Preparation Of Starch Nanocrystals Research Articles

High-efficiency preparation of starch nanocrystals with small size and high crystallinity by ethanol-acid penetration and dry-heating pretreatment

Ethanol-acid penetration and drying-heating treatment was developed to shorten the preparation time and improve the quality of starch nanocrystals (SNCs). After treatment by optimized parameters, including 40 % ethanol solution, 10.6 mM chloric acid, and heating time of 1.5 h or 2.0 h, the starches exhibited weakened internal structure and relatively complete crystalline structure. Compared with the regular preparation of only acid hydrolysis, the regular final yield (8.5 % after 5 days) was reached in 48 h and 12 h of the starch heated at 1.5 h and 2.0 h, respectively. The micromorphology, molecular weight, and crystalline structure evaluation demonstrated that the collected nanoparticles were indeed SNCs with smaller size and higher relative crystallinity than regular SNCs. Further analysis found that the SNCs had better crystalline lamellae, higher thermal stability, and lower proportion of phosphorus and sulfur atoms than regular SNCs. This provided a potential method for the high-efficiency preparation of SNCs.

Rapid preparation of starch nanocrystals by the mixed acid of sulfuric acid and hydrochloric acid

In this work, waxy maize starch nanocrystals were prepared by mixed acid of sulfuric acid and hydrochloric acid for the first time. Physicochemical properties, crystalline structure, and particle size of starch nanocrystals prepared by mixed acid (HSNC) were measured. The results showed that there was no difference in particle morphology, group structure, and surface elements of HSNC and starch nanocrystals prepared by sulfuric acid (SNC), which was a conventional preparation method. The yield of HSNC was lower than that of SNC. However, the preparation time of HSNC was greatly shortened to 1 h which is only 0.83 % of the time (5 d) to prepare SNC by the sulfuric acid, and HSNC showed higher relative crystallinity and smaller size than those of SNC. In addition, when the ratio of sulfuric acid and hydrochloric acid to provide H ion concentration was 1:1 to hydrolyze starch for >1 h, the crystal pattern of HSNC would be changed to V-typed, while the crystal pattern of SNC was still A-typed. Thus, this work provided efficient method for preparing starch nanocrystals is provided, which can replace sulfuric acid hydrolysis to prepare SNC.

Preparation of Starch Nanocrystals with Antimicrobial Property

The current pandemic brought to our attention the need for continuous research and development on the fight against pathogens. The use of derivatives of starch nanocrystals (SNC) with antimicrobial activities offers a good alternative to conventional antimicrobial agents since they can be sourced from readily available, biodegradable, and biocompatible raw materials. In this study, starch nanocrystals were prepared by acid hydrolysis and oxidized using hydrogen peroxide. The resulting oxidized starch nanocrystals showed inhibitory effect against E. coli. FTIR analysis showed that the antimicrobial activity could be due to the introduction of carbonyl groups in the starch chain. Due to the versatility of starch nanocrystals, other derivatives with improved antimicrobial activity or other tailored properties could also be developed.

Surface-charged starch nanocrystals from glutinous rice: Preparation, crystalline properties and cytotoxicity

The high-amylopectin glutinous rice is used in this study for the preparation of starch nanocrystals (SNCs) with the acid hydrolysis and enzymatic treatment. The fabricated SNC is carried out the surface modifications by phosphorylation and cationization to produce the nanocrystals with the charged surface. Four kinds of SNCs are obtained with the different surface charges involving the varied negative charges, positive charge and no charge. The chemical structures, morphologies and crystalline properties of four SNCs were investigated, together with the effect of surface charges to their cytotoxicity for two cell lines RAW267.4 and CAL27 by the cell proliferation and cell migration assay. The sulfuric acid-hydrolyzed SNC and phosphorylated SNC have more ordered regions and therefore display the higher crystallinities than the enzymatic treated SNC. Four obtained SNCs all exhibited weak cytotoxicity, indicating their good biocompatibility in the potential biomedical application.

Succeeded starch nanocrystals preparation combining heat-moisture treatment with acid hydrolysis.

Heat-moisture treatment (HMT) could be applied to increase the relative crystallinity (RC) of raw waxy maize starch (WMS) and mar the dense surface of starch granules. The optimal HMT conditions including temperature, treatment time, and moisture content were determined by response surface methodology (RSM). When the temperature, treatment time, and moisture content were 99.2 °C, 1.8 h, and 18.2%, respectively, the maximum RC of heat-moisture treated starch (HMTS) could reach to 42.44% and more holes, depressions, and cracks appeared on the surface of HMTS. Afterwards, HMTS was subjected to acid hydrolysis to prepare starch nanocrystals (SNCs). It was confirmed that SNCs could be successfully obtained with a hydrolysis time of 4 days and a yield of 26.7%. The results revealed that this method was more effective than conventional sulfuric acid hydrolysis method with a hydrolysis time of 5 days and a yield of 15.7%.

Conversion of Potato Starch and Peel Waste to High Value Nanocrystals

The present study aimed to convert starch and potato peel waste to nanocrystals. Starch nanocrystals were prepared using two methodologies: direct acid hydrolysis and enzyme pretreatment followed by acid hydrolysis. Direct hydrolysis broke down the starch granules to nanocrystals in 12 days. Enzyme pretreatment with starch hydrolytic enzymes (α-amylase and amyloglucosidase) reduced the time for preparation of starch nanocrystals by 6 days. Starch nanocrystals of optimum size were obtained with both the treatments and the resultant size ranged from 10 to 50 nm. Nanocrystals were disk-like platelets in appearance. Cellulose nanocrystals were derived from cellulosic material in the potato peel. Cellulose was isolated from peel waste with alkali treatment. Further, cellulose nanocrystals from potato peel and cellulose microcrystalline were prepared by acid hydrolysis. Microscopic images revealed that the aqueous suspension of cellulose nanocrystals derived from potato peel were single rod shaped, whereas those derived from cellulose microcrystalline were rod-like nanoparticles, agglomerated in the form of bundles including some of the rods in single units (well separated). The size of potato peel nanocrystals ranged from 40 to 100 nm (length) and cellulose microcrystalline ranged from 4 to 20 nm (diameter) by 110 to 250, given 4 to 20 nm (length), respectively. As starch nanocrystals as well as cellulose nanocrystals are derived from biopolymer, both can be considered safe for humans and the environment. Moreover, the biodegradable nature of these nanocrystals makes them superior over metallic nanoparticles, particularly in the field of nanocomposites.

Preparation of starch nanocrystals through enzymatic pretreatment from waxy potato starch

A comparative experiment about the production of starch nanocrystals (SNCs) with/without glucoamylase enzymatic pretreatment by sulfate acid hydrolysis from waxy potato starch (WPS) was employed in the present study. The research focused on the enhancement of the preparation efficiency while improving the dispersion of SNCs at the same time. The enzymatic pretreatment resulted in the decrease of acid hydrolysis duration. The minimum size and best dispersibility of nanocrystals was obtained after 5 days of hydrolysis. X-ray diffraction confirmed the increase of crystallinity (from 33% to 50.8%) and the polymorphic transitions (B–A) for nanocrystals harvested at day 5. The structure of nanocrystals was characterized by FT-IR, which suggested the presence of sulfate ester on the surface of SNCs. Zeta potential and size distribution revealed the prominent stability and dispersibility of nanocrystals at pH 7.0. SEM and TEM revealed that SNCs had square shapes with particle sizes ranging from 50 to 100 nm.

Starch nanocrystals based hydrogel: Construction, characterizations and transdermal application

Bio-based nanocomposites were prepared using starch nanocrystals obtained by acid hydrolysis of native starches using different acid sources. In recent times, focuses on starch nanocrystals (SNCs) have been increasing in number of research works dedicated to the development of bio-nanocomposites by blending with different biopolymeric matrices. The work mainly deals with the preparation of starch nanocrystals using different native starches by acid hydrolysis using hydrochloric acid and trifluroacetic acid. The as-prepared starch nanocrystals are having high crystallinity and more platelet morphologies, and used as a drug carrying filler material in the hydrogel formulations with the care of different polymer matrices. The condensed work also concentrates on the dispersion of antiviral drug in the hydrogels, which are applied onto biocompatible bio-membrane to be formulating a complete transdermal patch. The acid hydrolysed starch nanocrystals were thoroughly characterized using TEM, SEM, particle size analysis and zeta potential. Their thermal stability and the crystalline properties were also characterized using TG-DSC and XRD respectively. The physiochemical interaction and compatibility between the drug and the SNCs filler in the polymeric hydrogels were evaluated using FT-IR analysis. The formulated hydrogels were subjected to evaluation of in vitro permeation studies using Franz diffusion studies. The in vitro study was indicated substantial guarantee for the fabrication of drug dispersed in polymeric hydrogels using SNCs as filler matrices for a successful transdermal drug delivery.

An attempt to cast light into starch nanocrystals preparation and cross-linking

Potato starch was hydrolyzed with 2.2 or 3.7M hydrochloric acid in order to obtain the nanocrystals which afterwards were chemically cross-linked with sodium hexametaphosphate. The stronger acidity resulted in smaller nanocrystals with mean size of 48nm in a shorter time. X-ray diffraction confirmed the dominant crystalline nature of particles and Fourier transform infrared spectroscopy suggested the presence of lower number of free hydroxyl groups in nanocrystals after cross-linking. Starch nanocrystals showed two distinctive differential scaning colorimetry endotherms at 26 and 125°C, attributed to destruction of nanocrystals lattice and moblizing of each nanocrystal’s structure, respectively. Cross-linking resulted in a tenacious spatial arrangement of nanocrystals, strengthening the crystals lattice against phase transitions induced by heating. Scanning electron microscopy images confirmed the particle size measured for nanocrystals by light scattering. Atomic force microscopy topographic images suggested that starch nanocrystals were originated from small amylopectin blocklets in granular assembly of starch.

Optimization of the batch preparation of starch nanocrystals to reach daily time‐scale

AbstractCurrent environmental concerns have turned starch nanocrystals (SNC) into candidates of growing interest as bio‐nanofillers for nanocomposite applications. However, despite previous drastic optimization, the main drawbacks for the more extensive use of SNC remain (i) the preparation duration (5 days) and (ii) their relatively low yield (15%). Also, the final suspension of SNC actually contains both nanocrystals and microparticles. Thus, previous study optimized the SNC‐containing suspension yield, rather than the SNC yield. As an attempt to (i) further limit preparation time (to 1 day) and (ii) increase the yield of SNC assessed after filtration (as opposed to that of the heterogeneous SNC‐containing suspension), a response surface methodology (RSM) analysis has been undertaken. The modeling of size and sulfate content was not possible. On the contrary, a linear model with first‐order interactions was postulated for SNC mass yields. The model postulated to fit the SNC yield of the filtered suspension (1 µm) was more descriptive and predictive than that of the current poorly filtered suspension. Opposite effects for the same parameters have been evidenced. This confirmed the need to better isolate SNC, not only before use, but also for better modeling and optimization.

Evidence of Micro- and Nanoscaled Particles during Starch Nanocrystals Preparation and Their Isolation

Great work has been done to reduce the batch production time of starch nanocrystals (SNCs) and improve their compatibilization with different matrices. However, only one study was reported on SNC production kinetics and none on size distributions and isolation techniques. This study was designed to assess if nonsolubilized particles in the hydrolyzed starch suspension reflect the actual amount of SNC. It was observed that SNCs are produced from a very early stage. It suggests, for the first time, that (i) nanocrystals are mixed together with other microparticles and (ii) some nanocrystals might turn to sugar by the end of the batch production process explaining the low yields. An isolation process has been proposed, but limits of differential centrifugations as washing step and isolation technique were also evidenced. This study clearly shows the need for a continuous production and extraction process of SNC.