitting activity of COFs is rarely known. In this work, we firstly realized overall water splitting activity of β-ketoamine COFs by systematically engineering N-sites, architecture, and morphology. By in situ incorporating sub-nanometer platinum (Pt) nanoparticles co-catalyst into the pores of COFs nanosheets, both Pt@TpBpy-NS and Pt@TpBpy-2-NS show visible-light-driven overall water splitting activity, with the optimal H2 and O2 evolution activities of 9.9 and 4.8 μmol in 5 h for Pt@TpBpy-NS, respectively, and a maximum solar-to-hydrogen efficiency of 0.23%. The crucial factors affecting the activity including N-sites position, nano morphology, and co-catalyst distribution were systematically explored. Further mechanism investigation reveals the tiny diversity of N sites in COFs that induces great differences in electron transfer as well as reaction potential barriers.

Hydrogeological Characterization of Crystalline Bedrock Using Borehole Magnetic Resonance.

We aimed to test borehole magnetic resonance (BMR) method for determining hydraulic parameters (porosity, permeability, and hydraulic conductivity) required for hydrogeological modeling in two distinct crystalline rock environments. These sites comprise Proterozoic basement rocks of different compositions: mafic rocks at the Sakatti mining development site in northern Finland and felsic rocks at the Olkiluoto Island nuclear repository site in southwest Finland. Although BMR is widely used for determining storage and hydraulic properties in sedimentary environments, there have been few studies in crystalline bedrocks. The results indicate that BMR is a suitable tool for studying lithologically and hydrogeologically heterogeneous fractured crystalline bedrocks. It can produce continuous data from hydraulic properties of bedrock in addition to more time-consuming methods such as flowmeter and packer tests and can provide guidance on where to focus additional flow measurements. The intervals display fracture and reduced matrix porosity characteristics, both of which can be enhanced or reduced locally by chemical alteration and by tectonic processes. Flow parameters vary significantly throughout the studied intervals: independently from the lithological composition, these intervals locally display relatively high porosities, and may be correlated to the more intensely fractured and/or brecciated zones. However, due to the heterogeneity in mineralogy, grain/pore arrangement, and the variability of fracture flow-driven transport in each borehole, the challenge remains in finding a unique set of permeability constants for these crystalline rock types. The permeability models could be calibrated by laboratory measurements of the core, and possibly a new permeability model suitable for crystalline bedrock could be created.

Starch Chemical Composition and Molecular Structure in Relation to Physicochemical Characteristics and Resistant Starch Content of Four Thai Commercial Rice Cultivars Differing in Pasting Properties.

Variations in starch pasting properties, considered an alternative potential quality classification parameter for rice starches, are directly controlled by the diverse starch molecular composition and structural features. Here, the starch characteristics of four rice cultivars (i.e., RD57, RD29, KDML105, and RD6) differing in pasting properties were assessed, and their relationship was determined. The results revealed that protein and moisture contents and their crystalline type were similar among the four rice starches. However, their molecular compositions and structures (i.e., reducing sugar and amylose contents, amylopectin branch chain-length distributions, granule size and size distribution, and degree of crystallinity) significantly varied among different genotypes, which resulted in distinct swelling, solubility, gelatinization, retrogradation, and hydrolytic resistance properties. The swelling power and gelatinization enthalpy (∆H) were positively correlated with C-type granule and relative crystallinity, but were negatively correlated with amylose content, B-type granule and median particle size (d(0.5)). Conversely, the water solubility and resistant starch content negatively correlated with C-type granule, but positively correlated with amylose content, B-type granule, and d(0.5). The gelatinization onset temperature (To(g)), and retrogradation concluding temperatures (Tc(r)), enthalpy (∆H(r)), and percentage (R%) were positively impacted by the amount of protein, amylose, and B1 chains (DP 13-24), while they were negatively correlated with short A chains (DP 6-12). Collectively, the starch physicochemical and functional properties of these Thai rice starches are attributed to an interplay between compositional and structural features. These results provide decisive and crucial information on rice cultivars' suitability for consumption as cooked rice and for specific industrial applications.

Synthesis, structure, luminescence and photocatalytic properties of CaTiO(SiO4):Eu3+

Titanite CaTiO(SiO4):Eu3+ were synthesized by a solvothermal-calcination method and an improved high-temperature solid-state synthesis method. Their structure, luminescence properties and photocatalytic propoties were comparatively studied in detail. It was found that CaTiO(SiO4):Eu3+ synthesized by the two methods belong to two different types of crystalline and each of them has its own advantages and disadvantages. Titanite synthesized by solvothermal-calcination method has rough and porous surface morphology, larger BET, and smaller crystallite size, which result in a weaker luminescence intensity than the one synthesized by high-temperature solid-state method. But in the experiment of photocatalysis, all these disadvantages are turned into advantages. In addition, the high temperature process also increases the symmetry of Eu3+ occupation and leads to many surface traps, which result in a less red color and a shorter fluorescence life than solvothermal synthesized titanite. We hope that this comparative study will extend the applications and research ideas of titanite.

Preparation of Cellulose Nanocrystals: Controlling the Crystalline Type by One-Pot Acid Hydrolysis.

Cellulose nanocrystals (CNCs) have aroused increasing interest owing to their renewable origin and excellent properties derived from their size and morphology. Based on their chain orientation, CNCs can be prepared as two main allomorphs (I or II). However, achieving pure CNC allomorphs still requires enhanced control on the CNCs synthesis process and improved understanding of the involved reaction parameters. In this work, we study in detail a set of parameters for CNC synthesis using one-pot acid hydrolysis and evaluate their influence on the outcome with respect to yield, purity, and repeatability. We also demonstrate that a fast, nondestructive, and accurate methodology based on dynamic light scattering is an efficient alternative to the usual structural analysis of the synthesis outcome. Finally, we provide an improved protocol to reliably obtain each allomorph with mass yields of 25% for type I and 40% for type II. Emphasis is put on the reduction of the environmental impact and the overall preparation time.

Effects of octenyl succinylation on the properties of starches with distinct crystalline types and their Pickering emulsions

Effects of octenylsuccinic anhydride (OSA) esterification on the morphology, crystalline structure, and emulsifying properties of three representative starches with different crystalline types, namely waxy corn starch (A-type), potato starch (B-type), and pea starch (C-type) were investigated. XRD patterns testified OSA substitution occurred principally in the amorphous region without affecting the crystalline patterns, whereas SEM verified esterification was mainly a surface phenomenon. However, OSA esterification caused a decrease in the peak intensity and area of small-angle X-ray scattering profiles, indicating the semi-crystalline lamellae ordering was impeded to a certain extent. Compared with A- and C-type starches, B-type starch had a stronger affinity for OSA, as manifested by its higher degree of substitution (DS), graver surface detriment, and depressed order of semi-crystalline lamellae. The emulsifying properties of all starches were pronouncedly improved by OSA modification, especially for A-type starch even with comparatively lower DS. Pickering emulsion stabilized by OSA-modified A-type starch (A-OSAS) with smaller droplet size and more uniform droplet size distribution exhibited more splendiferous stability relative to the other two modified starches. Moreover, rheological tests revealed A-OSAS possessed the highest apparent viscosity and storage modulus (G′), insinuating strong intermolecular interactions between starch granules at the interface and/or in the continuous phase.

Consolidating the gelling performance of myofibrillar protein using a novel OSA-modified-starch-stabilized Pickering emulsion filler: Effect of starches with distinct crystalline types

Starch-stabilized Pickering emulsions were employed as a novel particulate filler in myofibrillar protein (MP)-based gels for improving the gelling characteristics. The role of emulsions prepared by native starches (NS) with distinctive crystalline types (i.e., A-type waxy corn starch, B-type potato starch, and C-type pea starch) and their OSA-modified counterparts (A-OS, B-OS, C-OS) in the gelling performance was evaluated and compared with MP-stabilized-emulsion. Compared with MP-emulsion, starch-emulsion caused substantial increases in the gelling properties, notably for OSA-starch emulsions. Herein, A-OS exhibited up to 1.26-, 5.3-, and 2.9-fold increments in storage modulus, gel strength, and water holding capacity relative to pure MP gel, respectively, higher than B-OS and C-OS. Moreover, light microscopy evinced a more compact gel network filled with smaller and uniform oil droplets when A-OS emulsions were incorporated into the gels. The addition of OSA-starch emulsions, especially A-OS emulsion, facilitated the protein conformational conversion from α-helix to β-sheet and caused a marked reduction of free sulfhydryls in the gels; yet, the chemical forces that stabilized the gels altered, where remarkable reinforcements in hydrogen bond and hydrophobic interaction were detected, in support of the construction of splendid MP gels. Hence, OSA-starch emulsions show promise as functional components in meat products.

Root cause for the difference in photovoltaic parameters of perovskite solar cells prepared by one- and two-step processes

Benefiting from good solubility of metal halide perovskites, low-temperature solution processes (including one- and two-step spin-coating) have become the most common approach for perovskite solar cells (PSCs). However, one confusing issue is that what are specifically effective strategies for the one-step process may not be applicable for the two-step process, and vice versa. Herein, the PSCs with the same perovskite composition and device configuration were prepared by one- and two-step processes, respectively. The results indicated that high performance PSCs with comparable power conversion efficiency over 22% were achieved by both methods, while the detailed photovoltaic parameters varied greatly depending on the one- or two-step process. Compared to the one-step counterpart, the two-step processed PSCs exhibit lower open-circuit voltage and fill factor, but superior short-circuit current, which was in-depth interpreted in terms of the crystalline growth mode, optical properties, defect types, and carrier transport mechanisms related to a perovskite film surface (including a top and a bottom surface). Understanding the root cause for such differences would be central toward identifying what is really crucial for further producing high performance PSCs.

Light-driven biodegradation of azo dyes by Shewanella decolorationis-CdS biohybrid in wastewater lacking electron donors.

The lack of electron donors prevents the effective degradation of azo dyes by bacteria, which severely limits the practical application of conventional biological treatment. Herein, we innovatively designed a bio-photoelectric reduction degradation system composed of CdS and Shewanella decolorationis, which could effectively degrade amaranth in anaerobic conditions driven by light when electron donors were unavailable. Compared with bare S. decolorationis and S. decolorationis (heat-killed)-CdS biohybrid, S. decolorationis-CdS biohybrid had 39.36-fold and 3.82-fold higher first-order kinetic constants, respectively. The morphology, particle size, elemental composition, crystalline type, photovoltaic properties, and band structure of the nanoparticles synthesized by S. decolorationis were carefully examined and analyzed. Light-driven biodegradation experiments showed that amaranth was degraded by the synergy of CdS and S. decolorationis. Reductive degradation of amaranth by electrons was demonstrated by electron and hole trapping. The effect of potential coexisting contaminants, which might serve as hole scavengers, on the degradation of amaranth was evaluated. Membrane protein inhibition experiments also suggested that NADH dehydrogenase, menaquinone, and cytochrome P450 played an important role in electron transfer between CdS and Shewanella decolorationis. The cyclic conversion of NAD+/NADH was probably the most critical rate-limiting step. Electrochemical measurements suggested that faster electron transfer might facilitate the degradation of amaranth. Our findings might contribute to the degradation of azo dyes in wastewater lacking electron donors and deepen our recognition of the microbe-material interface. KEY POINTS: • A BPRDS was constructed with Shewanella decolorationis and CdS. • Amaranth was effectively degraded by BPRDS in anaerobic conditions driven by light. • NDH, MQ, and CYP450 were involved in electron transfer.

Indole acetylated high-amylose maize starch: Synthesis, characterization and application for amelioration of colitis

Tryptophan metabolites such as indole-3-acetic acid (IAA) are critical for gut health, through their binding to the aryl hydrocarbon receptor (AhR), and may be useful for treatment of gastrointestinal diseases. Delivery of IAA to the colon is necessary, and one strategy is use of esterified starches which get digested in the colon by gut microbes. High amylose maize starch (HAMS) resists digestion in the upper gastrointestinal tract and is fermented by gut microbiota to release short-chain fatty acids (SCFAs), which are also beneficial to intestinal homeostasis. IAA esterified to HAMS (HAMSIAA) was synthesized with different degrees of substitution (DSs) by controlling the ratio of IAA vs HAMS. Successful incorporation of indole acetyl group was verified by NMR and FTIR spectra. XRD revealed that the crystalline type of HAMSIAA changed from B to V-type. SEM showed the destroyed surface of the starch granules. HAMSIAA with DS ~ 0.3 effectively increased IAA in the colon, to levels unachievable by oral IAA delivery. HAMSIAA increased pathways downstream of AhR activation, including CYP1A1 mRNA expression and IL-22 protein levels, and greatly improved DSS-induced colitis. HAMSIAA could serve as an ideal means for colon-targeted delivery of IAA and a promising nutraceutical for amelioration of inflammatory conditions.

Metal-organic framework-induced edge-riched growth of layered Bi2Se3 towards ultrafast Na-ion storage

Inner design and effective regulation of interlayer are the key factors for optimizing the capacity deliver. Herein, this work carries out precise regulation on crystalline type and facets orientation by using ordered guidance of Bi-MOF to control the metal crystal growth, and preferably oriented-growth along (00l) facets in Bi2Se3 is realized, the influence of the dominant-exposed facets on Na-storage is investigated. Experimental investigations and first-principle calculations indicates that perfect oriented growth along (00l) facets of monocrystalline Bi2Se3, and open 2D interlayer structure provides a large amount of electrochemically active areas and kinetically favorable interlayers. The elaborate design structure can not only afford more channels for Na+, but also accelerate the Na+ insertion/extraction among the host material. Highly conductive network is constructed by C–O–Bi oxygen-bridge bond. The Bi2Se3–C/G-1 composites can exhibit a high reversible capacity of 377 mAh g−1 and extraordinary rate performance with an extremely low capacity fading of 12% with current increase from 0.2 to 10 A g−1. The developed two-dimensional oriented-arranged interlayer and highly exposed edges effectively accelerates the diffusion of Na+, reduces the phase-transformation resistance, improves the reaction activity. The stronger interfacial reaction between graphene and bismuth selenide also provides an enhanced pathway for electrons.

Study of Changes in Crystallinity and Functional Properties of Modified Sago Starch (Metroxylon sp.) Using Physical and Chemical Treatment.

Sago starch has weaknesses such as low thermal stability and high syneresis. Modifications were made to improve the characteristics of native sago starch. In this study, sago starch was modified by autoclave-heating treatment (AHT), osmotic-pressure treatment (OPT), octenyl-succinic anhydride modification (OSA), and citric acid cross-linking (CA). This study aimed to examine the changes in chemical composition, crystallinity, and functional properties of the native sago starch after physical and chemical modifications. The results show that physical modification caused greater granule damage than chemical modification. All modification treatments did not alter the type of crystallinity but decreased the relative crystallinity of native starch. New functional groups were formed in chemically modified starches at a wavelength of 1700-1725 cm-1. The degree of order (DO) and degree of double helix (DD) of the modified starches were also not significantly different from the native sample, except for AHT and OPT, respectively. Physical modification decreased the swelling volume, while chemical modification increased its value and is inversely proportional to solubility. AHT and OPT starches have the best freeze-thaw stability among others, indicating that both starches have the potential to be applied in frozen food.

Effect of Electrode Morphology on Performance of Ionic Actuators Based on Vat Photopolymerized Membranes.

Bucky gel electrodes are composed of morphology-determining polyvinylidene difluoride (PVDF) filled with carbon nanotubes (CNT). The electrodes are commonly fabricated via the casting of a CNT dispersion containing PVDF and ionic liquid. In this study, several pore-forming additives such as polyethylene glycol (PEG), dibutyl phthalate (DBP), and the common ionic liquid BMIMBF4 were used to control the morphology of the bucky gel electrodes. The crystalline phase type and content of PVDF in the electrodes were determined by FT-IR and DSC, respectively. SEM revealed a sponge-like structure in the case of the use of BMIMBF4 and a spherulite structure if PEG and DBP were used as additives. A strong influence of morphology on the anisotropic increase in the volume of electrodes upon impregnation with electrolyte was observed. The PEG-based electrode elongated more than the others, while the BMIMBF4-based electrode thickened to a greater extent. Ionic actuators were fabricated to experimentally reveal the effect of electrode morphology on their electromechanical efficiency. A high-precision vat photopolymerization technique was used to fabricate identical ionic membranes and minimize their influence on the properties of the actuators. The electrodes were characterized by the same porosity and electrical capacitance, while the actuators differ significantly in performance. As a result, a simple method of using pore-forming additives made it possible to increase the maximum deformation of bucky gel ionic actuators by 1.5 times by changing the morphology of the electrodes.

Effects of Different Extraction Methods on the Gelatinization and Retrogradation Properties of Highland Barley Starch.

The purpose of this study was to compare the gelatinization and retrogradation properties of highland barley starch (HBS) using different extraction methods. We obtained HBS by three methods, including alkali extraction (A-HBS), ultrasound extraction (U-HBS) and enzyme extraction (E-HBS). An investigation was carried out using a rapid viscosity analyzer (RVA), texture profile analysis (TPA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Fourier-transform infrared spectrometry (FTIR). It is shown that the different extraction methods did not change the crystalline type of HBS. E-HBS had the lowest damaged starch content and highest relative crystallinity value (p < 0.05). Meanwhile, A-HBS had the highest peak viscosity, indicating the best water absorption (p < 0.05). Moreover, E-HBS had not only higher G′ and G″ values, but also the highest gel hardness value, reflecting its strong gel structure (p < 0.05). These results confirmed that E-HBS provided better pasting stability and rheological properties, while U-HBS provides benefits of reducing starch retrogradation.

Effect of ultrasonic pre‐treatments on the octenyl succinic anhydride substitution of potato starch and its physicochemical and emulsifying properties

SummaryTo investigate whether the ultrasonic pre‐treatments of starch will affect the octenyl succinic anhydride (OSA) esterification, different power ultrasonic pre‐treatments (150, 300, 450 and 600 W) were performed on potato starch, then the OSA esterification was performed and the physicochemical as well as the emulsifying properties of the OSA starch were analysed. Results indicated that ultrasonic pre‐treatments decreased the degree of substitution and reaction efficiency by 30%, regardless of the pre‐treatments condition, while little differences were observed in the crystalline type and the long‐range ordered structure. DSC results demonstrated that low‐power ultrasound decreased the values of To and Tp, but increased ΔH, while high‐power ultrasound had the opposite effect. In addition, high‐power sonication improved the emulsifying capacity of OSA starch, which ranged from 189.08 ± 0.23 m2/g to 334.70 ± 0.35 m2/g, while emulsion stability decreased from 277.02 ± 10.83 min to 42.75 ± 0.08 min. Overall, the result of the present work implied that OSA starch exhibited varied thermal and emulsifying properties under different ultrasonic pre‐treatments, and our work might provide basic theory for the preparation of OSA starch.

Understanding how electron beam irradiation doses and frequencies modify the multiscale structure, physicochemical properties, and in vitro digestibility of potato starch

To optimize the properties of native potato starch and to broaden its application in the food field, it was treated by electron beam irradiation (EBI) with different irradiation doses (6, 12, and 24 kGy) and frequencies (1, 2, 4, and 8 times), and the effects on the multi-scale structure, physicochemical properties, and in vitro digestibility were investigated. The results indicate that the increased dose aggravates starch degradation, generating more short chains and fragments, and reducing molecular weight, viscosity, and swelling power. Also, the higher dose facilitated the relative crystallinity, enhancing the ΔH and improving the RS content of potato starch. Furthermore, the repeated irradiation exhibited a cumulative dose effect: the short-range order, molecular weight, solubility, and swelling power improved after multiple irradiations. In addition, irradiation doses and frequencies neither destroyed starch's surface nor changed the polarized cross and growth ring. Also, all irradiated starch preserved starch's FT-IR spectrum and crystalline type. Moreover, multiple low-dose irradiations can not only improve the starch properties, but also achieve energy-saving purposes. Thus, as a rapid, green, non-thermal modification technology, EBI can impart low molecular weight, low viscosity and high solubility processing properties to starch, and improve its RS content without destroying the starch granular appearance.

Effect of enzymatic hydrolysis on digestibility and morpho-structural properties of hydrothermally pre-treated red rice starch

The objective of this work was to evaluate the effects of enzymatic hydrolysis on digestibility and morphological and structural properties of hydrothermally pre-treated (HPT) red rice starch. The pre-treatments were performed in autoclave and cooking for the modification of rice grains and native starch. In vitro starch digestibility was performed consecutively and semi-simultaneously using α-amylase and amyloglucosidase. A first-order mathematical model was used to adjust the hydrolysis kinetic data, which made it possible to calculate the surface area, hydrolysis index, and glycemic index of the starch. Scanning electron microscopy images (SEM), Fourier transform infrared (FTIR) spectra and X-ray diffraction (XRD) were also performed to investigate the characteristics of the post-hydrolysis starch samples. The autoclaved starch HSS-A3, which was subjected to 121 °C/1.08 bar for 10 min, showed the highest in vitro digestibility values (80.08 %). Both starch samples showed increase of particle size and enzymatic digestibility after HPT. FTIR spectra of the starch samples showed that there was no appearance of new functional groups. However, XRD evidenced that HPT changed the intensity of the peaks and the type of crystallinity was changed for autoclaved starch (A3) from type A to Vh, with crystallinity ranging from 21.71 % to 26.42 %. The semi-simultaneous approach showed more advantages due to the highest in vitro digestibility as well as reducing the processing time and use of reagents.