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![Methods for measuring the biodegradability of starch [13].](profile/Marita-Piglowska/publication/339080424/figure/fig1/AS:855671645958145@1581019426288/Methods-for-measuring-the-biodegradability-of-starch-13.jpg)
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![Figure 1. Methods for measuring the biodegradability of starch [13].](profile/Marita-Piglowska/publication/339080424/figure/fig1/AS:855671645958145@1581019426288/Methods-for-measuring-the-biodegradability-of-starch-13_Q320.jpg)
![Figure 3. Possible pathways during starch degradation [17].](profile/Marita-Piglowska/publication/339080424/figure/fig2/AS:855671645933568@1581019426334/Possible-pathways-during-starch-degradation-17_Q320.jpg)
The main aim of this study is to estimate the kinetic and thermodynamic parameters of thermal decomposition of starches by the Coats-Redfern method. This procedure is a commonly used thermogravimetric analysis/difference thermal gravimetry/differental thermal analysis (TG/DTG-DTA) kinetic method for single rate form. The study also shows a proposed...
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Context 1
... to the work of [12], at about 180 °C, the diffraction patterns are less sharp, and at 210-220 °C, the amorphous region is produced and the birefringence of molecules is destroyed. To better understand the methods for measuring the biodegradability of starch, Figure 1 was applied. It shows that this parameter could be obtained by respirometric, morphological, spectroscopic, gravimetric, chromatographic, microbiologic, and physical and morphological techniques. ...
Context 2
... should be remarked that the biodegradation grad depends on the physical and chemical parameters, such as pH, moisture, temperature, air content, and nutrients [13]. The biodegradation of starch could be examined through some different methods from the work of [13] and Figure 1. The reactive hydroxyl group content on starch surface was not found in the literature, so it could be an innovative method to determine. ...
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Citations
... The main decomposition peak of 60TPS occurs between 240 and 370 • C, with a maximum decomposition rate temperature (T max ) of 319.5 • C, also showing two distinct shoulders. The main decomposition process is associated with the depolymerization of the amylose and amylopectin chains that constitute starch, resulting in the breakdown of glucose rings [36]. It is also related to the evaporation or decomposition of glycerin and water associated with starch as a consequence of the gelatinization process. ...
... The second stage occurred in the range of 150-350 °C with 60%-70% mass loss. This loss was mainly due to a series of degradation reactions, such as condensation between hydroxyl groups, further loss of water molecules and depolymerization of furan structures [36]. ...
This work systematically analyzed the microstructure and physicochemical properties of amylose (AM) and amylopectin (AP) isolated from tigernut starch (TS). The yields of AM and AP were 66.50% and 72.80%, respectively. Scanning electron micrographs showed that AM and AP were, structurally, very different from TS. Granules of AM and AP had rough surfaces and irregular shapes. AM had a V-type crystalline structure, while AP was believed to be amorphous. These structural differences influence their functional properties. AM had superior thermal stability and swelling characteristics, as well as high resistance to digestion. Meanwhile, AM gel had superior springiness and high chewability. While AP had good solubility and its paste was a liquid showing high fluidity. Collectively, these results are expected to provide new information valuable for future developments in the industrial application of AM and AP derived from TS.
Graphical abstract
... At a temperature of around 280°C, the start of the degradation reactions occurs when the hydroxyl groups in the starch chains thermally condense, causing the creation of ether fragments and the release of water molecules. [58] Differential scanning calorimeter was employed to determine the reaction and glass transition temperature as shown in Figure 12b. From the graph, it can be observed that the glass transition temperature value of the biocomposite corresponds to TGA analysis. ...
three mutual weight ratios of corn starch powder and polyvinyl acetate PVA wood glue were created for biocomposite materials: 40% starch/60% PVA, 50% starch/50% PVA, and 60% starch/40% PVA. Studying their physical, mechanical, thermal, electrical, and structural characteristics allowed for the evaluation of these composite materials. At room temperature, the samples were manually mixed. The results showed a decrease in the values of the AC conductivity and the thermal conductivity with an increase in the percentage of starch up to 60%, whereas the mechanical properties of the samples that contained starch at a concentration of 60% increased. An FTIR spectroscopy study showed the generation of α-pinene, which has an anti-inflammatory effect that impacts bacterial and fungal growth, in addition to the alkane group, which leads to decreased thermal conductivity. The prepared material showed better solidity, improved tensile strength, and excellent stability. On the whole, the prepared material showed enhancement in physical, mechanical, and thermal properties. Thus, this study could have the potential to develop starch-incorporated composite materials.
... 73 In comparison, starch showed peaks stretching from 85°C to 150°C related to water vapor, followed by a single degradation step at 320°C composed mainly of H 2 O, CO 2 , as well as other signals assigned to CH-(2969 cm −1 ) CvO (1730 cm −1 ), C-O (1057 cm −1 ) bonds, likely related to volatile products, such as glycol-and acetaldehyde. 74,75 Individual vibration peak assignment of the evolved gases can be found in the ESI (Fig. S3 †). ...
Starch derivatizations require harsh chemicals as solvents or catalysts, which can negate the green nature of starch-based materials. Often, these reaction systems require several hours to achieve moderate degrees of substitution (DS), drastically reduce molar mass and can result in undesired crosslinking compromising solubility. Here, we report an efficient and sustainable starch esterification with acetic anhydride (AA) and the optimization of the process avoiding initiators in terms of molar ratios, time, and temperature. Furthermore, chromatographic (HPSEC-MALS-dRI) and spectroscopic (FTIR, 1H NMR, 2D HSQC and HMBC, Solid State CP/MAS 13C NMR, TG-IR) tools were implemented to elucidate the chemical composition and structure of the resulting starch acetates and potential intermediate side reaction products over the course of the reaction. Different combinations of choline chloride (ChCl) with several hydrogen bond acceptors (urea, tartaric, malonic, and malic acids) were used as both chaotropic solvents and reaction promoters for starch acetylation. The reaction system comprising 1 : 1 molar ChCl : urea and AA showed good miscibility at 100 °C after 30 min, representing a seemingly homogeneous reaction system while better preserving starch molar mass. Side products emerging from solvent-reagent interactions, such as starch carbamate and acetylurea, were identified. Reaction optimization resulted in no side products, fast reaction rates (36 min), high DS (2.87) and starch loads (20 wt%), and increased reaction throughput and atom economy. Catalyst-free starch acetylation reduced hygroscopicity and increased glass transition and degradation temperatures (162 °C and 397 °C, respectively), while generally keeping a relatively higher molar mass (1.5–2.9 × 106 Da) than traditional starch acetates.
... Ïðîöåñè äåêñòðèí³çàö³¿ êðîõìàëþ íåîäíîðàçîâî âèâ÷àëè òåðì³÷íèìè ìåòîäàìè àíàë³çó [4][5][6][7][8][9][10]. Âñ³ àâòîðè â³äì³÷àþòü, ùî íà òåðìîãðàâ³ìåò-ðè÷íèõ (ÒÃ) êðèâèõ ïðèñóòí³ äâ³ ä³ëÿíêè çìåíøåííÿ ìàñè äëÿ ð³çíèõ âèä³â íàòèâíèõ êðîõìàë³â. ...
... ISSN 0321-4095, Voprosy khimii i khimicheskoi tekhnologii, 2023, No. 6, pp. 150-157 Äðóãà ñòàä³ÿ çìåíøåííÿ ìàñè íà Òà êðèâèõ, ÿêó àâòîðè [10] íàçèâàþòü ãîëîâíîþ ñòà䳺þ ðîçêëàäàííÿ êðîõìàëþ, ïî÷èíàºòüñÿ ïðè 200 0 C ³ çà-ê³í÷óºòüñÿ ïðèáëèçíî ïðè 350 0 C. Ïîâ³äîìëÿºòüñÿ, ùî ïðè òåðì³÷íîìó ðîçêëàäàíí³ êðîõìàëþ íà ö³é ñòà䳿 âèä³ëÿºòüñÿ âîäà, âóãëåêèñëèé ãàç, ìîíîîêñèä âóãëåöþ, àöåòàëüäåã³ä, ìåòàí, ôóðàí ³ 2ìåòèëôóðàí [6]. Î÷åâèäíî, ùî ñï³ââ³äíîøåííÿ êîíñòàíò øâèäêîñòåé ðîçãëÿíóòèõ íà ñõåì³ õ³ì³÷íèõ ðåàêö³é ìîaeå âàð³þâàòèñÿ â çàëåaeíîñò³ â³ä ñêëàäó êðîõìàëþ òà áàãàòüîõ ³íøèõ ÷èííèê³â, òàêèõ ÿê øâèäê³ñòü íàãð³âó, ñòóï³íü êðèñòàë³-÷íîñò³, ñï³ââ³äíîøåííÿ àì³ëîçà/àì³ëîïåêòèí, ïðè-ñóòí³ñòü êàòàë³çàòîðó òîùî. ...
... Âèêî-íàí³ íèìè ðîçðàõóíêè ïîêàçàëè, ùî ðîçêëàäàííÿ êðîõìàëþ ç á³ëüøîþ ê³ëüê³ñòþ àì³ëîïåêòèíó ïîòðåáóº á³ëüøî¿ åíåð㳿 àêòèâàö³¿. Çà äàíèìè àâòîð³â [10] â ³íòåðâàë³ 290-330 0 Ñ åíåðã³ÿ àê-òèâàö³¿ ñêëàäຠ66,5 êÄae/ìîëü äëÿ êàðòîïëÿíîãî êðîõìàëþ ³ 167 êÄae/ìîëü äëÿ êóêóðóäçÿíîãî êðîõìàëþ. Àâòîðè [9] ïðîâåëè àíàëîã³÷í³ ðîçðàõóíêè äëÿ êðîõìàëþ ñîëîäêî¿ êàðòîïë³ ³ âñòàíîâèëè, ùî åíåðã³ÿ àêòèâàö³¿ ñêëàäຠ174 êÄae/ìîëü. ...
In order to compare the kinetic characteristics of the heat treatment of starches and solve the question of what has a greater influence on the processes of their dextrinization, the chemical composition or their botanical origin, we carried out research by using methods of thermogravimetry and differential scanning calorimetry. It was shown for the first time that there is a process with heat absorption at 1300C in the temperature range of 25–2000C, in addition to the stages of dehydration of starches, which is not accompanied by a decrease in weight. This endoeffect is well explained by the melting process of the low-molecular amylose fraction of starches. In contrast to literature data, it was also established that the stage of starch decomposition in the temperature range of 200–3500C should be considered as a set of three consecutive processes. It was established that the activation energies of dehydration processes of pre-dehydrated starches are equal to 60 kJ mol–1. The average activation energy аor the stages of destruction of starches is 400–500 kJ mol–1. Such values of the activation energy of starch destruction processes are explained by the presence in their composition of a number of semi-crystalline subcomponents characterized by different thermal stability. When comparing the values of the activation energies of the dehydration and dextrinization processes of the investigated starches, a linear correlation was established for the first time, which testifies to the uniformity of such processes and their independence from the botanical origin of the starches.
... A trace of glucose was also observable in the enzymeless control: this reaction mixture had been incubated for the longest incubation time (coinciding with those of amylase and Driselase) at the highest temperature (37 C). These conditions might have provoked the degradation of a glucose-containing polymer such as starch (Pigłowska et al., 2020). Driselase is unlikely to contain L-galactosidase activity, although it does contain activities that might have been expected to release other monosaccharides present in Chlorokybus pectin: Ara (assumed to be L-), and Xyl and GalA (both assumed to be D-). ...
All land‐plant cell walls possess hemicelluloses, cellulose and anionic pectin. The walls of their cousins, the charophytic algae, exhibit some similarities to land plants’ but also major differences. Charophyte ‘pectins’ are extractable by conventional land‐plant methods, although they differ significantly in composition. Here, we explore ‘pectins’ of an early‐diverging charophyte, Chlorokybus atmophyticus , characterising the anionic polysaccharides that may be comparable to ‘pectins’ in other streptophytes. Chlorokybus ‘pectin’ was anionic and upon acid hydrolysis gave GlcA, GalA and sulphate, plus neutral sugars (Ara≈Glc>Gal>Xyl); Rha was undetectable. Most Gal was the l ‐enantiomer. A relatively acid‐resistant disaccharide was characterised as β‐ d ‐GlcA‐(1→4)‐ l ‐Gal. Two Chlorokybus ‘pectin’ fractions, separable by anion‐exchange chromatography, had similar sugar compositions but different sulphate‐ester contents. No sugars were released from Chlorokybus ‘pectin’ by several endo‐hydrolases [(1,5)‐α‐ l ‐arabinanase, (1,4)‐β‐ d ‐galactanase, (1,4)‐β‐ d ‐xylanase, endo‐polygalacturonase] and exo‐hydrolases [α‐ and β‐ d ‐galactosidases, α‐(1,6)‐ d ‐xylosidase]. ‘Driselase’, which hydrolyses most land‐plant cell wall polysaccharides to mono‐ and disaccharides, released no sugars except traces of starch‐derived Glc. Thus, the Ara, Gal, Xyl and GalA of Chlorokybus ‘pectin’ were not non‐reducing termini with configurations familiar from land‐plant polysaccharides (α‐ l ‐Ara f , α‐ and β‐ d ‐Gal p , α‐ and β‐ d ‐Xyl p and α‐ d ‐Gal p A), nor mid‐chain residues of α‐(1→5)‐ l ‐arabinan, β‐(1→4)‐ d ‐galactan, β‐(1→4)‐ d ‐xylan or α‐(1→4)‐ d ‐galacturonan. In conclusion, Chlorokybus possesses anionic ‘pectic’ polysaccharides, possibly fulfilling pectic roles but differing fundamentally from land‐plant pectin. Thus, the evolution of land‐plant pectin since the last common ancestor of Chlorokybus and land plants is a long and meandering path involving loss of sulphate, most l ‐Gal and most d ‐GlcA; re‐configuration of Ara, Xyl and GalA; and gain of Rha.
... The maximum value of the peak in the DTG curve represented the maximum mass loss rate, and the peak temperature reflected the thermal stability of the polymer. Compared to unfreeze-thawed native starch, freeze-thaw treatment could improve the thermal stability of Castanea henryi starch [47]. than that of the sample without Tremella fuciformis polysaccharide, as shown in Figure 4B (245.3 °C) < Figure 4C (301.27 ...
... The maximum value of the peak in the DTG curve represented the maximum mass loss rate, and the peak temperature reflected the thermal stability of the polymer. Compared to unfreeze-thawed native starch, freeze-thaw treatment could improve the thermal stability of Castanea henryi starch [47]. ...
The purpose of this study was to investigate the effect of Tremella fuciformis polysaccharides on the physicochemical properties of freeze–thawed cone chestnut starch. Various aspects, including water content, crystallinity, particle size, gelatinization, retrogradation, thermal properties, rheological properties, and texture, were examined. The results revealed that moderate freezing and thawing processes increased the retrogradation of starch; particle size, viscosity, shear type, hinning degree, and hardness decreased. After adding Tremella fuciformis polysaccharide, the particle size, relative crystallinity, and gelatinization temperature decreased, which showed solid characteristics. Consequently, the inclusion of Tremella fuciformis polysaccharide effectively countered dehydration caused by freezing and thawing, reduced viscosity, and prevented the retrogradation of frozen–thawed chestnut starch. Moreover, Tremella fuciformis polysaccharide played a significant role in enhancing the stability of the frozen–thawed chestnut starch. These findings highlight the potential benefits of incorporating Tremella fuciformis polysaccharides in starch-based products subjected to freeze–thaw cycles.
... This indicates that the addition of non-starch ingredients destroys the thermal stability of the samples, which to some extent, explains the collapse of the internal structure of the bread during baking and the change in specific volume. The peak of the samples represents the maximum loss rate (Pigøowska et al., 2020). The maximum loss rates of four samples were exhibited as below: WF = 0.19%, WF + P = 0.18%, WF + β = 0.19% and WF + P + β = 0.16%. ...
Whole wheat bread is rich in nutrition, but its starch digestibility is unsatisfactory. Thus, how to reduce its digestibility has attracted much attention. This study investigated the effects of highland barley protein and β‐glucan on the pasting properties, and thermal properties of whole wheat flour to reveal the mechanism of highland barley protein and β‐glucan regulating the in vitro digestibility. The digestibility results showed that β‐glucan and protein could slow down starch digestion to some degree. The cross‐section structure determination results indicated that β‐glucan and protein decreased the porosity. The differential scanning calorimetry and thermogravimetric analysis results showed that β‐glucan and protein increased the onset of pasting, decreased the peak temperature and enthalpy of pasting and decreased the thermal stability. The Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy results revealed a blue‐shift in the ‐OH position of the bread added with protein and β‐glucan (from 995.59 to 996.07 cm⁻¹), indicating that the hydrogen bonding might form intramolecularly. In this study, the addition of highland barley protein and β‐glucan was proved to be helpful in decreasing the in vitro digestibility and showed modification in the texture quality of bread, which might be suitable for diabetic patients.
... However, all treated samples that were precipitated with sodium hydroxide show stages of decomposition. The maximum DTG peaks represent the maximum rate of mass loss [28]. ...
In this work, nanorod particles were synthesized from a locally available source, glutinous rice flour, using sodium hydroxide (NaOH) through a simple precipitation process. The synthesized nanofillers were then presented as an alternative organic filler for dental impression application to support the making of a diagnostic and working model. Dynamic Light Scattering, Scanning Electron Microscope, Fourier Transform Infrared Spectroscopy, X-ray Diffraction, Energy Dispersive Spectroscopy, Thermogravimetric Analysis, and Differential Scanning Colorimeter were used to characterize the fillers. The particle size measurement, morphology interaction, and composition of glutinous rice flour nanorod particles were also investigated. The cell viability using 3T3L1 cells was assessed to determine the safety of nanorod particles using the MTT assay and trypan blue solution. All treated samples exhibit a change in particle morphology from polyhedral to rod. We observed a decrease in crystallinity, dehydration, and gelatinization temperature. Its functional group interacting with sodium hydroxide also changes slightly after size reduction. The samples treated with 3000 centrifugation speed without surfactant addition showed changes from the control sample's 3931.71 nm to the smallest average width particle size of 73.26 nm with an average length of 865.15 nm. All of the treated samples with NaOH and NaOH-surfactant additions met the non-cytotoxicity acceptance criteria in the range of 73.54-99.58%, according to the cell viability results. The incorporation of 15 wt% of the synthesized nanorod fillers resulted in a 20 µm continuous line as the impression materials specimen, yielding a satisfactory detail reproduction test result. In conclusion, nanorod particles with biocompatible properties have been successfully manufactured and can potentially be used in the future as an alternative dental impression filler materials.
... 4,28 Finally, the TGA results (Table 1) showed that triticale starch was the most heat-resistant material with an intense endothermic curve in a temperature range of 272-350°C, with ~50% of mass degradation (within the maximum peak at 315°C) and activation energy (Ea) of 126.75 kJ/mol, similar to the TGA/Ea results from different starch sources. 29 It has been reported that the first stage of pyrolysis is due to chain depolymerization, followed by ring decomposition, and carbonization as the final degradation process. The increase in amylose promotes thermal degradation, so the initial drop in weight was due to catalytic depolymerization of the α-1,4 bond, starting with the lowest molecular weight chains. ...
... The increase in amylose promotes thermal degradation, so the initial drop in weight was due to catalytic depolymerization of the α-1,4 bond, starting with the lowest molecular weight chains. 29,30 Although there are recent reports of the thermal characterization of triticale starch by differential scanning calorimeter and hybrid rheometer, those studies only reached gelatinization temperatures (~60°C), and by TGA/DTG the thermal decomposition of triticale straw was reported, however, the straw contains polymeric mixtures and diverse biomass of low molecular weight that allowed higher heat resistance (200- The TGA kinetics results presented in Table 1 together with the TGA/DTG figure ( Figure S2 in supporting information) reinforced the previous theory by considering that triticale starch was the most heat-resistant material followed by HG-I, which allowed a slightly higher thermal stability (peak temperature Tp~180-327°C) compared to HG-II and HG-III (Tp~169-324°C). In turn, a similar Ea (at the same temperature rate) is necessary for a lower weight drop in HG-I compared to HG-II and HG-III; Ea can be obtained from the onset and the final decomposition temperature range (To and Tf), while weight drop can be obtained from the peak temperature Tp in the DTGs (see Figure S3 in supporting information for comparative visualization of the Ea). ...
... The first weight loss is related to the water evaporation (100-150°C), followed by the breaking of the acid bond between 200°C, and consequent pyrolysis of the properties of glycosidic bonds between polymer chains (274-350°C). 29,30,39 The degradation kinetic parameters of the present study were slightly similar between the control hydrogel and the experimental ones (see Figure S2 in supporting information). At first, the control HG showed slightly higher thermal stability in the range of 25-300°C. ...
Considering the FAO perspectives for agriculture towards 2030, many natural sources will be no longer profitable for the synthesis of many biomaterials. Triticale (X Triticosecale Wittmack) is a cereal crop synthesized to withstand those marginal conditions; however, it is primarily used as fodder worldwide. We reported for the first time the synthesis of a natural anionic hydrogel with gastrointestinal pH stimulus-response as new alternative of smart material, based on Eronga triticale starch as sustainable biomass, using citrate (pKa~3.1, 4.7 and 6.4) as cross-linking agent. By scanning electron microscopy and X-ray diffraction, starch granules exhibited size and semi-crystallinity A-type. The presence of the anionic sensing group (COOH) was verified by infrared spectroscopy, and through thermal analysis hydrogels exhibited four endothermic curves (115-393°C, ~1.4-38 kJ/mol Ea). The rheological analyzes showed viscoelastic tendency (G’>G’’) with high stability (Tan δ<1) in frequency, time, and strain sweeps. Gastrointestinal pH sensitivity (~2-7.8) was verified (α≤0.01) following Fick’s diffusive parameters, which resulted in a tendency to gradually release BSA with increasing pH~3-7 by anomalous and case-II diffusion, showing greater release at pH~7.8/3.5h (80-96%). We aim to expand the biomaterials area focusing on triticale starch due its limited reported investigations, low-cost, green modification, and its rheological performance as plastic.
