Acid Hydrolysis Research Articles

Controlled reaction dynamics of cellulose: Revealing the dual morphology nanocrystals

Cellulose nanocrystals exhibit diverse morphology with embedded crystallinity derived from the ordered crystalline regimes of cellulose fibers. Acid hydrolysis parameters controls the morphology of nanocrystals and is the primary efficient route for the synthesis of cellulose nanocrystals. In this study, we explored the impact of temperature on the morphology engineering of cellulose nanocrystals derived from banana pseudostem by oxalic acid hydrolysis, an underexplored method. Confirmation of successful cellulose extraction was achieved through fibrous morphology observed in FESEM and TEM analyses. X-ray diffraction and Raman spectroscopy affirmed the presence of type II cellulose. Notably, for the first time, we report the derivation of toroidal and spherulitic sheet-like morphologies in cellulose nanocrystals synthesized by hydrothermal method from banana psuedostem. Our investigation revealed that cellulose hydrolysis at 120 °C yields nanocrystals characterized by toroidal and spherulitic sheet-like morphologies with excellent crystallinity, as confirmed by FESEM and TEM analyses, with average thicknesses of 13.70 nm and 18.05 nm, respectively. Interestingly, elevating the hydrolysis temperature to 180 °C led to the collapse of these structures into carbon dots, exhibiting notable cyan emission.

Valorization of Eichhornia crassipes for the production of cellulose nanocrystals further investigation of plethoric biobased resource

Chemical processing is among the significant keys to tackle agro-residues utilization field, aiming to obtain value-added materials. Extraction of cellulose nanocrystals (CNCs) is an emerging route to valorize lignocellulosic wastes into high value particles. In this investigation, effect of acidic hydrolysis duration was monitored on size and morphology of obtained crystals; namely: CNCs from Nile roses fibers (NRFs) (Eichhornia crassipes). Different acidic hydrolysis duration range or different characterization techniques set this article apart from relevant literature, including our group research articles. The grinded NRFs were firstly subjected to alkaline and bleaching pretreatments, then acid hydrolysis process was carried out with varied durations ranging from 5 to 30 min. Microcrystalline cellulose (MCC) was used as reference for comparison with NRFs based samples. The extracted CNCs samples were investigated using various techniques such as scanning electron microscopy (SEM), Atomic force microscopy (AFM), Raman spectroscopy, and thermogravimetric (TGA) analysis. The figures gotten from SEM and AFM depicted that NRFs based CNCs appeared as fibril-like shapes, with reduced average size when the NRFs underwent pulping and bleaching processes. This was indicated that the elimination of hemicellulose and lignin components got achieved successfully. This outcome was proven by chemical composition measurements and TGA/DTG curves. On the other hand, AFM-3D images indicated that CNCs topology and surface roughness were mostly affected by increasing hydrolysis durations, besides smooth and homogeneous surfaces were noticed. Moreover, Raman spectra demonstrated that the particle size and crystallinity degree of NRFs based CNCs can be affected by acidic hydrolysis durations and optimum extraction time was found to be 10 min. Thermal stability of extracted CNCs-NRFs and CNCs-MCC was measured by TGA/DTG and the kinetic models were suggested to identify the kinetic parameters of the thermal decomposition of CNCs for each acid hydrolysis duration. Increasing hydrolysis duration promoted thermal stability, particularly for NRFs based CNCs. Results showcased in this article add new perspective to Nile rose nanocellulose and pave down the way to fabricate NRFs based humidity nano-sensors.

Identification and Characterization of Rotigotine Degradation Products by HPLC Coupled DAD and CAD Detectors and HRMS Through Q-Orbitrap and Electrospray Ionization

Rotigotine (RTG) is a dopamine agonist used in the treatment of Parkinson's disease. As it is susceptible to oxidation, stability studies must be carefully designed for the identification and characterization of all possible degradation products. Here, RTG degradation was evaluated according to the International Conference on Harmonization guidelines under various stress conditions, including acidic and basic hydrolysis, oxidative, metallic, photolytic, and thermal conditions. Additionally, more severe stress conditions were applied to induce RTG degradation. Significant degradation was only observed under oxidative and photolytic conditions. The samples were analyzed by high performance liquid chromatography coupled to photodiode array detectors, charged aerosol, and high-resolution mass spectrometry. Chromatographic analyses revealed the presence of eight substances related to RTG, four of which were already described and were qualified impurities (impurities B, C, K and E) and four new degradation products (DP-1 – DP-4), whose structures were characterized by high-resolution mass spectrometry through Q-Orbitrap and electrospray ionization. In the stress testing of the active pharmaceutical ingredient in solid form, significant RTG degradation was observed in the presence of the oxidative matrix. The results corroborate the literature that confirm the high susceptibility of RTG to oxidation and the importance of using different detectors to detect degradation products in forced degradation studies.

Plasma fatty acid esters of hydroxy fatty acids and surrogate fatty acid esters of hydroxy fatty acids hydrolysis activity in children with or without obesity and in adults with or without coronary artery disease.

Fatty acid esters of hydroxy fatty acids (FAHFA) are a class of bioactive lipids with anti-inflammatory, antidiabetic and cardioprotective properties. FAHFA hydrolysis into its fatty acid (FA) and hydroxy fatty acid (HFA) constituents can affect the bioavailability of FAHFA and its subsequent biological effects. We aimed to investigate FAHFA levels and FAHFA hydrolysis activity in children with or without obesity, and in adults with or without coronary artery disease (CAD). Our study cohort included 20 children without obesity, 40 children with obesity, 10 adults without CAD and 28 adults with CAD. We quantitated plasma levels of four families of FAHFA [palmitic acid hydroxy stearic acid (PAHSA), palmitoleic acid hydroxy stearic acid (POHSA), oleic acid hydroxy stearic acid (OAHSA), stearic acid hydroxy stearic acid] and their corresponding FA and HFA constituents using liquid chromatography-tandem mass spectrometry analysis. Surrogate FAHFA hydrolysis activity was estimated as the FA/FAHFA or HFA/FAHFA ratio. Children with obesity had lower plasma PAHSA (p = .001), OAHSA (p = .006) and total FAHFA (p = .011) levels, and higher surrogate FAHFA hydrolysis activity represented by PA/PAHSA (p = .040) and HSA/OAHSA (p = .025) compared with children without obesity. Adults with CAD and a history of myocardial infarction (MI) had lower POHSA levels (p = .026) and higher PA/PAHSA (p = .041), POA/POHSA (p = .003) and HSA/POHSA (p = .038) compared with those without MI. Altered FAHFA metabolism is associated with obesity and MI, and inhibition of FAHFA hydrolysis should be studied further as a possible therapeutic strategy in obesity and MI.

Determination of chloropropanol esters and glycidyl esters in nutritional foods by gas chromatography–tandem mass spectrometry based on acid hydrolysis and solid-phase extraction

This study presents a method based on acid transesterification and the purification by solid-phase extraction (SPE) coupled with gas chromatography–tandem mass spectrometry for quantifying 3- and 2-monochloropropanediol esters (3-MCPDE, 2-MCPDE) and glycidyl esters (GE) in nutritional foods. The fat was extracted by liquid–liquid extraction with petroleum ether and diethyl ether after the sample was hydrolysed with ammonia. Then the extract was purified by a SPE cartridge filled with the aminopropyl sorbents. It was demonstrated that the optimal elution volume for 3-MCPDE, 2-MCPDE and GE greatly depended on the sample matrix and varied from 6 to 12 mL for four different kinds of food matrices. All three analytes in the sample solution could be fully collected in the first 10–12 mL of eluate. By this way, monoacylglycerols commonly present in the samples were fully removed. Therefore, the overestimation of GE quantification was effectively eliminated. The modified analytical procedure was fully validated in a single laboratory and has been recommended as a Chinese Food Safety National Standard. In addition, two derivatisation agents, heptafluorobutyrylimidazole and phenylboronic acid, were proved to be equivalent in method accuracy and precision for the quantification of three analytes.

Crystalline Hepatopathy Associated With Bietti Crystalline Dystrophy: A Striking Manifestation of Disordered Fatty Acid Metabolism.

Bietti crystalline dystrophy (BCD) is a rare heritable retinal disease characterized by crystal deposition primarily in the retina. It is associated with atrophy of the retinal pigment epithelium (RPE) and is caused by variants in CYP4V2 , which encodes a cytochrome P450 hemethiolate protein superfamily member. CYP4V2 is involved in the selective hydrolysis of saturated medium chain fatty acids, and patients with BCD demonstrate abnormalities in fatty acid metabolism, including abnormal lipid profiles and the accumulation of the pathogenic crystals within the RPE, which leads to the visual pathologies characteristic of BCD. However, the precise identity of the crystals is currently unknown, and BCD has no established extraocular manifestations. Here, we report granulomatous hepatitis associated with abundant diffuse crystalline clefts in the hepatic parenchyma in 3 patients with retinal dystrophy and dyslipidemia: 2 with pathogenic CYP4V2 variants and 1 patient with clinical ophthalmologic findings suggestive of BCD but without available genetic testing. The unique and striking histologic features unifying the liver biopsies in all 3 patients strongly support a process related to abnormal fatty acid metabolism underlying the genetic disease of BCD, expanding the spectrum of BCD and shedding light on the importance of CYP4V2 in systemic fatty acid metabolism.

Chromatographic analysis of the amino acid composition of gallstones

Gallstone disease (cholelithiasis) is a multifactorial disease characterised by the formation of gallstones. Studying the composition of gallstones is necessary to understand the mechanism of their formation and to solve many practical issues. At present, it is not clear which protein component is involved in the formation of gallstones and how it is related to their components. The study showed the possibility of qualitative and quantitative determination of amino acids in the composition of gallstones of men and women of different ages using a GC-17A gas chromatograph (Shimadzu). Analysis of the amino acid composition of gallstones includes acid hydrolysis of samples with 6M HCl at 105C° for 12 hours, subsequent purification, obtaining derivatives of isolated amino acids, and their determination by gas chromatography. This technique enables the determination of D- and L-forms of amino acids. Statistical processing of the obtained data was carried out using Statistica 6.0. The study revealed that cholesterol gallstones belonging to women up to 50 years of age have the lowest amino acid content. The amino acid composition of cholesterol gallstones is dominated by glycine and L-forms of serine, alanine, and glutamic acid. Cholesterol gallstones with mineral content are typical for elderly women (over 60 years) and middle-aged men (from 37 years), and have higher amino acid content than cholesterol gallstones. Glycine and the L-forms of leucine, glutamic acid, and asparagic acid are prevalent in these types of gallstones. The highest amino acid content was recorded in pigment gallstones of both men and women over 55 years of age. The amino acid composition of pigment gallstones is dominated by glycine and L-forms of glutamic acid, asparagic acid, leucine, and alanine. In cholesterol gallstones, no D-amino acids were found. In cholesterol gallstones with mineral content and pigmented gallstones, D-aspartic acid was detected. The obtained results allow us to recommend the method of gas chromatography for studying the amino acid composition of gallstones.

Determination of Luteolin and Apigenin in Herbal Teas by Online In-Tube Solid-Phase Microextraction Coupled with LC-MS/MS.

Herbal teas have attracted attention as functional beverages containing luteolin and apigenin, which exhibit antioxidant and anti-inflammatory effects. The objective of this study was to develop a sensitive online automated method to determine these flavones' contents in herbal teas using in-tube solid-phase microextraction (IT-SPME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). These compounds were extracted and concentrated by IT-SPME using a Supel Q PLOT capillary column and then separated and detected within 6 min using a CAPCELL PAK C18 MG III analytical column and a negative electrospray ionization-mode multiple-reaction monitoring system by LC-MS/MS. The detection limits (S/N = 3) for luteolin and apigenin were 0.4 and 0.8 pg mL-1, respectively, and the calibration curves were linear in the range of 2-2000 pg mL-1 with correlation coefficients above 0.9995, and intra-day and inter-day precisions with relative standard deviations below 2.9 and 3.6% (n = 6), respectively. The luteolin and apigenin in herbal tea were quantified using IT-SPME/LC-MS/MS following the acid hydrolysis of their glycosides. Among the 10 herbal teas tested, luteolin was detected in peppermint and sage at concentrations of 375 and 99 µg mL-1, respectively, while apigenin was detected in German chamomile at 110 µg mL-1, which were higher than in the other herbal teas. The method is expected to be a useful method for evaluating the efficacy of luteolin and apigenin in herbal teas as functional beverages.

Site-directed mutagenesis reveals the interplay between stability, structure, and enzymatic activity in RidA from Capra hircus.

Reactive intermediate deaminase A (RidA) is a highly conserved enzyme that catalyzes the hydrolysis of 2-imino acids to the corresponding 2-keto acids and ammonia. RidA thus prevents the accumulation of such potentially harmful compounds in the cell, as exemplified by its role in the degradation of 2-aminoacrylate, formed during the metabolism of cysteine and serine, catalyzing the conversion of its stable 2-iminopyruvate tautomer into pyruvate. Capra hircus (goat) RidA (ChRidA) was the first mammalian RidA to be isolated and described. It has the typical homotrimeric fold of the Rid superfamily, characterized by remarkably high thermal stability, with three active sites located at the interface between adjacent subunits. ChRidA exhibits a broad substrate specificity with a preference for 2-iminopyruvate and other 2-imino acids derived from amino acids with non-polar non-bulky side chains. Here we report a biophysical and biochemical characterization of eight ChRidA variants obtained by site-directed mutagenesis to gain insight into the role of specific residues in protein stability and catalytic activity. Each mutant was produced in Escherichia coli cells, purified and characterized in terms of quaternary structure, thermal stability and substrate specificity. The results are rationalized in the context of the high-resolution structures obtained by x-ray crystallography.

Biowaste Valorization of Palm Tree Phoenix dactylifera L. for Nanocellulose Production.

The desire to reduce reliance on oil resources arises from the concerns about carbon footprint and nonrenewability. Conversely, the global presence of over 100 million palm trees poses a significant challenge due to the substantial amount of biowaste generated annually. Additionally, the use of nanocellulose (NC) as a cost-effective material is steadily gaining recognition for its growing adaptability over time. The main goal of this study is to biosynthesized NC from Iraqi date palm Phoenix dactylifera leaves waste with low-concentration acid-alkali treatment. The date palm leaves waste yields 20 g of NC from 100 g of leaves before acid hydrolysis treatment. The chemical components of biosynthesized NC were 47.90%, 26.78%, and 24.67% for α-cellulose, hemicellulose, and lignin, respectively. In order to study their properties, NC from raw date palm leaves was studied by microscopic techniques such as scanning electron microscopy (SEM), energy dispersive X-ray (EDX) spectroscopy, and atomic force microscope (AFM). SEM results revealed rod-like structured NC as well as combined long-fine fibrous structures rather than compacted bundles with sizes ranging between 31 and 74 nm. With EDX, all spectra exhibit the peaks of carbon and oxygen as the main elements with 63.8% and 10.44%, respectively, in their compositions, which relate to the typical composition of cellulose. The 3D image of AFM NC with a tapping mode presented a highly uniform distribution of NC with a size of ∼15 nm. The statistical roughness analysis shows that the obtained roughness average is 7.20 nm with the root-mean-square roughness value of 21.56 nm, which corresponded relatively with the micrographs of SEM. The results of this study demonstrate the promise of using date palm waste as raw material to produce NC as green nanocomposite from biodegradable nanomaterials for water purification and sustained drug delivery for biomedical applications. In this regard and because of the insufficient reports about the extraction of NC from palm tree leaves waste, the objective of this study was designed to fabricate NC biologically from fibers sourced from the waste of Iraqi date palm P. dactylifera leaves that left in agricultural lands or burned, which can be an ecological and health problem as a bionanocomposites in the medical and industrial field and as alternative resources of wood materials.

Efficient acid hydrolysis for compound-specific δ15N analysis of amino acids for determining trophic positions

Compound-specific isotope analysis of nitrogen in amino acids (CSIA-AA, δ15NAA) has gained increasing popularity for elucidating energy flow within food chains and determining the trophic positions of various organisms. However, there is a lack of research on the impact of hydrolysis conditions, such as HCl concentration and hydrolysis time, on δ15NAA analysis in biota samples. In this study, we investigated two HCl concentrations (6 M and 12 M) and four hydrolysis times (2 h, 6 h, 12 h, and 24 h) for hydrolyzing and derivatizing AAs in reference materials (Tuna) and biological samples of little egret (n = 4), night heron (n = 4), sharpbelly (n = 4) and Algae (n = 1) using the n-pivaloyl-iso-propyl (NPIP) ester approach. A Dowex cation exchange resin was used to purify amino acids before derivatization. We then determined δ15NAA values using gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS). The results revealed no significant differences (p > 0.05) in δ15NAA values among samples treated with different HCl concentrations or hydrolysis times, particularly for δ15NGlx (range: 21.0–23.5‰) and δ15NPhe (range: 4.3–5.4‰) in Tuna (12 M). Trophic positions (TPs) calculated based on δ15NAA at 2 h (little egret: 2.9 ± 0.1, night heron: 2.8 ± 0.1, sharpbelly: 2.0 ± 0.1 and Algae: 1.3 ± 0.2) were consistent with those at 24 h (3.1 ± 0.1, 2.8 ± 0.1, 2.2 ± 0.1 and 1.1 ± 0.1, respectively), suggesting that a 2-h hydrolysis time and a 6 M HCl concentration are efficient pretreatment conditions for determining δ15NAA and estimating TP. Compared to the currently used hydrolysis conditions (24 h, 6 M), the proposed conditions (2 h, 6 M) accelerated the δ15NAA assay, making it faster, more convenient, and more efficient. Further research is needed to simplify the operational processes and reduce the time costs, enabling more efficient applications of CSIA-AA.

Campylobacter jejuni and casein hydrolysate addition: Impact on poultry in vitro cecal microbiota and metabolome.

This study investigates the impact of casein hydrolysates on the poultry ceca inoculated with Campylobacter focusing on microbial molecular preferences for different protein sources in the presence of Campylobacter jejuni. Three casein sources (intact casein (IN), casein enzyme hydrolysate (EH), and casein acid hydrolysate (AH)) were introduced to cecal contents in combination with inoculated C. jejuni in an in vitro model system incubated for 48 h at 42°C under microaerophilic conditions. Samples were collected at 0, 24, and 48 h. Genomic DNA was extracted and amplified using custom dual-indexed primers, followed by sequencing on an Illumina MiSeq platform. The obtained sequencing data were then analyzed via QIIME2-2021.11. Metabolite extracts were analyzed with ultra-high-performance liquid orbitrap chromatography-mass spectrometry (UHPLC-MS). Statistical analysis of metabolites was conducted using MetaboAnalyst 5.0, while functional analysis was performed using Mummichog 2.0 with a significance threshold set at P < 0.00001. DNA sequencing and metabolomic analyses revealed that C. jejuni was most abundant in the EH group. Microbial diversity and richness improved in casein supplemented groups, with core microbial differences observed, compared to non-supplemented groups. Vitamin B-associated metabolites significantly increased in the supplemented groups, displaying distinct patterns in vitamin B6 and B9 metabolism between EH and AH groups (P < 0.05). Faecalibacterium and Phascolarctobacterium were associated with AH and EH groups, respectively. These findings suggest microbial interactions in the presence of C. jejuni and casein supplementation are influenced by microbial community preferences for casein hydrolysates impacting B vitamin production and shaping competitive dynamics within the cecal microbial community. These findings underscore the potential of nutritional interventions to modulate the poultry GIT microbiota for improved health outcomes.

Characteristics of infant formula consumed in the first months of life and allergy in the EDEN mother-child cohort.

The evidence regarding the association between infant formula (IF) composition and the prevention of allergy and respiratory diseases remains sparse and inconclusive. This study aimed to evaluate whether some IF characteristics were associated with the risk of allergy or respiratory diseases in childhood. Among1243 formula-fed children from the EDEN mother-child cohort, IF characteristics concerning long-chain polyunsaturated fatty acids (LCPUFAs) enrichment, prebiotic/probiotic enrichment, and hydrolysis of proteins were identified from the ingredients list. Eczema, wheezing, food allergy, asthma, and allergic rhinitis up to age 8 years were prospectively collected and summarized into four allergic and respiratory multimorbidity clusters. Associations between 4-month IF characteristics and risk of allergy or respiratory diseases were tested using logistic regressions adjusted on main confounders. The consumption of LCPUFA-enriched formula was not linked to allergic and respiratory multimorbidity clusters, but to a lower risk of any allergy, eczema, and wheezing. Probiotic-enriched formula consumption was associated with a lower risk of belonging to the 'Allergy without asthma' cluster (odds ratio [OR][95% confidence interval,CI] = 0.63 [0.40-0.99]), and consumption of a formula enriched in Bifidobacterium lactis was associated with a lower risk of any allergy (OR[95% CI] = 0.59 [0.41-0.85]). Partially hydrolysed formula (pHF) consumption was associated with a higher risk of belonging to the 'Allergy without asthma' cluster (OR[95%CI] = 2.73 [1.65-4.51]). This study confirms the positive association between pHFconsumption and the risk of allergy found in previous observational studies and suggests that consumption of LCPUFA-enriched or probiotic-enriched formula was associated with a lower risk of allergy.

Physicochemical Properties of Cellulose Nanocrystals Extracted from Postconsumer Polyester/Cotton-Blended Fabrics and Their Effects on PVA Composite Films.

The utilisation of cotton waste as precursors in the synthesis of nanocrystalline cellulose has gained significant attention. This approach suggests a sustainable solution to address the growing concern of textile waste accumulation while simultaneously producing a valuable material. The main aim of this study is to examine the properties of cellulose nanocrystals (CNCs) obtained from postconsumer polyester-cotton waste and assess the effect of different fabric structures on the extraction and these properties. To acquire nanocellulose, a thorough decolourisation pretreatment process was utilised, which involved the treatment of polyester-cotton waste with sodium dithionite and hydrogen peroxide. Consequently, the postconsumer material was then treated with an acid hydrolysis method employing a 64% (v/v) sulphuric acid solution at 50 °C for 75 min, resulting in the formation of CNCs with average yield percentages ranging from 38.1% to 69.9%. Separation of the acid from the CNC was facilitated by a centrifugation process followed by dialysis against deionised water. Uniform dispersion was then achieved using ultrasonication. A variety of analytical techniques were employed to investigate the morphological, chemical, thermal, and physical properties of the isolated CNCs. Among these techniques, attenuated total reflection-Fourier-transform infrared spectroscopy (ATR-FTIR), energy-filtered transmission electron microscopy (EF-TEM), thermogravimetric analysis (TGA), and X-ray diffraction (XRD) were utilised to analyse the CNCs. The findings indicated that the separated CNCs exhibited a rod-shaped morphology, measuring between 78 and 358 nm in length and 5 and 16 nm in diameter, and also exhibited high crystallinity (75-89%) and good thermal stability. The extracted CNCs were mixed with polyvinyl alcohol (PVA) and glycerol to assess their reinforcing effect on plastic films. The prepared composite film exhibited improved mechanical properties and thermal stability. Incorporating CNCs led to a 31.9% increase in the tensile strength and a 42.33% rise in the modulus of elasticity. The results from this research proved that CNCs can be extracted from postconsumer mixed fabrics as a potential solution to effectively address the mounting concerns surrounding waste management in the textile industry and also provide avenues for enhancing the qualities of eco-friendly composite films.

Development of a protocol for fractionating and characterising fibres from lignocellulosic food waste

This study aims to explore an advanced protocol for characterising dietary fibre (DF) fractions to meet the growing demand for accurate and reliable data. Although current enzymatic-gravimetric approaches, e.g., AOAC and Van Soest analysis, provide information about soluble and insoluble DF quantification, they present limitations related to the lack of fractions characterisation. To overcome these limitations, the proposed protocol integrates the official AOAC 991.43 method with the sequential fibre fractionation by exploiting the different resistance of the fibre fractions to acid hydrolysis treatments (TFA and H2SO4), utilising hazelnut shells as a case-study. Each hydrolysed fraction was quantified and characterised through GC–MS analysis of monosaccharides. The data obtained for hemicellulose, cellulose, and lignin fractions were then discussed and compared with the Van Soest method. This approach yields a comprehensive procedure applicable to different food and nutraceutical products, emphasising the importance of DF characterisation for a deeper understanding of their bio-functional properties.

Cellulose nanocrystals isolated from sugarcane bagasse using the formic/peroxyformic acid process: Structural, chemical, and thermal properties

Sugarcane bagasse (SCB) is a renewable biomass source for cellulose extraction. In the pretreatment, SCB is processed to break down the cellulose-lignin-hemicellulose matrix and isolate components. This work proposes a formic/peroxyformic acid process for extracting cellulose nanocrystals (CNCs) from SCB. Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and solid-state 13C nuclear magnetic resonance (ss- 13C NMR) were employed to evidence the removal of wax, hemicellulose, and lignin from the raw SCB. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA) were used for analyzing crystallinity, morphology, and thermal properties. SEM results showed that after lignin removal, the size of purified cellulose fibrils decreased significantly, and the structure of cellulose microfibers became smoother and more apparent. After acid hydrolysis of bleached cellulose microfibers, XRD analysis showed CNCs had the highest crystallinity (70.8 %). In TEM images, rod-like structures of CNCs were measured to be 23 ± 2.7 nm wide and 610 ± 18 nm long. The eco-friendly formic/peroxyformic acid procedure with a chlorine-free bleaching stage produced a white, cellulose-rich solid powder of CNCs.

Three New Ionone Glycosides from Rhododendron capitatum Maxim.

Six ionone glycosides (1-3 and 5-7), including three new ones, named capitsesqsides A-C (1-3), together with an eudesmane sesquiterpenoid glycoside (4) and three known triterpenoid saponins (8-10) were isolated from Rhododendron capitatum. The structures of these compounds were determined by extensive spectroscopic techniques (MS, UV, 1D-NMR, and 2D-NMR) and comparison with data reported in the literature. The absolute configurations were determined by comparison of the experimental and theoretically calculated ECD curves and LC-MS analyses after acid hydrolysis and derivatization. The anti-inflammatory activities of these compounds were evaluated in the LPS-induced RAW264.7 cells. Molecular docking demonstrated that 2 has a favorable affinity for NLRP3 and iNOS.

Molecular Basis of the Granular Characteristics of Small-Granule Starch: A Comparative Study.

Small-granule starches (SGSs) have technological advantages over starches of conventional sizes for many applications. The study compared the granular characteristics of three SGSs (from amaranth, quinoa, and taro) with those of maize and potato starches and revealed their molecular basis. The results indicated that the supramolecular architecture of starch granules was not necessarily correlated with granule size. Acid hydrolysis of amaranth and quinoa starches was fast due to not only their small granule sizes but also the defects in the supramolecular structure, to which short external and internal chain lengths of amaranth and quinoa amylopectins contributed. By comparison, the granular architecture of taro starch granules was more stable partly due to the longer external chain length of taro amylopectin. Comparison of the molecular composition of branched subunits (released by using α-amylase of Bacillus amyloliquefaciens) in amylopectins and that in lintnerized starches suggested a significant heterogeneous degradation of amaranth and quinoa starches at supramolecular levels.

The study of galactomannans with different molecular weights and their ability to form microparticles suitable for pulmonary delivery

The influence of locust bean gum (LBG) galactomannans (GMs) molecular weight (Mw) to assemble microparticulate systems was evaluated, and carriers for deep lung delivery were developed. A commercial batch of LBG with a mannose/galactose (M/G) ratio of 2.4 (batch 1) was used to study the influence of different microwave partial acid hydrolysis conditions on carbohydrate composition, glycosidic linkages, and aqueous solutions viscosity. The microwave treatment did not affect the composition, presenting 4-Man (36–42 %), 4,6-Man (27–35 %), and T-Gal (24–25 %) as the main glycosidic linkages. Depolymerization led to a viscosity reduction (≤0.005 Pa·s) with no major impact on polysaccharide debranching. The structural composition of the LBG galactomannans were further elucidated with sequence-specific proteins using carbohydrate microarray technologies. A second batch of LBG (M/G 3.3) was used to study the impact of GMs with different Mw on microparticle assembling, characteristics, and insulin release kinetics. The low-Mw GMs microparticles led to a faster release (20 min) than the higher-Mw (40 min) ones, impacting the release kinetics. All microparticles exhibited a safety profile to cells of the respiratory tract. However, only the higher-Mw GMs allowed the assembly of microparticles with sizes suitable for this type of administration.

Mechanistic insights into the plant biostimulant activity of a novel formulation based on rice husk nanobiosilica embedded in a seed coating alginate film.

Seed coating ensures the targeted delivery of various compounds from the early stages of development to increase crop quality and yield. Silicon and alginate are known to have plant biostimulant effects. Rice husk (RH) is a significant source of biosilica. In this study, we coated mung bean seeds with an alginate-glycerol-sorbitol (AGS) film with embedded biogenic nanosilica (SiNPs) from RH, with significant plant biostimulant activity. After dilute acid hydrolysis of ground RH in a temperature-controlled hermetic reactor, the resulting RH substrate was neutralized and calcined at 650°C. The structural and compositional characteristics of the native RH, the intermediate substrate, and SiNPs, as well as the release of soluble Si from SiNPs, were investigated. The film for seed coating was optimized using a mixture design with three factors. The physiological properties were assessed in the absence and the presence of 50 mM salt added from the beginning. The main parameters investigated were the growth, development, metabolic activity, reactive oxygen species (ROS) metabolism, and the Si content of seedlings. The results evidenced a homogeneous AGS film formation embedding 50-nm amorphous SiNPs having Si-O-Si and Si-OH bonds, 0.347 cm3/g CPV (cumulative pore volume), and 240 m2/g SSA (specific surface area). The coating film has remarkable properties of enhancing the metabolic, proton pump activities and ROS scavenging of mung seedlings under salt stress. The study shows that the RH biogenic SiNPs can be efficiently applied, together with the optimized, beneficial alginate-based film, as plant biostimulants that alleviate saline stress from the first stages of plant development.