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Recent research has increasingly focused on the health benefits of dietary fibre (DF), including improved digestion, blood glucose and cholesterol regulation, satiety, and prebiotic effects, which depend on the specific DF type. Traditional gravimetric methods (e.g. Van Soest and AOAC) quantify DF fractions but lack molecular or monosaccharide detail. Advanced chromatographic methods offer more insights but require extensive sample preparation. To address this limitation, the study developed a method using proton Nuclear Magnetic Resonance ( 1 H NMR) spectroscopy to directly analyse DF hydrolysed fractions (mainly pectin, hemicellulose, and cellulose) without the need for derivatisation or neutralisation. It provides detailed structural insights, including the monosaccharide composition, carbohydrate modifications (methylation and acetylation), and the degradation products. The method was validated and then applied to hydrolysed DF fractions obtained from the AOAC process. 1 H NMR shows a comparable monosaccharide distribution to GC-MS, but yields higher recoveries, particularly for uronic acids. In addition, it offers faster sample preparation and acquisition, making it a powerful tool for comprehensive DF analysis. Dietary fibre (DF) analysis is crucial for understanding its health benefits, yet traditional methods lack molecular detail. Here, the authors develop a 1H NMR spectroscopy method to directly analyze hydrolysed DF fractions with high recovery and fast preparation while revealing detailed structural information including monosaccharide composition, carbohydrate modifications and the degradation products.

Hulled wheats (einkorn, emmer, and spelt) and old genotypes of bread wheat ( T. aestivum L. ssp. aestivum ) have been attracting attention in plant breeding and in the food industry for food diversification and value addition purposes. This study investigated the agronomic behavior, the grain quality, the contaminants, the bioactive compounds (e.g., alkylresorcinols and phenolic acids), and the antioxidant capacity (FRAP and DPPH) of modern genotypes of hulled wheat (einkorn, emmer, and spelt), as well as old Italian bread wheat genotypes, under standard cropping conditions. These genotypes were compared with modern bread wheat genotypes used as commercial references in four location-by-year experiments in Northwest Italy. The treatments were assigned to experimental units using a completely randomized block design and three replications. The modern bread wheat genotypes displayed better agronomic performance, while the old bread wheat genotypes had higher protein contents, but were characterized by higher dough weakening, even with increasing levels of nitrogen fertilization. The old genotypes did not offer advantages in terms of toxic celiac disease epitopes, but exhibited an overall reduced susceptibility to mycotoxin accumulation, although a large variability was observed within the modern hulled and bread wheat genotypes. The bioactive compound content and the antioxidant capacity were closely related to the growing conditions. Majority of the differences among the genotypes emerged from the soluble fraction of phenolic acids, with a slightly higher content in the old bread wheat genotypes than in the modern ones and a different profile for the hulled wheats. On the other hand, the alkylresorcinol content was higher in the modern genotypes than in the old ones and was closely related to kernel size. Overall, the results highlighted considerable differences among genotypes and a broader variability in the modern genotypes than the old ones for many of the studied traits. Substantial agronomic and qualitative differences were observed within the hulled wheats, thus suggesting opportunities for genetic selection and the development of improved hulled or bread wheat genotypes.

Recent research has increasingly focused on the health benefits of dietary fibre (DF), including improved digestion, blood glucose and cholesterol regulation, satiety, and prebiotic effects, which depend on the specific DF type. Traditional gravimetric methods (e.g. Van Soest and AOAC) quantify DF fractions but lack molecular or monosaccharide detail. Advanced chromatographic methods offer more insights but require extensive sample preparation. To address this limitation, the study developed a method using proton Nuclear Magnetic Resonance ( H NMR) spectroscopy to directly analyse DF hydrolysed fractions (mainly pectin, hemicellulose, and cellulose) without the need for derivatisation or neutralisation. It provides detailed structural insights, including the monosaccharide composition, carbohydrate modifications (methylation and acetylation), and the degradation products. The method was validated and then applied to hydrolysed DF fractions obtained from the AOAC process. H NMR shows a comparable monosaccharide distribution to GC-MS, but yields higher recoveries, particularly for uronic acids. In addition, it offers faster sample preparation and acquisition, making it a powerful tool for comprehensive DF analysis.

In a context where the commercial and nutritional interest in insect chitin is always increasing, an accurate and precise method to quantify this biopolymer, especially in food/feed, is required. In addition, quantification of insect crude protein through nitrogen determination is normally overestimated due to the presence of chitin. In this work, for the first time, an RP-UPLC-ESI/MS method for the simultaneous quantification in insects of chitin, as glucosamine (GlcN), and protein, as total amino acids, is presented. The method is based on acid hydrolysis and derivatization of amino acids and GlcN with the AccQ Tag reagent. Method was optimized and validated in terms of linearity, LOD and LOQ, intraday and inter-day repeatability, and accuracy. A hydrolysed commercial chitin was selected as reference standard for calibration. The instrumental LOD and LOQ correspond respectively to a concentration of 0.00068 mM and 0.00204 mM. The intraday precision satisfied the Horwitz ratio. Data from inter-day precision showed the necessity to perform the analysis within 1 week utilizing standard calibration solutions freshly prepared. A matrix effect was observed, which suggested the necessity to use an internal calibration curve or to work in a particular concentration range of GlcN. The chitin and protein content in black soldier fly ( Hermetia illucens ) and lesser mealworm ( Alphitobius diaperinus ) were found in agreement with results obtained by independent methods. The optimized method was also tested on two different commercial food supplements, suggesting its applicability on a wide range of matrices. This newly developed method proved to be simple, more accurate, and faster if compared to methods which separately analyse chitin and protein content.