Impact of Ultrasonic-Assisted Preparation of Water Caltrop Starch–Lipid Complex: Structural and Physicochemical Properties

Abstract

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.