Lih-Shiuh Lai

This study investigates the effects of microwave post-treatment and fatty acid type on the physicochemical properties of starch–lipid complexes derived from water caltrop (Trapa taiwanensis Nakai) starch. Complexes were prepared using stearic acid (C_18:0) or oleic acid (C_18:1), followed by microwave post-treatment at varying durations. Morphological analysis revealed that the starch–stearic acid complex exhibited more plate-like structures and birefringent spots compared to the starch–oleic acid complex. The complexing index increased with extended microwave exposure, indicating enhanced complex formation. Fourier-transform infrared spectroscopy showed no significant variation in the 1047/1022 cm⁻¹ absorption ratio, suggesting that the short-range molecular order remained unaffected. However, X-ray diffraction analysis indicated increased relative crystallinity, particularly in the stearic acid complex (10.4%) compared to the oleic acid complex (4.8%), likely due to the higher linearity and saturation of stearic acid. Differential scanning calorimetry confirmed the presence of both type I and type II crystallization in all samples. The starch–stearic acid complex exhibited greater thermal stability, promoted type II crystallization, and enhanced the ordered structure of type I crystallization. In contrast, microwave treatment had limited influence on the thermal properties of the starch–oleic acid complex. These findings demonstrate that microwave post-treatment facilitates starch–lipid complex formation and improves structural organization, particularly when saturated fatty acids are employed.

This study investigates the effect of ultrasonic-assisted preparation on the structural and physicochemical properties of water caltrop starch-palmitic acid complexes as a function of ultrasound intensity and treatment time. All samples exhibited the characteristic birefringence of starch-lipid complexes under the polarized microscope, and flake-like and irregular structure under scanning electron microscope (SEM), indicating the formation of complexes through ultrasonic-assisted preparation. X-ray diffraction pattern further confirmed the transition from the original A-type structure for native starch to V-type structure for starch-lipid complexes, and the relative crystallinity of starch-lipid complexes increased as the ultrasound intensity and treatment time increased. Attenuated total reflectance-Fourier-transform infrared spectroscopy (ATR-FTIR) analysis indicated a decreasing trend in absorbance ratio at wavenumber of 1022 cm⁻¹/995 cm⁻¹, suggesting that the increase in the complex promoted the self-assembly within the short-range ordered structure, leading to the formation of bonds between the complexes. However, rapid-visco analysis (RVA) demonstrated that the viscosity generally decreased as the ultrasound intensity and treatment time increased, possibly due to the reduction in molecular weight by ultrasound. Differential scanning calorimetric (DSC) analysis revealed that the control starch-lipid complex without ultrasound treatment (US-0-0) exhibited two distinct endothermic peaks above 90 °C, representing Type I (95–105 °C) and Type II (110–120 °C) V-type complexes. However, ultrasound-treated samples showed only one peak around 95–105 °C and increased enthalpy (∆H), which was likely due to the breakdown of amylose and amylopectin, leading to more complex formation with palmitic acid, while the resulting shorter chains in the ultrasound-modified sample favor the formation of Type I complexes.

The effects of treatment time of continuous annealing (ANN) and cycle numbers of cycled ANN on the structural, physicochemical, and digestive properties of water caltrop starch were studied under 70% moisture at 65 °C. It was found that continuous and cycled ANN have no significant effects on the morphology of starch granules. However, the relative crystallinity and content of resistant starch increased pronouncedly, possibly due to crystalline perfection, which also led to the rise in gelatinization temperature and the narrowed gelatinization temperature range of starch. The treatment time in continuous ANN generally showed a pronounced effect on the rheological properties of water caltrop starch. During pasting, the breakdown viscosity and setback viscosity of all treatment decreased, implying that ANN modified starch was less susceptible to the condition in heating and continuous shearing, and less likely to cause short-term retrogradation. In contrast, peak viscosity decreased with increasing treatment time of continuous ANN, indicating crystalline perfection restricted the swelling of starch granules and viscosity development during pasting process, which was consistent with the results of steady and dynamic rheological evaluation. All ANN-modified samples showed pseudoplastic behavior with weak gel viscoelastic characteristic. Under a total annealing time of 96 h, the pasting and rheological properties of water caltrop starch were essentially less affected by annealing cycle numbers. However, multistage ANN showed stronger resistance to enzyme hydrolysis.

The structural and functional properties of Citrus grandis Osbeck (CGO) seed mucilage by different extraction practices, including conventional citrate buffer, ultrasonic-assisted (UAE), enzymatic-assisted extraction (EAE) with cellulase or Celluclast^® 1.5 L and various ultrasonic-assisted enzymatic extraction (UAEE) procedures were investigated. It was found that CGO seed from agricultural and processing byproducts is an excellent new source of high methoxyl pectin with quite high intrinsic viscosity (about 108.64 dL/g) and molecular weight (about 1.9 × 10⁶) as compared with other pectin sources. UAEE with Celluclast^® 1.5 L enhanced the extraction yield most pronouncedly (about 2.3 times). Moreover, the monosaccharide composition of CGO seed mucilage is least affected by EAE with Celluclast^® 1.5 L. In contrast, EAE with cellulase dramatically reduces the galacturonic acid (GalA) content to less than 60 molar%, and increases the glucose (Glc) content pronouncedly (to about 40 molar%), which may be considered as an adverse effect in terms of pectin purity. Though extraction procedures involved with ultrasound and cellulolytic enzymes generally show a decrease in GalA contents, weight average molar mass and intrinsic viscosity, EAE with Celluclast^® 1.5 L is least affected, followed by UAE and UAEE with Celluclast^® 1.5 L. These features can be leveraged in favor of diversified applications.

The influence of hydrothermal treatments on the structural properties and digestibility of water caltrop starch was investigated. Scanning electron microscopy (SEM) showed some small dents on the surface of starch granules for samples treated with heat moisture treatment (HMT), but not for samples treated with annealing (ANN) which generally showed smoother surfaces. The gelatinization temperature of starch was generally increased by hydrothermal treatments, accompanied by a trend of decreasing breakdown viscosity. These results implied the improvement of thermal and shearing stability, particularly for HMT in comparison to ANN. After being cooked, the native and ANN-modified water caltrop starch granules were essentially burst or destroyed. On the other hand, the margin of starch granules modified by HMT and dual hydrothermal treatments remained clear with some channels inside the starch granules. X-ray diffraction revealed that the crystalline pattern of water caltrop starch changed from the C_A-type to the A-type and the relative crystallinity reduced with increasing moisture levels of HMT. Results of ANN-modified water caltrop starch were mostly similar to those of the native one. Moreover, water caltrop starch modified with HMT20 and dual modification contained a pronouncedly higher resistant starch content. These results suggested that HMT, ANN, and dual modification effectively modified the functional properties of water caltrop starch.

This study focused on the effect of cycled heat-moisture treatment (cHMT) on the in vitro digestibility, rheological, and physicochemical properties of water caltrop starch. The amylose content increased significantly by cHMT, whereas damaged starch content decreased only in the groups with more than two cycles applications. cHMT generally increased the weight-average molecular weight, except for single cycle treatment which showed the reverse result. In thermal properties, the onset temperature (T₀), peak temperature (T_p), and conclusion temperature (T_c) increased, while the enthalpy needed to complete the gelatinization was lowered by cHMT. Water caltrop starch paste showed less shear-thinning behavior with cHMT. Meanwhile, the viscosity and tendency to form strong gel were enfeebled with modification. cHMT significantly changed predicted glycemic index (pGI) value, especially in samples that underwent the most cycles of treatment, which showed the lowest pGI compared to native and other treatment. These results suggested that cHMT water caltrop starch was effectively modified and showed diversified properties.

Heat-moisture treatment (HMT) changed the morphology and the degree of molecular ordering in lotus rhizome (Nelumbo nucifera Gaertn.) starch granules slightly, leading to some detectable cavities or holes near hilum, weaker birefringence and granule agglomeration, accompanied with modified XRD pattern from C- to A-type starch and lower relative crystallinity, particularly for high moisture HMT modification. In contrast, annealing (ANN) showed less impact on granule morphology, XRD pattern and relative crystallinity. All hydrothermal treatment decreased the resistant starch (from about 27.7–35.4% to 2.7–20%), increased the damage starch (from about 0.5–1.6% to 2.4–23.6%) and modified the functional and pasting properties of lotus rhizome starch pronouncedly. An increase in gelatinization temperature but a decrease in transition enthalpy occurred after hydrothermal modification, particularly for hydrothermal modification involved with HMT. HMT-modified starch also showed higher pasting temperature, less pronounced peak viscosity, leading to less significant thixotropic behavior and retrogradation during pasting-gelation process. However, single ANN treatment imparts a higher tendency of retrogradation as compared to native starch. For dual hydrothermally modified samples, the functional properties generally resembled to the behavior of single HMT-modified samples, indicating the pre- or post-ANN modification had less impact on the properties HMT modified lotus rhizome starch.