Solid state cationization reaction of microporous starch with betaine hydrochloride under repeated heating/cooling cycles: Design of a green approach for corn starch modification.

In this research, the cationization process of microporous starch with betaine hydrochloride (BHC) in the presence of H3PO4 (as a catalyst) under heating/cooling cycles was reported for the first time. Granular microporous starch was initially prepared from normal corn starch (NS) through amyloglucosidase treatment. Then, solid state cationization reaction of microporous starch (MS) with betaine hydrochloride (BHC) was performed under repeated dry-heat modification. The cationic microporous starch showed higher substitution degree (0.031) and reaction efficiency (89.1 %) in comparison with cationic starch based on NS (0.021, 60.3 %), which this can be attributed to the increased probability of effective collision between BHC molecules and starch granules after enzymatic treatment. The analysis of cationic starches by FTIR and 13C NMR confirmed the presence of cationic functional groups on starch chains. Further examinations on the modified starches by single and dual treatments were accomplished with respect to morphology, particle size distribution, X-ray powder diffraction (XRD), colour parameters, zeta potential, amylose content, viscosity, solubility, and swelling power. The greenness of the suggested dual treatment (score: 82) in this work was evaluated and compared to a conventional method reported in literature (score: 67) on the preparation of cationic starches.

Ultra-trace determination of cadmium in water and food samples by a thin-film microextraction using a supported liquid membrane combined with smartphone-based colorimetric detection.

A mixture of n-octanol and dithizone was introduced as an effective and novel extraction agent in a thin-film microextraction technique for the pre-concentration of cadmium ions. The extraction agent was immobilized on small pieces of porous polypropylene flat membrane as a supported liquid membrane. The analyte extraction was performed by immersing the modified film in the sample solution, and via a complex formation between the immobilized dithizone on the film and cadmium ions. After the thin-film microextraction process, the colored cadmium-dithizone complex was directly measured by a smartphone colorimetric analysis. Under optimized conditions, the linear dynamic range, the limit of detection, and the limit of quantification were 0.5-300.0, 0.1, and 0.4 µg L-1, respectively. The developed technique was successfully employed to quantify cadmium ions in water and food samples. The high relative recovery values (95.0-103.0%) along with relative standard deviations of less than 2.5% were obtained for the spiked samples.