Modified starch granules as particle-stabilizers of oil-in-water emulsions

Oil-in-water (O/W) emulsions of 20 vol% n-tetradecane have been prepared using food-compatible hydrophobic starch particulates as the primary emulsifier. As such, the systems appear to be Pickering emulsions. The starch particulates were generated from chemically cross-linked granules that do not swell on prolonged contact with water and which were made partially hydrophobic by reaction with octenyl succinic anhydride. The degree of substitution was of the order of 0.03. The size of the modified starch particulates was reduced by freezer-milling before preparing the emulsions via a jet homogenizer. Conventional light transmission microscopy, confocal laser scanning microscopy, scanning electron microscopy, multi-angle light scattering and laser Doppler light scattering all suggested that a wide range of starch particle sizes was produced. Some particles were considerably smaller than the original starch granule sizes, but a large proportion appeared to be above several microns in size. The emulsion droplets produced using 1–3 wt.% of starch as emulsifier were quite large (from approximately 1 to 20 μm in diameter), i.e., of the same order of size as a large proportion of the starch particulates. Consequently, the emulsions creamed readily, but they were extremely stable to coalescence with no significant change in the emulsion droplet-size distributions appearing for over 3 months. Further tests on the surface tensions of the homogenized and non-homogenized starch dispersions themselves confirmed the supposition that the O/W emulsions were stabilized by starch particulates and not starch molecules.     

α-Amylolysis of native potato and corn starches - SEM, AFM, nitrogen and iodine sorption investigations

Scanning electron microscopy (SEM), atomic force microscopy (AFM), as well as iodine and nitrogen sorption measurements were applied to investigate potato and corn starch granules surface after an action of Bacillus subtilis α-amylase. The SEM images revealed holes and pits (corn starch) or scratches (potato starch) on the surface of modified granules. These results were confirmed by AFM investigation which showed the presence of depressions of approximately 121 nm in diameter. Structure of the surface was not uniform. It consisted of small particles, amylopectin blocklets, of approximately 20 nm in diameter. They became more distinctive after α-amylolysis. Values of iodine binding capacity (IBC) obtained for hydrolyzed granules were lower than for native ones which indicated that the amylose and amylopectin chains building their surface were shortened. Specific surface area, volume and average diameter of mesopores increased for both starches after α-amylolysis.     

Physicochemical,thermal and pasting properties of starch separated from γ-irradiated and stored potatoes

The morphological, thermal and pasting properties of starch separated from potatoes of three varieties (Kufri Chandramukhi, Kufri Jyoti and Kufri Chipsona-2), treated either with CIPC (isopropyl N-(3 chlorophenyl) carbamate) or γ-irradiation (Co⁶⁰, 0.1 and 0.5 kGy) and subsequently stored at 8, 12 and 16 °C for 90 days, were studied. Scanning electron microscopy (SEM) showed the presence of oval and irregular shaped starch granules with a diameter range of 15–16 μm. Mean granule size of starch separated from potatoes stored at 12 °C ranged from 18–25 μm and irradiation treatment resulted in an increase in the proportion of small size granules. The irradiation of potatoes with 0.5 kGy resulted in starch with significantly lower peak-, trough- and breakdown-viscosity as compared to starch from potatoes treated with either CIPC or 0.1 kGy irradiation. The irradiation of potatoes with 0.5 kGy caused a significant increase in setback and pasting temperature. Pasting temperature of starch was observed to vary with the storage temperature. Starch separated from potatoes stored at higher temperature showed lower pasting temperature and vice versa. The starch from potatoes stored at 8 °C showed higher peak-, trough- and breakdown-viscosity and lower setback. Peak viscosity increased and swelling volume decreased with increase in storage temperature. FTIR spectra showed that the starch from irradiated potatoes displayed a significant decrease in the intensity of the C–H stretch region between 2800 and 3000 cm⁻¹, which was observed to be irradiation dose-dependent, and higher with 0.5 than 0.1 kGy. However, a slight broadening of O–H stretch (3000–3600 cm⁻¹) in starches from irradiated potatoes was observed. The spectral changes caused by γ-irradiation were apparent in the O–H stretch (3000–3600 cm⁻¹), C–H stretch (2800–3000 cm⁻¹) and bending mode of water (1600–1800 cm⁻¹).     

Synthesis and characterization of nano-encapsulated catechin by molecular inclusion with beta-cyclodextrin

Nano-encapsulation of catechin (CAT) with beta-cyclodextrin (BCD) at 1:1 ratio resulted in the production of nano-encapsulated powder (BCD + CAT) by molecular inclusion method. The interactions between CAT and BCD were analyzed by differential scanning calorimeter (DSC), Raman laser spectroscopy (RLS), scanning electron microscopy (SEM) and X-ray diffractometer (XRD). The results obtained strongly confirmed supra molecular complex formation. DSC thermograph obtained for nano-encapsulated powder resulted in the appearance of new endothermic melting peak at 250 °C with complete disappearance of peaks at 100, 150 and 200 °C present in catechin and beta-cyclodextrin indicating the inclusion complex formation which was also confirmed by spectral characterization (RLS). Particles ranging from 67 to 470 nm were obtained by SEM micrographs. Structural characterization by XRD at 2θ angle from 0° to 80° for nano-encapsulated powder indicated change of state from crystalline to amorphous phase with average particle size of 518.78 nm.     

Phase structures impact the rheological properties of rennet-casein-based imitation cheese containing starch

The dynamic rheological and microstructural properties of rennet-casein-based imitation cheeses containing various concentrations of potato starch were investigated using a stress-controlled rheometer and confocal laser scanning microscopy. The influence of added starch on the size of the oil droplets in the imitation cheeses was also examined. Imitation cheeses with 0–15% protein replaced by starch were processed in a Rapid Visco Analyser (RVA) at 90 °C for 10 min at a shear rate of 800 rev/min and were then evaluated using oscillatory shear measurement and a temperature sweep (20–90 °C). The storage modulus (G′) of the rennet casein imitation cheeses increased abruptly at added starch concentrations >4%. In the temperature range 20–90 °C, tan δ of the imitation cheeses decreased with increasing starch concentration and was <1 at added starch concentrations >4%. A binary continuous phase consisting of a protein phase and a starch phase was observed in systems containing >4% starch, whereas the starch was dispersed in the protein matrix as small particles of irregular shapes at added starch concentrations ≤4%. As the dispersed phase, the size of the oil droplets increased with starch addition in the imitation cheeses. The marked increase in G′ and the reduction in tan δ may be attributed to the formation of a binary continuous separated phase structure in imitation cheeses containing added starch that is driven by thermodynamic incompatibility between rennet casein and starch.     

Microstructural changes of starch in cooked wheat grains as affected by cooking temperatures and times

The changes of starch microstructure in soft and hard wheat grains after cooking in a pressure cooker were investigated using a scanning electron microscope (SEM) and a light microscope (LM) in conjunction with image analysis. The conditions studied included variation of the cooking times (20-120 min) at the constant temperature (120 °C) and with variable temperatures (110-140 °C) for constant time (40 min). SEM images showed that steam induced changes in the intact starch granules of cooked wheat grains, with the microstructure becoming more in mud-like structure, with increased cooking time or temperature. The swelling and gelatinization of starch granules could contribute to this change. Suspensions of cooked wheat flour were selectively stained with iodine, for observation using the LM. The image analysis software was used for quantitative analysis of the images captured from the LM, providing both the number and area of the starch granules (determined from the dark-blue spots) per fixed image size. With increased cooking time or temperature, the number of starch granules decreased and the area increased as a result from the swelling and melting of starch granules. This study demonstrated the use of SEM and LM for the investigation of starch granules in cooked wheat grains without prior starch isolation.     

Enzymatic hydrolysis of granular native and mildly heat-treated tapioca and sweet potato starches at sub-gelatinization temperature

The effect of mild heat treatment (below gelatinization temperature) towards the susceptibility of granular starch to enzymatic hydrolysis was investigated. Tapioca and sweet potato starches were subjected to enzymatic hydrolysis with a mixture of fungal α-amylase and glucoamylase at 35 °C for 24 h. Starches were hydrolyzed in native (granular) state and after heat treatment below gelatinization temperature (60 °C for 30 min). The dextrose equivalent (DE) value of heat-treated starch increased significantly compared to native starch, i.e., 36–50% and 27–34% for tapioca and sweet potato starch, respectively. Scanning electron microscopy examination showed that enzymatic erosion occurred mainly at the surface of starch granules. Hydrolyzed heat-treated starch exhibited rougher surface and porous granules compared to native starch. X-ray analysis suggested that enzymatic erosion preferentially occurred in amorphous areas of the granules. The amylose content, swelling power and solubility showed insignificant increase for both starches. Evidently, heating treatment below gelatinization temperature was effective in enhancing the degree of hydrolysis of granular starch.     

Viscoelastic behavior and microstructure of aqueous mixtures of cross-linked waxy maize starch,whey protein isolate and κ-carrageenan

The viscoelasticity and microstructure of mixtures of cross-linked waxy maize starch (CH10), whey protein isolate (WPI) and κ-carrageenan (κC) at pH 7.0 with 100 mM NaCl were investigated by oscillatory rheometry and confocal laser scanning microscopy (CLSM). Mixtures were heated to 90 °C (1.5 °C/min), held for 10 min at this temperature and cooled. Within the range of concentrations studied, CH10 swollen granules reinforced WPI and κC networks. The mechanical behavior of the three-component mixtures was modified by different WPI concentrations, but κC governed the overall response due to its gelling ability. CLSM images of three-component mixtures showed particulate systems in which swollen starch granules are surrounded by κC and WPI. CH10 granules were immersed in a single phase and a separate phase of κC and WPI, for low and high concentrations of these components, respectively. Therefore, it is possible to obtain two- and three-phase mixtures.     

酶预处理和酸水解制备糯玉米淀粉纳米晶及其表征

采用糖化酶对糯玉米原淀粉进行预处理,通过X射线衍射(XRD)确定糖化酶预处理的最佳用量,再对酶预处理淀粉进行硫酸酸水解,制备糯玉米淀粉纳米晶,采用傅里叶变换红外光谱（FT-IR）、扫描电子显微镜(SEM)、粒径测量和Zeta电位分析等对淀粉纳米晶进行表征。结果表明,用1000U/(g淀粉)活性的糖化酶对糯玉米原淀粉处理2h,再结合酸水解2天,得到粒径约100nm、分散性好、产率为24.1%的糯玉米淀粉纳米晶;相较于仅硫酸酸水解处理,酶预处理结合酸水解法制备糯玉米淀粉纳米晶的反应时间缩短了3天,产率提高了70.9%,淀粉纳米晶的Zeta电位达-22.3 mV。     

Microstructure and elastic modulus of mixed gels of gelatin + oxidized starch: Effect of pH

The microstructure and elastic shear modulus of cold-set gels formed from high-sugar aqueous mixtures of gelatin (7 wt%) + oxidized starch (0-6 wt%) were investigated as a function of pH. Samples prepared at 90 °C, with citric acid added to adjust the pH, were rapidly quenched to ∼1 °C, subjected to a standard thermal treatment (40 °C for 10 min), and then investigated by confocal microscopy and small-deformation rheology at 24 °C. Under ‘natural’ conditions of pH ≈ 5.2 (no citric acid addition), the samples exhibited phase separation with a characteristic spinodal-type morphology. The spatial extent of the structural heterogeneity, expressed by a single length-scale parameter, was found to increase with starch concentration. Gradual acidification led to a reduction in this length-scale parameter, leading to complete inhibition of phase separation below a certain characteristic pH value in the range 4.5-4.9 (depending on starch content). Over the investigated pH range, the effect of starch addition was to reduce the storage modulus of the resulting gel. This reduction was more pronounced for the phase-separated samples. The pH of maximum rigidity was found to decrease from pH_max ≈ 4.6 for 0 wt% starch to pH_max ≈ 4.2 for 6 wt% starch. Taken all together, these observations can be understood in terms of the effects of pH on the cross-linking behaviour of the gelatin and the nature of the gelatin-starch electrostatic interactions. The microscopy results are consistent with a transition in behaviour from thermodynamic incompatibility (segregative interactions) at high pH to soluble complexation (associative interactions) at low pH.     

In vitro digestion rate and resistant starch content of tortillas stored at two different temperatures

In vitro indicators of starch bioavailability were evaluated in freshly prepared maize tortillas and compared to those exhibited by 24, 48 or 72 h-stored samples. Storage took place either at room temperature (approx. 25 °C) or under refrigeration (4 °C). Potentially available starch (AS) content decreased from 670 g kg⁻¹ in the control tortilla to 583 g kg⁻¹ in 72 h-stored preparations. Concomitant increases in total resistant starch (RS) and retrograded resistant starch (RRS) were recorded upon storage. RRS content in 72 h-stored samples (35-39 g kg⁻¹) doubled that of freshly prepared tortillas. Changes in AS, RS and RRS were not affected by storage temperature. Both initial rate and final point of starch hydrolysis by pancreatic amylase were reduced in samples kept for 48 and 72 h, without influence of storage temperature. Storage length is suggested as a major determinant of the bioavailability of starch in tortillas.     

生物酶法制备蜡质玉米淀粉纳米晶及其表征

淀粉纳米晶是从天然淀粉中制得的一种纳米尺寸的聚多糖晶体。本试验通过糖化酶部分酶解蜡质玉米淀粉,并对其进行超声波处理,离心后经真空冷冻干燥得到淀粉纳米晶。采用扫描电子显微镜、激光粒度分布仪、X-射线衍射、傅里叶红外光谱等手段对淀粉纳米晶进行表征。结果表明:淀粉纳米晶颗粒表面粗糙,颗粒之间由于静电引力相互聚集;酶解得到的淀粉纳米晶的粒径集中在100 nm左右,结晶度为75.86%,产率达到27.53%。酶法制备过程对环境无污染,是一种新型的纳米晶绿色制备技术。     

Water dynamics in white bread and starch gels as affected by water and gluten content

Three levels of water (180, 220 and 260 g/345 g flour) and three levels of gluten (giving 11.2, 13.0 and 14.2 g protein/100 g flour) were used to study the effects of water and gluten on water mobility in white bread using ¹H nuclear magnetic resonance (NMR) relaxometry. Changes in the transverse relaxation time (T₂) were related to water mobility. The three water levels resulted in three different moisture contents in the finished bread (0.55-0.77 g H₂O/g solids). Distributed exponential analysis showed two distinct regions of T₂ (30-600 μs and 1-60 ms), associated with multiple domains of water in the bread crumb. There was no significant difference in peak T₂ values with different gluten content, but significant differences were observed with different moisture content. The results suggested that the mobility of water associated with starch decreased dramatically because of gelatinization. To further investigate the effect of gluten on starch gelatinization, NMR measurements were made directly on model systems containing starch and various gluten amounts. The starch-gluten gels had higher T₂ values than pure starch gels, indicating less swelling of starch granules and absorption of water. This was attributed to less water available to starch in the presence of gluten.     

Microstructural evaluation of deep-fat fried chicken nugget batter coating using confocal laser scanning microscopy

Porosity and pore size distribution are very important microstructural properties of fried foods needed in process optimization and product development. The objective of this study was to characterize the pore properties and quantify fat distribution in deep-fat fried chicken nuggets batter coating using confocal laser scanning microscopy. Samples were fried at three temperatures namely 170, 180 and 190 °C. Detached batter coatings were stained non-covalently and 2-D images were obtained at fluorescence and reflection modes of the microscope. The images were analyzed for fat and pore distribution. Fat distribution obtained from image analysis was significantly (P < 0.05) affected by the frying temperature and time, and it decreased within the depth of the sample thickness. There was a strong correlation between fat distribution and fat content obtained by the conventional method at two temperatures, 180 and 190 °C. Porosity ranged between 4.97% and 32.7% and was significantly influenced by frying temperature. Pore size varied approximately between 1.20 and 550 μm. Frying process led to the formation of more micropores (pores < 40 μm) and bigger (pore ? 216 μm) pores.     

Technical note: a near-infrared reflectance spectroscopy technique to predict particle size of starch within corn silage

Starch particle size characteristics of 81 diverse corn silage samples, which included 27 combinations of hybrid, planting dates, and harvest dates subjected to 3 different degrees of kernel processing, were determined via vertical shaking through 9 screens with nominal square apertures of 19.0, 13.2, 9.5, 6.7, 4.75, 3.35, 2.36, 1.18, and 0.6 mm and a pan. Starch content of dry matter remaining on each screen and on the pan for each corn silage was determined, and geometric mean particle size (GMPS, μm), starch particles(SP)/g, starch surface area (SSA, cm²/g), kernel processing score (KPS), % starch < 4.75 mm, and the percentage of total starch remaining on each screen of the vertical shakers were calculated. Near-infrared reflectance spectra were obtained by scanning 3 types of samples: 1 mm of dried ground corn silage; whole undried, unground corn silage; and undried, unground corn silage that passed through a 19-mm screen. Calibrations to predict GMPS, SP, SSA, and KPS characteristics of corn silage starch were attempted from each spectral origin. Calibrations to predict GMPS, SP, SSA, KPS, and the percentage of total starch retained on screens of the vertical shaker was unattainable (R² < 0.45) using spectra obtained from 1 mm of dried ground corn silage or whole undried, unground corn silage. However, reasonable near-infrared reflectance spectra equations (R² > 0.81) for GMPS, SSA, and KPS were attained using spectra from undried, unground corn silage that passed through a 19-mm screen. This technique holds promise as a rapid and efficient method to determine particle size characteristics of starch within corn silage.     

Use of transient and steady-state methods and AFM technique for investigating the water transfer through starch-based films

The aim of this study was to investigate the water transfer properties of starch films using steady-state and transient methods and to evaluate the influence of air relative humidity on the film roughness using atomic force microscopy (AFM). Films were prepared with 3% starch and 0.3 g glycerol/g dry starch. Composite-films were prepared with the addition of 0.3 g cellulose/g dry starch. Water transfer through the films exhibited a dependence on the relative humidity RH. Using AFM, film roughness was observed to increase from a few nanometers to 45 nm over 1.5 h when the films were exposed to high RH. Results indicated that the equilibrium conditions at the film surface were not reliable boundary conditions and that the diffusion coefficients determined by both transient and steady-state methods may be different because they were determined at different conditions. Further studies of water permeability, assisted by AFM, could be performed for a better understanding of film barrier properties.     

Effect of gelatinisation on slowly digestible starch and resistant starch of heat-moisture treated and chemically modified canna starches

The effects of gelatinisation on slowly digestible (SDS) and resistant starch (RS) of native and modified canna starches were investigated. Starch slurries (10% w/w) were gelatinised at 100 °C for 5, 10, 20 and 40 min using a rapid visco analyzer (RVA). Significant change in the degree of gelatinisation (DG) values of all starch samples was observed during the initial 10 min of gelatinisation; after that the DG values increased gradually with gelatinisation time. The RS contents in all gelatinised starches decreased with increasing gelatinisation time, while the SDS values fluctuated. Chemical modification affected DG values as well as RS/SDS contents. The RS contents in 10% (w/w) acetylated, hydroxypropylated, octenyl succinylated and cross-linked canna starches gelatinised at 100 °C for 40 min were 26.6%, 32.0%, 45.3% and 19.8%, respectively, which were higher than that of the native starch (12.4%). Canna starch modified by crosslinking had the highest SDS content when gelatinised for 20-40 min. Modification of canna starch by heat-moisture treatment resulted in a lower content of RS for all treated samples. However, the Vt-HMT25 (canna starch containing moisture content of 25% during heat treatment) when gelatinised for 5-20 min contained a higher amount of SDS, compared to unmodified starch. The most effective modification method for RS and SDS formation was octenyl succinylation, where the sum of RS and SDS approached that of Novelose260.     

Evaluation of lower-starch diets for lactating Holstein dairy cows

The objective of this experiment was to measure ruminal and lactational responses of Holstein dairy cows fed diets containing 3 different starch levels: 17.7 (low; LS), 21.0 (medium; MS), or 24.6% (high; HS). Twelve multiparous cows (118 ± 5 d in milk) were assigned randomly to dietary treatment sequence in a replicated 3 × 3 Latin square design with 3-wk periods. All diets were fed as total mixed rations and contained approximately 30.2% corn silage, 18.5% grass silage, and 5.0% chopped alfalfa hay. Dietary starch content was manipulated by increasing dry ground corn inclusion (% of dry matter) from 3.4 (LS) to 10.1 (MS) and 16.9 (HS) and decreasing inclusion of beet pulp and wheat middlings from 6.7 and 13.4 (LS) to 3.4 and 10.1 (MS) or 0 and 6.8 (HS). In vitro 6-h starch digestibility of the diet increased as nonforage sources of fiber replaced corn grain (% of dry matter; 73.6, HS; 77.3, MS; 82.5, LS) resulting in rumen-fermentable starch content by 14.6, 16.2, and 18.1% for the LS, MS, and HS diets, respectively. Diets had similar neutral detergent fiber from forage and particle size distributions. Dry matter intake, solids-corrected milk yield, and efficiency of solids-corrected milk production were unaffected by diet, averaging 26.5 ± 0.8, 40.8 ± 1.6, and 1.54 ± 0.05 kg/d, respectively. Reducing dietary starch did not affect chewing time (815 ± 23 min/d), mean ruminal pH over 24 h (6.06 ± 0.12), acetate-to-propionate ratio (2.4 ± 0.3), or microbial N synthesized in the rumen (585 ± 24 g/d). Total tract organic matter digestibility was higher for HS compared with MS and LS diets (69.2, 67.3, and 67.0%, respectively), but crude protein, neutral detergent fiber, and starch digestibilities were unaffected. As dietary starch content decreased, in vitro ruminal starch fermentability increased and, consequently, the range between HS and LS in rumen-fermentable starch (3.5 percentage units) was less than the range in starch content (6.9 percentage units). Under these conditions, dietary starch content had no measurable effect on ruminal fermentation or short-term lactational performance of high-producing Holstein dairy cows.     

Preparation and properties of octenyl succinic anhydride modified potato starch

Potato starch was esterified with octenyl succinic anhydride (OSA) in aqueous slurry systems and the major factors affecting the esterification were systematically investigated. The physico-chemical properties of the products were determined by means of Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction and a viscosity analyser (VA). The results indicated that suitable parameters for the preparation of OSA starch from potato in aqueous slurry systems were as follows: concentration of starch slurry, 35% (in proportion to water, w/w), reaction period, 3 h, pH of reaction system, 8.0, reaction temperature, 35 °C, amount of OSA, 3% (in proportion to starch, w/w), OSA dilution-fold, 5. The degree of substitution (DS) was 0.017 and the reaction efficiency (RE) was 72 ± 1.8%. FT-IR spectroscopy showed characteristic absorption of the ester carbonyl groups in the OSA starch at 1724 cm⁻¹. SEM and X-ray diffraction revealed that OSA groups acted by first attacking the surface and some pores formed, but OSA modification caused little change in the crystalline pattern of potato starch (DS 0.045). Apparent pastiness measurement indicated that the starch derivatives gelatinized within a shorter time to achieve higher viscosities over the range of designed concentration of OSA potato starch.     

Effect of high pressure on binding aroma compounds by maize starches with different amylose content

Hylon VII, waxy maize starch and their mixtures were subjected to high pressure treatment (650 MPa/9 min). To obtain starch-odorants products: (i) the pressurised and native starches were incubated with odorants; and (ii) the native starches mixed with odorants were treated under high pressure (650 MPa/9 min). The sorption capacity of odorants by investigated starches was studied using capillary gas chromatography.The sorption capacity of odorants by native starches was found to stronger depend on hydrophobicity and molecular structure of odorants rather than the starch botanical origin. The highest sorption was observed for polar hydrophobic compounds (hydrocarbons) and for aliphatic esters, whereas the lower one—for guaiacol and methyl anthranilate. The high pressure-treated Hylon VII demonstrated slight changes in melting enthalpy and degree of gelatinisation compared to other starches and it showed the highest sorption capacity of the majority of odorants. The treatment of a starch with odorant under 650 MPa for 9 min resulted in a diminished average sorption of the aroma compounds. However hexanol, guaiacol and methyl antrinilate, that were slightly or not sorbed by native and high pressure-treated starches, demonstrated the highest degree of binding with waxy starch and its mixtures under high pressure conditions.