This study focuses on the analysis of polysaccharide residues from the cell walls of fruits and vegetables: tomato, potato, pumpkin, carrot and celery root. An alcohol-insoluble residue was prepared from plant material by extraction using the hot ethyl alcohol method and then cell wall fractions soluble in trans-1,2-diaminocyclohexane-N,N,N′,N′-tetraacetate, sodium carbonate and alkaline solution were sequentially extracted. Infrared spectroscopy combined with Fourier transform (FT-IR) was used to evaluate differences among cell wall residues and among species after each step of sequential extraction of pectins and hemicelluloses. Additionally, pectic substances were identified using an Automated Wet Chemistry Analyser. Principal component analysis (PCA) was applied to FT-IR spectra in two regions: 1,800–1,200 cm−1 and 1,200–800 cm−1 in order to distinguish different components of cell wall polysaccharides. This method also allowed us the possibility of highlighting the most important wavenumbers for each type of polysaccharide: 1,740, 1,610 and 1,240 cm−1 denoting pectins or 1,370 and 1,317 cm−1 denoting hemicelluloses and cellulose, respectively.

Abstract:A new fractionation process was developed to achieve valorization of fruit and vegetable pomaces. The importance of the residues from fruits and vegetables is still growing; therefore; the study presents the novel route of a fractioning process for the conversion of agro-industrial biomasses, such as pomaces, into useful feedstocks with potential application in the fields of fuels, chemicals, and polymers. Hence, the biorefinery process is expected to convert them into various by-products offering a great diversity of low-cost materials. The final product of the process is the cellulose of the biofuel importance. The study presents the novel route of the fractioning process for the conversion of agro-industrial biomasses, such as pomaces, into useful feedstocks with a potential application in the fields of fuels, chemicals, and polymers. Therefore the aim of this paper was to present the novel route of the pomaces fraction and the characterization of residuals. Pomaces from apple, cucumber, carrot, and tomato were treated sequentially with water, acidic solution, alkali solution, and oxidative reagent in order to obtain fractions reach in sugars, pectic polysaccharides, hemicellulose, cellulose, and lignin. Pomaces were characterized by dry matter content, neutral detergent solubles, hemicellulose, cellulose, and lignin. Obtained fractions were characterized by the content of pectins expressed as galacturonic acid equivalent and hemicelluloses expressed as a xyloglucan equivalent. The last fraction and residue was cellulose characterized by crystallinity degree by X-ray diffractometer (XRD), microfibril diameter by atomic force microscope (AFM), and overall morphology by scanning electron microscope (SEM). The hemicelluloses content was similar in all pomaces. Moreover, all the materials were characterized by the high pectins level in extracts evaluated as galacturonic acid content. The lignins content compared with other plant biomasses was on a very low level. The cellulose fraction was the highest in cucumber pomace. The cellulose fraction was characterized by crystallinity degree, microfibril diameter, and overall morphology. Isolated cellulose had a very fine structure with relatively high crystalline index but small crystallites.

BackgroundThe primary cell wall of fruits and vegetables is a structure mainly composed of polysaccharides (pectins, hemicelluloses, cellulose). Polysaccharides are assembled into a network and linked together. It is thought that the percentage of components and of plant cell wall has an important influence on mechanical properties of fruits and vegetables.ResultsIn this study the Raman microspectroscopy technique was introduced to the visualization of the distribution of polysaccharides in cell wall of fruit. The methodology of the sample preparation, the measurement using Raman microscope and multivariate image analysis are discussed. Single band imaging (for preliminary analysis) and multivariate image analysis methods (principal component analysis and multivariate curve resolution) were used for the identification and localization of the components in the primary cell wall.ConclusionsRaman microspectroscopy supported by multivariate image analysis methods is useful in distinguishing cellulose and pectins in the cell wall in tomatoes. It presents how the localization of biopolymers was possible with minimally prepared samples.

Raman and Fourier Transform Infrared (FT-IR) spectroscopy was used for assessment of structural differences of celluloses of various origins. Investigated celluloses were: bacterial celluloses cultured in presence of pectin and/or xyloglucan, as well as commercial celluloses and cellulose extracted from apple parenchyma. FT-IR spectra were used to estimate of the Iβ content, whereas Raman spectra were used to evaluate the degree of crystallinity of the cellulose. The crystallinity index (XCRAMAN%) varied from −25% for apple cellulose to 53% for microcrystalline commercial cellulose. Considering bacterial cellulose, addition of xyloglucan has an impact on the percentage content of cellulose Iβ. However, addition of only xyloglucan or only pectins to pure bacterial cellulose both resulted in a slight decrease of crystallinity. However, culturing bacterial cellulose in the presence of mixtures of xyloglucan and pectins results in an increase of crystallinity. The results confirmed that the higher degree of crystallinity, the broader the peak around 913 cm−1. Among all bacterial celluloses the bacterial cellulose cultured in presence of xyloglucan and pectin (BCPX) has the most similar structure to those observed in natural primary cell walls.

Main conclusionDuring on-tree ripening, the pectin distribution changed from polydispersed in cell wall to cumulated in cell wall corners. During apple storage, the pectin distribution returned to evenly dispersed along the cell wall.The plant cell wall influences the texture properties of fruit tissue for example apples become softer during ripening and postharvest storage. This softening process is believed to be mainly connected with changes in the cell wall composition due to polysaccharides undergoing an enzymatic degradation. These changes in polysaccharides are currently mainly investigated via chemical analysis or monoclonal labeling. Here, we propose the application of Raman microscopy for evaluating the changes in the polysaccharide distribution in the cell wall of apples during both ripening and postharvest storage. The apples were harvested 1 month and 2 weeks before optimal harvest date as well as at the optimal harvest date. The apples harvested at optimal harvest date were stored for 3 months. The Raman maps, as well as the chemical analysis were obtained for each harvest date and after 1, 2 and 3 months of storage, respectively. The analysis of the Raman maps showed that the pectins in the middle lamella and primary cell wall undergo a degradation. The changes in cellulose and hemicellulose were less pronounced. These findings were confirmed by the chemical analysis results. During development changes of pectins from a polydispersed form in the cell walls to a cumulated form in cell wall corners could be observed. In contrast after 3 months of apple storage we could observe an substantial pectin decrease. The obtained results demonstrate that Raman chemical imaging might be a very useful tool for a first identification of compositional changes in plant tissue during their development. The great advantage Raman microspectroscopy offers is the simultaneous localization and identification of polysaccharides within the cell wall and plant tissue.Electronic supplementary materialThe online version of this article (doi:10.1007/s00425-015-2456-4) contains supplementary material, which is available to authorized users.

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Dietary fibres are regarded as the source of polysaccharides and antioxidants such as polyphenols. However, addition of dietary fibre to bread causes significant reduction in its quality. The bread quality is connected with the structure of gluten proteins. For this reason, Fourier transform Raman spectroscopy was applied to determine changes in structure of gluten proteins modified by seven dietary fibres. The fibres were added to model flour reconstituted with wheat gluten and wheat starch. The model flour was used to provide gluten proteins of definite structure. The obtained results showed that six out of seven fibres caused similar changes in β-turn structures. The appearance of the band at 1642 cm À1 and the shift toward lower wavenumbers of the band at 1670 cm À1 in the difference spectra indicated hydrogen bonding of carbonyl groups in β-turns leading to protein folding/aggregation. Addition of fibre preparations caused also changes in conformation of disulfide bridges (S-S), corresponding to transformation to trans-gauche-gauche and trans-gauche-trans conformations at the expense of the stable gauche-gauchegauche conformation. The S-S bonds in less stable conformations were formed inside the protein complex as well as between protein complexes in the form of β-structures. Generally, the observed changes in gluten proteins after addition of dietary fibres were results of interactions between fibre polysaccharides and gluten proteins rather than between polyphenols and gluten proteins.