Academic literature on the topic 'Pectine – Composés'

We prepared humo-pectic hydrogels through ionotropic gelation by crosslinking natural pectins of different degree of methyl-esterification with either humic substances (HS) extracted from cow manure compost or humic-like substances (HULIS) from depolymerized lignocellulose biorefinery waste. The hydrogels were characterized by solid-state 13C-NMR spectroscopy, scanning electron microscopy, spectroscopic magnetic resonance imaging and rheological analyses. Their ability to work as controlled release systems was tested by following the release kinetics of a previously incorporated model phenolic compound, like phloroglucinol. Our results indicated that the release properties of hydrogels were influenced by the molecular composition of HS and HULIS and by the different degrees of methyl-esterification of pectins. The hydrogel made by the high methoxyl pectin and HS showed the fastest rate of phloroglucinol release, and this was attributed not only to its morphological structure and crosslinking density but also to the least formation of ionic interactions between phloroglucinol and the polysaccharidic chains. Our study suggests that the efficiency of novel humo-pectic hydrogels as sustainable carriers of agroproducts to crops is related to a careful choice of the characteristics of their components.

Currently, pectins are widely used in the cosmetic, pharmaceutical, and food industries, mainly as texturizing, emulsifying, stabilizing, and gelling agents. Pectins are polysaccharides composed of a large linear segment of α-(1,4) linked d-galactopyranosyluronic acids interrupted by β-(1,2)-linked l-rhamnoses and ramified by short chains composed of neutral hexoses and pentoses. The characteristics and applications of pectins are strongly influenced by their structures depending on plant species and tissues but also extraction methods. The aim of this review is therefore to highlight the structures of pectins and the various methods used to extract them, including conventional ones but also microwave heating, ultrasonic treatment, and dielectric barrier discharge techniques, assessing physico-chemical parameters which have significant effects on pectin characteristics and applications as techno-functional and bioactive agents.

Our previous research has indicated that the pit membrane regulates deep supercooling of xylem parenchyma in woody plants. This area of the cell wall is composed of three layers that may be rich in pectins. Since pectins may define the porosity of the cell wall they may also regulate deep supercooling. The present study examined pectin distribution in ray cells using monoclonal antibodies, that recognize un-esterified (JIM5) and methyl-esterified (JIM7) epitopes of pectin, in conjuction with immunogold electron microscopy. Antibodies were obtained courtesy of J. Paul Knox, John Innes Inst., U.K. Dormant and non-dormant tissues of Prunus persica, Cornus florida and Salix babylonica were utilized. Labelling with JIM7 revealed that methyl-esterified pectins were abundant and evenly distributed within the primary cell wall and amorphous layer. Labelling with JIM5 revealed that un-esterified pectins were located specifically within the pit membrane, in the outer region of the primary cell wall. No differences were observed between species, however, preliminary data indicated that JIM5 labelling was greater in dormant than in non-dormant tissues.

Curcumin-loaded chitosan-pectin microparticles based on polymeric microencapsulation were prepared by two methods to delay the release of curcumin in the digestive system, employing Mg2+ as a pectin-crosslinking agent for the first time. Pectin-coated curcumin-chitosan microparticles (C-g-PMg) and curcumin-loaded chitosan-pectin composite microparticles (C-PMg-g) were formulated, and their release profiles at pH 1.2 and at pH 6.8 were tested. The former (C-g-PMg) showed slower curcumin release profiles than the latter (C-PMg-g) because the C-g-PMg are composed of two layers, a chitosan-glutaraldehyde layer and a pectin-Mg2+ layer, which together hold the curcumin for a longer duration. Of the pectin-coated microparticles, those crosslinked with Mg2+ showed a slower release rate than those crosslinked with Ca2+, but the former showed a faster release rate at pH 6.8 in the presence of pectinase, acting as a promising drug delivery carrier for treating a colonic disease. The pectin layer and the pectin-crosslinking agent play a vital role in prolonging the release of curcumin until pectin is degraded by pectinase.

Pectin and hemicellulose were solubilized from cell walls of peach [Prunus persica (L.) Batsch] fruit differing in firmness by extraction with imidazole and sodium carbonate (pectin extracts), followed by a graded series of potassium hydroxide (hemicellulose extracts). The extracts were subjected to size exclusion chromatography. In imidazole extracts, as fruit softened, there was an increase in proportion of a large apparent molecular mass peak, with a galacturonosyl to rhamnosyl residue ratio resembling a rhamnogalacturonan-like polymer. A smaller apparent molecular mass peak was enriched in galacturonic acid and probably represented a broad polydisperse peak derived from more homogalacturonan-like polymers. In sodium carbonate extracts, a homogalacturonan-like polymer appeared to elute primarily as a higher apparent molecular mass constituent, which increased in quantity relative to other constituents as fruit softened. In cold 1 mol·L-1 KOH extracts three peaks predominated. A xyloglucan-like polymer appeared to elute predominantly in the second peak and fucose was strongly associated with it. In 4 mol·L-1 KOH extracts (tightly bound hemicellulose) the higher apparent molecular mass peak was predominantly acidic and presumably of pectic origin. The smaller apparent molecular mass peaks were composed primarily of neutral sugars, the second peak became smaller and the third peak larger as fruit softened. The ability to separate pectin and xyloglucan-like polymer as two separate fractions based on charge suggests that the nature of any pectin-hemicellulose interaction in this fraction is probably one of physical entrapment of pectin fractions by hemicellulose and not principally by covalent crosslinking between the two polysaccharide classes in peach. Flesh firmness serves as an important determinant of quality in peaches. Our results indicate that apparent molecular mass of both pectins and hemicelluloses changed as peaches softened, resulting in alteration of cell wall structure and associated with decreased tissue cohesion.

Pectate lyase 10A (Pel10A) enzyme from Pseudomonas cellulosa is composed of 649 residues and has a molecular mass of 68.5kDa. Sequence analysis revealed that Pel10A contained a signal peptide and two serine-rich linker sequences that separate three modules. Sequence similarity was seen between the 9.2kDa N-terminal module of Pel10A and family 2a carbohydrate-binding modules (CBMs). This N-terminal module of Pel10A was shown to encode an independently functional module with affinity to crystalline cellulose. A high sequence identity of 66% was seen between the 14.2kDa central module of Pel10A and the functionally uncharacterized central modules of the xylan-degrading enzymes endoxylanase 10B, arabinofuranosidase 62C and esterase 1D, also from P. cellulosa. The 35.8kDa C-terminal module of Pel10A was shown to have 30 and 36% identities with the family 10 pectate lyases from Azospirillum irakense and an alkaliphilic strain of Bacillus sp. strain KSM-P15, respectively. This His-tagged C-terminal module of the Pel10A was shown to encode an independent catalytic module (Pel10Acm). Pel10Acm was shown to cleave pectate and pectin in an endo-fashion and to have optimal activity at pH10 and in the presence of 2mM Ca2+. Highest enzyme activity was detected at 62°C. Pel10Acm was shown to be most active against pectate (i.e. polygalacturonic acid) with progressively less activity against 31, 67 and 89% esterified citrus pectins. These data suggest that Pel10A has a preference for sequences of non-esterified galacturonic acid residues. Significantly, Pel10A and the P. cellulosa rhamnogalacturonan lyase 11A, in the accompanying article [McKie, Vincken, Voragen, van den Broek, Stimson and Gilbert (2001) Biochem. J. 355, 167–177], are the first CBM-containing pectinases described to date.

Abstract A novel adsorbent, composed of cross-linked de-esterified pectin microspheres, was prepared via cross-linking with Ca(II) and modification by de-esterified pectin, low-methoxyl pectin (LMP) and pectic acid (PA). Fourier transform infrared (FTIR), energy dispersive spectrometry (EDS), scanning electron microscopy (SEM) and atomic absorption spectroscopy (AAS) were applied too, exhibiting a successful fabrication, good adsorption ability, and well-defined surface microstructure beneficial to Pb(II) adsorption. The adsorption ability of pectin microspheres (PMs), low-methoxyl pectin microspheres (LMPMs) and pectic acid microspheres (PAMs) for Pb(II) in aqueous solution were explored. The maximum adsorption capacity of PMs, LMPMs and PAMs was 127 mg·g−1, 292 mg·g−1 and 325 mg·g−1 at pH 5.0 respectively, indicating a great improvement of LMPMs and PAMs in the adsorption ability for Pb(II) compared with PMs. Furthermore, the adsorption mechanism was proposed. The experimental data were well fitted with pseudo-second-order kinetic and Langmuir isotherm models. Five-cycle reusability tests demonstrated that microspheres could be used repeatedly. All the results confirmed that LMPMs and PAMs, which presented outstanding adsorption capability and reusability, could be a good candidate for wastewater purification.

Goiabas (Psidium guajava L.) cultivar Pedro Sato foram utilizadas para extração de pectina. Os frutos separados polpa e polpa com casca foram secos em estufa com circulação de ar. Amostras secas foram caracterizadas física e quimicamente. O planejamento composto central rotacional com quatro pontos axiais e três repetições no ponto central foi utilizado para determinar o rendimento de extração de pectina das farinhas de polpa e de polpa com casca de goiaba. A extração foi realizada em 4 g de farinha para 200 mL de solução de ácido cítrico em diferentes concentrações e em diferentes tempos de extração, a temperatura de 97 ºC. As pectinas obtidas nas melhores condições de extração foram caracterizadas. A extração de pectina com ácido cítrico e precipitação alcoólica forneceu rendimentos acima de 11% para a farinha de polpa e de polpa com casca de goiaba. As melhores condições de extração foram: concentração de ácido cítrico de 5 g.100 g-1 e tempo de extração de 60 minutos. As pectinas obtidas apresentaram-se de baixa esterificação e com teor de ácido galacturônico próximo ao padrão comercial (65%).

As the outer boundary of plant cells, the cell wall is integral to all aspects of plant growth, development, and interactions with the environment. Dicot primary cell walls are composed of a network of cellulose, hemicellulose and proteins embedded in a matrix of acidic pectins. Pectins are synthesized in the Golgi apparatus by the sequential addition of nucleotide sugars by glycosyltransferases, following which they are secreted to the apoplast. During their differentiation, the mucilage secretory cells (MSCs) of the Arabidopsis seed coat undergo sequential biosynthesis and secretion of a primarily pectinaceous mucilage followed by secondary cell wall production. Several genes affecting MSC differentiation have been identified with roles ranging from the production of nucleotide sugar substrates for pectin synthesis to putative cell wall modification enzymes to transcription factors required to control MSC differentiation. These preliminary studies of the MSCs demonstrate that they will play a valuable role in gene discovery related to cell wall production and modification. Furthermore, they have the potential to become an important system in which to study the interaction and regulation of pectin biosynthetic factors in differentiating cells. These results will contribute to answering the important question of how cell wall production and modification occur throughout a growing plant living in a complex environment.

The segregative phase separation behavior of biopolymer mixtures composed entirely of polysaccharides was investigated. First, the electrical, optical, and rheological properties of alginate, modified beet pectin, and unmodified beet pectin solutions were characterized to determine their electrical charge, molecular weight, solubility, and flow behavior. Second, suitable conditions for inducing phase segregation in biopolymer mixtures were established by measuring biopolymer concentrations and segregation times. Third, alginate–beet pectin mixtures were blended at pH 7 to promote segregation and the partitioning of the biopolymers between the upper and lower phases was determined using UV–visible spectrophotometry, colorimetry, and calcium sensitivity measurements. The results revealed that phase separation depended on the overall biopolymer concentration and the degree of biopolymer hydrophobicity. A two-phase system could be formed when modified beet pectins (DE 68%) were used but not when unmodified ones (DE 53%) were used. Our measurements demonstrated that the phase separated systems consisted of a pectin-rich lower phase and an alginate-rich upper phase. These results suggest that novel structures may be formed by utilization of polysaccharide–polysaccharide phase separation. By controlling the product formulation and processing conditions it may therefore be possible to fabricate biopolymer particles with specific dimensions, shapes, and internal structures.

Ce rapport décrit une étude de recherche visant à améliorer la connaissance des propriétés émulsifiantes de la pectine. L’étude a été initiée par une demande commerciale de la société Cargill visant à trouver un additif alimentaire choisi dans une gamme de polysaccharides capable de remplacer la gomme arabique pour une utilisation en tant qu’agent émulsifiant. La recherche documentaire a montré que la pectine était un bon candidat avec des propriétés émulsifiantes reconnues. Cependant, si l’origine des propriétés émulsifiantes de la gomme arabique a été étudiée, celle de la pectine n’a fait l’objet d’aucune recherche spécifique au moment de cette étude. Le travail de recherche a mis en oeuvre 3 phases qui ont permis de comprendre l’origine des propriétés émulsifiantes de la pectine et ses limites. La première partie a porté sur la mise en évidence des capacités tensioactives de certains biopolymères, notamment de la pectine. Il en a été déduit que la pectine peut abaisser la tension à l’interface de systèmes eau/huile et que parmi les pectines celles de citron de faibles masses molaires et de betterave sont les plus efficaces. Les propriétés émulsifiantes sont corrélées avec les résultats de tensions et de bons résultats en matière de qualité d’émulsions ont été obtenus avec la pectine. Un examen du potentiel Zéta n’a pas apporté de contribution spécifique. La seconde partie a été consacrée aux aspects structuraux. La pectine a été séparée en fonction de son affinité pour l’huile en utilisant deux méthodes, une méthode physique de séparation à partir d’une émulsion et une méthode chromatographique (HIC). Dans tous les cas les fractions ont été analysées, ce qui a permis de reconnaitre des éléments structuraux contribuant aux fonctions amphiphiles. Le plus important est une protéine, qui fait probablement partie d’un ensemble arabinane-protéine-phénol. D’une façon quantitative on a trouvé que 26,7% de la pectine pouvait s’adsorber sur l’huile et que 3,83 mg/m2 de pectine recouvraient l’huile. Le rôle des acétyles n’est pas apparu comme essentiel. Et les protéines n’ont pas pu être séparées de la pectine, montrant ainsi la probabilité d’une liaison chimique entre des fractions protéiques et la pectine. Il est également ressorti de cette partie que la nature de l’huile est un paramètre qui a un effet sur l’adsorption de la pectine. Ainsi l’huile végétale comme celle de colza fixe plus de pectine et requiert moins de protéines que l’huile essentielle d’orange. La troisième partie a été axée vers la stabilité des émulsions préparées avec la pectine. Des émulsions modèles et d’autres plus proches de systèmes applicatifs ont été étudiées. Des limites quant à la capacité émulsifiante de la pectine ont été mises en évidence. Un processus de déstabilisation des émulsions préparées avec la pectine a été identifié. La présence d’agrégats a été observée et il a été reconnu que ces agrégats étaient responsables de l’instabilité des émulsions. L’origine de ces agrégats a été étudiée et il est en ressorti qu’ils sont liés à la présence de cations polyvalents et particulièrement du calcium qui stabilise des groupes de globules d’huile par pontage calcique. La stabilisation des émulsions par la pectine est possible mais il faut réduire les interactions avec le calcium en réduisant l’affinité du polymère pour les cations divalents. Ceci peut être réalisé en utilisant par exemple la pectine de betterave qui est moins sensible au calcium que la pectine de citron. On peut également réduire la masse molaire des pectines, ce qui réduit également les possibilités de recouvrement des chaines de pectines appartenant à des globules distincts. Enfin en utilisant moins d’huile, la faible fraction de pectine adsorbable peut de recouvrir davantage les globules ce qui permet d’augmenter la quantité de pectine adsorbée à la surface ainsi que les forces de répulsion
This report describes a research study that aims at a better understanding of the emulsifying capacities of pectin. This research study started with a commercial request regarding the need of a product and possibly a polysaccharide material that has emulsifying abilities equivalent to those of gum arabic and that can replace it in beverage applications. Literature has shown that pectin has good emulsifying ability and could be successfully used for this purpose. However, no study was done to elucidate the emulsifying properties of pectin whereas those of gum arabic were studied in depth. This research study was organised within 3 phases that have provided information about the origin and limits of emulsifying functionalities of pectin. The first part of the study focused on the observation of surface properties of biopolymers and specially pectins. It was turned out that pectin can lower surface tensions at oil/water interfaces and among the pectin variety, low molecular weight citrus pectin and sugar beet pectin gave the best results. Emulsifying abilities and surface properties are quite well correlated. However zeta potential measurements did not bring relevant information. In the second part, the chemistry of emulsifying properties of pectin was studied. Thus, pectin fractions were separated as a function of their affinity for the oily phase. Two approaches were made, first by separating and recovering the 2 phases in an emulsion and by hydrophobic interaction chromatography (HIC). In both cases fractions were analysed, and components that contribute to amphiphilic behaviour were identified. The first one is a protein that probably belongs to group made of arabinan-protein-phénolic acid. Quantitative results have shown that 26,7% of the pectin mass can absorb on the oil and that 3,83 mg/m2 is surface coverage load. It was not observed that acetyls have an important role regarding surface properties. As protein could not be separated from pectin, then we came up to the hypothesis of a strong chemical link between pectin and protein. It was also observed that the oil nature has an effect upon the surface adsorption. Thus pectin adsorbs more on rapeseed oil and lower protein content in the pectin is needed than for adsorption on orange oil. Within the third part of the study, the stability on storage of the emulsions made with pectin was examined. Model emulsions and commercial emulsion formulas were tested. So limits when using pectin in emulsions were observed and a process of pectin made emulsions was identified. Aggregates were observed and they were recognized as responsible for emulsions instability. The aggregates origin was studied and it was concluded that they are due to presence of divalent cations and specifically calcium that stabilizes groups of droplets by bridging. Indeed, pectin can stabilise emulsions; however calcium interaction must be carefully controlled. As it is not always feasible to use a calcium free medium, then the affinity of the polyelectrolyte for calcium has to be lowered. This can be achieved in using sugar beet pectin that is much less calcium sensitive than citrus pectin. Molecular weight of pectin can also be considered, when reducing the molecular weight, the overlapping of pectin chains belonging to separate droplets is reduced, therefore calcium bridging flocculation is reduced. At last, it is recommended to use less oil in the emulsion; this allows the small pectin fraction that has emulsifying capacity to better cover the oil

La pectine est un polysaccharide anionique extrait des végétaux supérieurs et, en particulier, de l'écorce des fruits et des légumes. Ce polymère a été modifié chimiquement par fixation de chaines alkyles en C₁₂, C₁₆ et C₁₈, par trois voies de synthèse différentes, de manière à obtenir des dérivés associatifs dans lesquels les chaines apolaires sont associées au squelette polymère par des liaisons covalentes et/ou des liaisons ioniques. Les propriétés physico-chimiques des différents dérivés hydrophobisés résultants ont été étudiées de façon comparative par viscosimétrie, spectrométrie de fluorescence, en rhéologie et par des mesures de tension de surface, dans l'eau pure ou en présence de sels. Quel que soit le mode de synthèse et donc de fixation des chaines hydrophobes au polymère, tous ces dérivés présentent des propriétés associatives. En régime dilué, des interactions intramoléculaires se mettent en place, conduisant à une diminution de la viscosité macroscopique du milieu. En régime plus concentré, des interactions hydrophobes intermoléculaires s'établissent, conduisant à l'obtention de solutions aqueuses de très haute viscosité, voire même de réseaux tridimensionnels physiquement pseudo - réticulés ayant l'apparence d'hydrogels. Cependant, à coté de ces ressemblances, les chaines hydrophobes ne s'organisent pas au niveau moléculaire de la même façon, selon qu'elles sont associées au squelette polysaccharidique de façon covalente ou ionique. Cette différence de structure se traduit au plan macroscopique, en particulier par des propriétés de surface et des comportements rhéologiques sensiblement dissemblables.

Cette thèse porte sur la fonctionnalisation de la pectine de citron par des composés phénoliques. Une première stratégie a consisté à greffer les produits issus de l’oxydation de l’acide férulique (AF), en milieu aqueux (pH 7,5, 30 ° C), en présence de la laccase de Myceliophthora thermophila (obtention de pectine F). L’enjeu était de démontrer le greffage covalent de composés phénoliques exogènes sur le polysaccharide, de recueillir des informations sur la structure et les propriétés du polymère fonctionnalisé et de les comparer aux caractéristiques du polymère natif. Une deuxième stratégie de fonctionnalisation de la pectine a été envisagée, basée sur l'adsorption des produits d'oxydation de l'AF sur la pectine (obtention de pectine POX). Quel que soit le mode de fonctionnalisation, des analyses biochimiques ont montré l'incorporation de composés phénoliques dans la pectine. La structure et les propriétés des pectines modifiées dépendent du type de fonctionnalisation subie par le polysaccharide (greffage covalent ou adsorption). Des analyses structurales suggèrent que le greffage covalent de phénols fait intervenir les fonctions carboxyles de la pectine (formation de liaisons ester) sur lesquelles des oligomères d'acide férulique viendraient se lier. Les propriétés des pectines fonctionnalisées (POX et F) et de la pectine native ont été étudiées et comparées afin de mettre en évidence les changements apportés. L'étude des propriétés thermiques des différentes poudres de pectine suggèrent une structure moins organisée et moins compacte pour les polymères fonctionnalisés par rapport à la pectine native. L’activité antioxydante des pectines fonctionnalisées est améliorée tandis que leur caractère hygroscopique est diminué en raison de l'incorporation de composés phénoliques hydrophobes. De même que la pectine native, les pectines POX et F présentent un profil rhéofluidifiant. Toutefois, la viscosité et la vitesse de gélification mesurées dans le cas de la pectine F sont significativement diminuées par rapport à celles obtenues pour la pectine native. La pectine POX présente un comportement intermédiaire. Des résultats préliminaires d'assemblages ont montré qu'il est possible d'associer la pectine native ou modifiée à un autre polysaccharide, le chitosane. Les microparticules obtenues ont montré leur capacité à encapsuler un principe actif tel que la curcumine
This dissertation concerns the functionalization of the citrus pectin with phenolic compounds. A first strategy consisted in grafting the products issued from the oxidation of ferulic acid (FA), in aqueous medium (pH 7,5, 30 ° C), in the presence of the laccase of Myceliophthora thermophila (pectin F). The main objectives were to demonstrate the covalent grafting of exogenous phenols onto the polysaccharide, to collect information about the structure and the properties of the modified polymer and to compare them with the characteristics of the native one. A second strategy of functionalization was applied, based on the adsorption of FA oxidation products onto the pectin (pectin POX). Whatever the functionalization pathway, biochemical analyses showed the incorporation of phenolic compounds into the pectin. The structure and the properties of the modified pectins depended on the type of modification undergone by the polysaccharide (covalent grafting or adsorption). Structural analyses suggested that the covalent grafting of phenols involved the carboxyl groups of the pectin (ester bound) on which FA oligomers were bound. The properties of native and modified pectins (POX and F) were studied and compared aiming to highlight the changes brought by functionalization. The study of the thermal properties of pectin POX and F suggested less organized and less compact structures compared to the native one. The antioxidant activity of the modified pectins was improved whereas their hygroscopic character was decreased because of the incorporation of hydrophobic phenolic compounds. As the native pectin, the pectins POX and F presented a shear-thinning profile. However, the viscosity and the gelation rate measured for the pectin F were significantly decreased, compared with those obtained for the native pectin. The pectin POX presented an intermediate behavior. Preliminary results of assemblies demonstrated the possibility to associate the native or modified pectin to another polysaccharide, the chitosan, leading to microparticles capable to encapsulate an active ingredient such as the curcumin

L'allongement de l'hypocotyle de lin résulte de la sommation des élongations des cellules épidermiques. Après 3 jours de culture à l'obscurité, les parois des cellules de l'hypocotyle sont très déformables. L'extensiométrie montre la nature plastique et élastique de la déformation. Les propriétés mécaniques de déformation des parois sont très diminuées quand l'élongation cellulaire est inhibée par la lumière. Même s'il n'y a pas d'évolution significative des surfaces et des compositions globales pariétales pendant la croissance, les liaisons des pectines dans les parois sont modifiées. Après 3 jours de germination à l'obscurité, les trois-quarts des molécules extraites par l'eau bouillante ou le chélateur du calcium CDTA,Na2 sont enchevêtrés. Ces polysaccharides sont majoritairement constitués d'oses neutres contenant des séquences riches en acides galacturoniques neutralisés par le magnésium. Le quart restant, lié de façon covalente et/ou ionique est un mélange de polysaccharides neutres, de rhamnogalacturonanes de type I intensément acétyles et de courts homogalacturonanes non linéaires. Ces polyanions neutralisés par le calcium in vivo présentent une faible affinité pour le calcium in vitro et réagissent avec le rouge de ruthénium et l'hydroxylamine ferrique. Quatre jours après repiquage sur milieu liquide ionique et transfert à la lumière continue, 90% des composés pectiques pariétaux appartiennent aux familles suivantes: 1) des rhamnogalacturonanes de type I porteurs de chaînes latérales arabinanes et galactanes liés de façon covalente ; 2) des acides polygalacturoniques liés aux parois par des ponts calcium localisés principalement dans l'épiderme ; 3) des rhamnogalacturonanes de type I en continuité avec des homogalacturonanes probablement non linéaires neutralisés par le magnésium in vivo. Ces polymères sont moins acétyles que les molécules de composition similaire après trois jours de croissance à l'obscurité

La couleur, la fermeté, la saveur, ou l’aptitude à la conservation, sont les principaux critères de qualité qui déterminent le choix du consommateur, les procédés de transformation et la stabilité des fruits charnus. Ces critères dépendent des mécanismes déterminants la qualité des productions, faisant intervenir les ions métalliques, les composés phénoliques et les parois cellulaires. Pour appréhender ces mécanismes, les travaux ont été réalisés sur deux variétés de pommes à cidre et étendus aux variétés de raisins de cuve. Le développement de méthodes de cryo-microscopie associées à la fluorescence X et UV a permis l’identification et la distribution tissulaire des ions métalliques et des composés phénoliques. Les métaux de transition et les flavanols sont retrouvés majoritairement dans la cuticule alors que le calcium, le magnésium et les pigments phénoliques sont co-localisés dans les couches sous-cuticulaires. Une distribution homogène du potassium est observée de la couche sous-cuticulaire au cortex externe, zones riches en acides phénoliques. Parmi ces acides, les acides hydroxycinnamiques sont potentiellement estérifiés dans les parois cellulaires. L’impact de ces composés sur la qualité des fruits lors de leur consommation ou transformation a été abordé par l’étude des interactions entre les ions métalliques, la pectine des parois cellulaires et les composés phénoliques en présence de peroxyde d’hydrogène. L’ensemble des résultats : distribution des ions métalliques et composés phénoliques, ainsi que les interactions et les mécanismes réactionnels possibles est résumé dans un modèle conceptuel qui servira de base pour de futurs travaux visant à un meilleur contrôle des propriétés organoleptiques des fruits frais et transformés
Colour, firmness, taste and long storage ability, are the main quality parameters that define consumer choice, processing and shelf-life of fleshy fruits. These quality criteria rely on physiological and physicochemical mechanisms that involve metallic ions, phenolic compounds and cell wall. To better understand these mechanisms, the thesis study was realised on two cider apples varieties and extended to wine grapes. The development of cryo-microscopy methods associated to X-ray and deep UV fluorescence highlighted the identification and distribution at the tissue scale of metallic ions and phenolic compounds. Transition metals and flavanols were mostly found in the cuticle while calcium, magnesium and phenolic pigments were co-localised in the sub-cuticle tissue layers. A homogeneous distribution of potassium was observed from the sub-cuticle to the outer cortex cell layers, a region that is rich in phenolic acids. Among these acids, hydroxycinnamic acids were found to be potentially esterified within cell wall. The impact of these compounds on the quality of fruit during consumption or processing was considered by studying the interactions between metal ions, cell wall pectin and phenolic compounds in the presence of hydrogen peroxide. All results: distribution of metal ions and phenolic compounds, as well as possible interactions and mechanisms of reaction, are summarized in a conceptual model that will serve as a basis for future work aiming at better controlling the organoleptic properties of fresh and processed fruit

Orientadores: Telma Teixeira Franco, Cristiana Maria Pedroso Yoshida
Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Química
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Resumo: Complexos de polieletrólitos (PEC) podem ser obtidos a partir de polímeros que apresentam cargas opostas, como quitosana e pectina. A inovação deste trabalho foi desenvolver sistemas carreadores de compostos bioativos (antocianina (ATH) e insulina), na forma de membranas e nanocomplexos (NCXs) obtidos a partir da interação eletrostática existente entre os polímeros naturais quitosana e pectina. Quitosana é um polímero linear catiônico composto por N-glucosamina e N-acetilglucosamina, e apresenta diferentes graus de acetilação (GA). Pectina é um polímero linear aniônico composto principalmente por ácido D-galacturônico com uma fração dos grupos carboxilas sendo metoxilados. Membranas PEC foram desenvolvidas para incorporar a ATH formando um dispositivo inteligente indicador de pH, com alteração visual e reversível da cor. NCXs foram elaborados na forma de micro/nanopartículas carregadas de insulina (pI = 5,3) para avaliar a liberação controlada do fármaco, via oral, em sistemas in vitro. Membranas PEC foram estudadas usando quitosana e pectina em diferentes pH (3,0, 4,0, 5,0 e 5,5) e relações molares pectina:quitosana. Soluções de pectina e quitosana, ambas de 0,50 g/100 g de solução e mesma força iônica foram misturadas e homogeneizadas. As membranas PEC apresentaram superfície rugosa e parcialmente homogênea. A máxima formação do PEC foi em pH 5,5, com aproximadamente 60,0 % de rendimento. O processo de difusão do bioativo ATH a partir das membranas PEC indicou que o composto foi incorporado na matriz, onde menos de 2,0 % (em massa) do bioativo migrou para a solução tampão em que estavam imersos (pH 4,0, 5,5 e 7,0). A compatibilidade entre os polímeros e ATH foi verificada pelas análises termogravimétricas, microscopia eletrônica de varredura, espectroscopia de infravermelho com transformada de Fourier e difração de raios X. Os NCXs foram obtidos a partir da homogeneização das soluções de quitosana (5,0 mg/mL) e pectina (5,0 mg/mL) em diferentes pH (2,70, 4,0, 5,0 e 5,5), relações de carga, carga total e molaridade das soluções de NaCl. A melhor condição para obtenção das micro/nanopartículas foi em pH < 4,0, havendo formação de partículas entre 250-2500 nm e rendimento de formação entre 18-33 % (em massa). O GA da quitosana influenciou na citotoxicidade das células Caco-2. A relação de carga promoveu efeito significativo na associação da insulina às partículas, na ordem de 34,0-62,0 %. As micrografias indicaram a formação de partículas esféricas, compactas e distribuídas homogeneamente. A liberação de insulina ocorreu de forma lenta e gradativa em fluido intestinal simulado (SIF)
Abstract: Polyelectrolyte complex (PEC) with very strong intermolecular interaction can be obtained from polysaccharides that present opposite charges such as chitosan and pectin. The innovation of this work was developing carrier systems of bioactive compounds (anthocyanin (ATH) and insulin) using membranes and nanocomplexes (NCXs) obtained from electrostatic interaction that exists between the polymers chitosan and pectin. Chitosan is a linear cationic polysaccharide composed by N-glucosamine and N-acetil glucosamine and presents different degree of acetylation (DA). Pectin is a linear anionic polysaccharide composed mainly by D-galacturonic acid with one part of carboxyl group methoxylated. PEC membranes were developed to entrap ATH forming an intelligent pH indicator device, with visual and reversible colour change. NCXs were elaborated such as micro and nanoparticles loading insulin (pI = 5.3) to evaluate drug controlled delivery, oral pathway, in systems in vitro. PEC membranes were studied using chitosan and pectin in different pH (3.0, 4.0, 5.0, and 5.5) and molar ratios pectin:chitosan. Pectin and chitosan solutions, both at 0.50 g/100 g of solution and the same ionic force were mixed and homogenized. PEC membranes were characterized by rough and partially homogeneous surface. The maximum PEC formation was at pH 5.5, with approximately 60.0 % of yield. The diffusion process of bioactive ATH from PEC membranes indicated great entrapment of compound on matrix, where less than 2.0 % (mass) of pigment migrated to the aqueous buffer solution (pH 4.0, 5.5 and 7.0). The compatibility between the polymers and ATH was verified by thermogravimetric analysis, scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The NCXs were obtained from homogenization of chitosan (5.0 mg/mL) and pectin (5.0 mg/mL) solutions at different pH (2.7, 4.0, 5.0 and 5.5), charge ratios, total charge and molarity of NaCl solutions. The best condition to obtain micro/nanoparticles was in pH < 4.0, with size particles formation between 250-2500 nm and yield of NCXs formation between 18-33 % (mass). The DA of chitosan influenced on cytotoxicity of Caco-2 cells. The charge ratio promoted significant effect on drug efficient association to the particles, around 34.0-62.0 %. The micrograpH indicated the formation of shape and compact particles distributed homogeneity. The insulin delivery occurred slowly and gradually on simulated intestinal fluid (SIF)
Doutorado
Engenharia de Processos
Doutor em Engenharia Química

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Conselho Nacional de Desenvolvimento Científico e Tecnológico
Researches based on the mixture of synthetic with natural polymers have intensified in recent times. The idea of using polysaccharides nano or micro level with polyolefins is the new of this work. Three compositions of polypropylene and commercial citrus pectin was prepared in proportions of 1, 3 and 5%. A coupling agent was used, the graphitized polypropylene with maleic anhydride to advance interaction between natural and synthetic particles. The obtaining of particles in nanometric scale pectin was made from colloid mill grinding. Some particles arrived near 100nm and majority the particles reached scales around 300nm. The structural analysis by X-ray diffraction and Fourier transform infrared spectroscopy demonstrated an interaction between maleic anhydride and pectin despite clusters of hydrophilic particles that were seen by scanning electron microscopy In the X-ray diffraction, the presence of crystals of sugars were detected. These crystals may have caramelized because processing temperatures are close to 200 C and were detected by colorimetry. Based on the mechanical data, it is possible realize that pectin had a plasticizing effect on the synthetic polymer, corroborating the rheological data and thermogravimetric tests, considering that the addition of higher amount of particles produces more thermal stability of the synthetic polymer.
Os estudos baseados na mistura de polímeros sintéticos com polímeros naturais têm se intensificado nos últimos tempos. A ideia de usar polissacarídeos em nano ou micro escala junto com poliolefinas é a novidade deste trabalho. Foram preparadas três composições de polipropileno e pectina cítrica comercial em proporções de 1, 3 e 5%. Foi utilizado um agente compatibilizante, o polipropileno grafitizado com anidrido maleico para favorecer a interação entre partículas naturais e as sintéticas. A obtenção de partículas em escala nanométricas de pectina foi feita partir de moagem em moinho coloidal e chegou próxima da faixa de 100nm, pois as partículas atingiram escalas em torno de 300nm. A análise estrutural feita por infravermelho e difração de raios-X demonstrou que houve interação entre o anidrido maleico e a pectina apesar dos aglomerados de partículas hidrofílicas que foram percebidos através da microscopia eletrônica de varredura. Também a partir dos dados de difração de raios-X, a presença de cristais de açúcares foram detectados, que por colorimetria podem ter se caralemizado devido temperaturas de processamento estarem próximas de 200ºC. A partir dos dados mecânicos, é possível perceber que a pectina teve um efeito plastificante no polímero sintético, corroborando com dados reológicos e com os testes termogravimétricos, considerando que quanto maior adição de partículas, maior a estabilidade térmica do polímero sintético.

Orientador: Carlos R. F. Grosso
Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos
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Resumo: Uma alternativa interessante na produção de filmes comestíveis com propriedades mecânicas e de permeabilidade melhoradas é a mimetização de estruturas biológicas como a parede celular e a cutícula dos tecidos vegetais por conterem na sua composição polissacarídeos, proteínas e lipídios. O objetivo do presente trabalho foi produzir e caracterizar filmes compostos de glucomanana, pectina, metilcelulose, gelatina e lipídios. O trabalho foi desenvolvido em três etapas: (1) produção de filmes a partir dos polissacarídeos: glucomanana, pectina e metilcelulose, (2) produção de filmes à base de polissacarídeos e gelatina em diferentes proporções e pHs e (3) produção de filmes à base de misturas de polissacarídeos/gelatina e lipídios: cera de carnaúba, ácidos graxos esteárico e palmítico, estearoil-2-lactil-lactato de sódio (SSL) e éster de sacarose (ES). Nesta última etapa, os lipídios foram incorporados na forma de emulsão (contendo todos os lipídios) e na forma de dispersão (contendo SSL ou ES). Os filmes foram caracterizados quanto às suas propriedades mecânicas, permeabilidade ao vapor de água (PVA), morfologia, solubilidade, absorção de água, opacidade e estrutura (infravermelho e raios X). Na primeira etapa foram obtidos filmes com propriedades mecânicas melhoradas a partir da mistura metilceluloseglucomanana- pectina na proporção 1:4:1, respectivamente. Estes filmes mostraram superfícies homogêneas sem separação de fases e um valor de PVA intermediário em relação às outras formulações. Também foram evidenciadas interações entre os polissacarídeos nesta mistura, através dos espectros de infravermelho e raios X. Na segunda etapa foram obtidos filmes com PVA reduzida a partir da mistura de polissacarídeos e gelatina nas proporções 90/10 e 10/90, respectivamente, em pH 5. Para estes filmes foram observados altos valores de absorção de água a 95% de umidade relativa em relação às outras formulações. A seção transversal dos filmes com PVA reduzida mostrou uma estrutura pouco compacta e em camadas, e as propriedades mecânicas não foram melhoradas significativamente. Na terceira etapa também foram obtidos filmes com PVA reduzida a partir da mistura polissacarídeo/gelatina com adição de lipídios, onde as dispersões não prejudicaram as propriedades mecânicas. Os filmes polissacarídeo/gelatina contendo as emulsões mostraram glóbulos de tamanhos variados dispersos na superfície, enquanto que, os produzidos com as dispersões apresentaram superfícies lisas, com microfuros e granulosidade. A opacidade aumentou significativamente em função do uso das emulsões, enquanto que, as dispersões provocaram mudanças pouco significativas. Filmes comestíveis com bom desempenho, ou seja, com altos valores de tensão na ruptura e elongação foram obtidos através da mistura dos polissacarídeos e; filmes com baixos valores de PVA foram obtidos a partir da combinação dos polissacarídeos com a gelatina, ou da combinação polissacarídeo/gelatina com os lipídios
Abstract: One interesting alternative in edible films production with improved mechanical properties and water vapor permeability is the mimic of biological structures like cell wall and cuticle of plant tissue by containing in their composition polysaccharides, proteins and lipids. The objective of this work was to produce and to characterize composite films of glucomannan, pectin, methylcellulose, gelatin and lipids. This work was developed in three stages: (1) films production from polysaccharides: glucomannan, pectin and methylcellulose, (2) films production from polysaccharides and gelatin in different ratios and pHs and (3) films production from mixture of gelatin/polysaccharides and lipids: carnauba wax, stearic and palmitic fatty acid, sodium stearoyl-2-lactylate (SSL) and sucrose ester (ES). In this last stage, lipids were added like emulsions (containing all lipids) and like dispersion (containing SSL or ES). The films were characterized by their mechanical properties, water vapor permeability (WVP), morphology, solubility, water absorption, opacity and structure (infrared spectroscopy and x ray). In the first stage, films with improved mechanical properties were obtained from methylcellulose-glucomannan-pectin mixture in the ratio of 1/4/1, respectively. These films showed homogeneous surfaces without phases separation and WVP intermediate values with regard to others formulations. Also, interactions were verifyed between the polysaccharides in this mixture through infrared spectroscopy and x ray. In the second stage, films with reduced WVP were obtained from mixture of gelatin/polysaccharides in the ratios of 90/10 and 10/90, respectively, in pH 5. For these films were observed high water absorption values at 95% relative humidity with regard to other formulations. The transversal section microscopy of films with reduced WVP showed a structure few compact and in layers, and the mechanical properties were improved significantly. In the third stage, films with reduced WVP were obtained from mixture of gelatin/polysaccharides and lipids, where the dispersions had not impaired the mechanical properties. The films polysaccharides/gelatin containing emulsions showed globules of different size dispersed in the surface, whereas, the ones containing the dispersions showed homogeneous surfaces with micro holes and granularity. The opacity increased significantly by use of emulsions, whereas, the dispersions caused few changes. Edible films with good performance, that is, with high tensile strength and elongation values were obtained through of polysaccharides mixtures; and films with low WVP values were obtained from the combination of polysaccharides with gelatin or the combination of polysaccharides/gelatin with lipids
Doutorado
Consumo e Qualidade de Alimentos
Doutor em Alimentos e Nutrição

A manga é uma das frutas tropicais mais produzida no mundo, sendo amplamente consumida in natura e processada. O seu processamento gera grande quantidade de resíduos, sendo 15 % a 20 % do seu peso representado pela casca. A casca da manga contém quantidades significativas de fitoquímicos, como os compostos fenólicos, os carotenoides e a pectina. Devido à sua composição química, rica em compostos benéficos à saúde, e à grande quantidade de resíduos gerados anualmente a casca da manga apresenta enorme potencial para ser utilizada como ingrediente funcional. Dessa forma, o objetivo deste trabalho foi estudar a extração sequencial de compostos fenólicos e pectina da casca da manga com o auxílio do ultrassom. O trabalho foi divido em duas etapas. A primeira etapa avaliou a extração dos compostos fenólicos através de um planejamento experimental 32. As variáveis independentes foram a concentração de etanol na solução aquosa de extração (25-75 %, v/v) e a potência do ultrassom (25-75 %). Os resultados mostraram que o ultrassom não afetou significativamente a extração dos compostos fenólicos. Visando reduzir a quantidade de solvente e energia gastas no processo de extração, o melhor rendimento (67 %) foi obtido com solução aquosa com 50 % de etanol, sem aplicação do ultrassom, e 8 minutos de processamento. A segunda etapa do trabalho teve como objetivo estudar a influência do ultrassom e da extração prévia dos compostos fenólicos na qualidade e rendimento da pectina. Os resultados demostraram aumento superior a 50 % no rendimento da pectina com a aplicação do ultrassom no resíduo da extração dos compostos fenólicos. A extração prévia dos compostos fenólicos não prejudicou o rendimento e a qualidade da pectina extraída da casca da manga demostrando que os compostos fenólicos e pectina podem ser extraídos da casca da manga com auxílio de uma tecnologia emergente.
Mango is an important tropical fruit consumed in fresh or processed form worldwide. Commercial processing of mango into juice, nectar, pulp, puree, and jam produces 15-20 % peel waste. Mango peel contains significant amounts of phytochemicals, like phenolic compounds, carotenoids and pectin, which makes it suitable to be processed for value-added applications in functional foods and nutraceuticals. Mango peel has enormous potential as a functional ingredient. Thus the aim of this work was to study the ultrasound technology potential for sequential extraction of phenolic compounds and pectin from this agroindustrial waste. The work was divided in two steps. The first step was to explore the phenolic compound extraction assisted by ultrasound using an experimental design (32). The independent variables were ethanol concentration (%) and ultrasound power intensity (%). The results showed that the ultrasound power intensity did not affect the phenolic compound content extracted. Aiming to reduce the amount of solvent and the spending energy, the best extraction yield (67 %) was obtained using 50 % of ethanol concentration, without ultrasound intensity and 8 minutes of experiment under stirring. In the second step, the aim was to investigate the potential of ultrasound intensity and the influence polyphenols removal on the extracted pectin quality. Results showed that extraction yield enhance over than 50 % when ultrasound (75 %) was used on the phenolic extraction residue and the pectin obtained a galacturonic acid content higher than 65 %. The phenolic extraction did not affect the quality of the pectic polymer extracted from mango peel. The results showed that the phenolic compounds and pectin from mango peel can be extracted using an emerging technology.

Rice (Oryza sativa) is cultivated in swampy geographical locations of tropical Nigeria, West Africa. Here it is infected by a host of fungal pathogens on the field or contaminated at postharvest. This has led to its loss and reduction in its production in both the national and global market. Lasiodiplodia theobromae and Rhizoctonia solani have recently been identified as the major fungal phytopathogens causing the deterioration of this grain on the field and at postharvest and affecting its production in Nigeria leading to gross capital loss. Hence the need to determine physiological control measures for the eradication of both phytopathogens on the field and at postharvest. In this study, tropical strains of Lasiodiplodia theobromae and Rhizoctonia solani obtained from deteriorated rice (Oryza sativa) were grown in a growth nutrient medium composed of MgSo4.7H20, K2HPO4, FeSO4.7H20, potassium nitrate and pectin at 30°C. Endo-Polygalacturonase activities were produced by the fungal isolates in the growth medium within ten days. The endo-polygalacturonases from both fungi were purified by a combination of ammonium sulphate precipitation, dialysis, gel filtration (on Sephadex G-100 column) and ion-exchange chromatography (on CM-Sephadex C-50 and CM-Sephadex C-25 columns). The molecular weight of endo-polygalacturonase from the Lasiodiplodia theobromae using Sephadex G-100 was estimated as 124,000 Daltons while that of the Rhizoctonia solani was estimated as 92,000 Daltons. The purified endo-polygalcuronase from the Lasiodiplodia theobromae exhibited optimum activity at 30°C and at pH 4.5 while that from the Rhizoctonia solani exhibited optimum activity at 32°C and at pH 5.0. The purified endo-polygalacturonases from both fungi exhibited optimum activities at 0.2% pectin concentration. They were stimulated by Ca2+ but inhibited by ethlylenediamine tetracetic acid (EDTA) and 2,4-dinitrophenol. The purified endo-polygalacturonase from the Lasiodiplodia theobromae lost 80% of its activity within 20 minutes of heat at 80°C. While the purified endo-polygalacturonase from the Rhizoctonia solani lost 82% of its activity within 20 minutes of heat at 80°C. Potassium nitrate as nitrogen source in the defined growth medium with pectin as carbon source supported highest activity of endo-polygalacturonase by the Lasiodiplodia theobromae while ammonium chloride as nitrogen source in the defined growth medium with pectin as carbon source supported highest activity of endo-polygalacturonase by the Rhizoctonia solani. In conclusion, the conditions inhibiting endo-polygalacturonases from Lasiodiplodia theobromae and Rhizoctonia solani capable of degrading the pectin portion of rice (Oryza sativa) can be adapted as feasible control measures limiting the infection and contamination of rice (Oryza sativa) by these phytopathogens on the field and at postharvest. Temperature and pH extreme from 30°C and pH 4.5 will be feasible inhibitory control measures for the growth of Lasiodiplodia theobromae on rice (Oryza sativa) in Nigeria while temperature and pH extreme from 32°C and pH 5.0 will inhibit growth of Rhizoctonia solani on the grain. These physiological conditions will preserve pectin in rice (Oryza sativa) from degradation by these two fungal phytopathogens.

Nowadays, people face many different dangers, such as stress, unsafety food, and environmental pollution, but not everyone suffers. Meanwhile, free radicals are the biggest threat for humans because they lead to over 80 different diseases composed of aging. Free radicals can only be eliminated or minimized with antioxidant foods or antioxidants. The chapter on the functional-antioxidant food presents the antioxidant functional food concept, the classification, the structure, and the extraction process of antioxidant ingredients. Various antioxidant substances such as protein (collagen), polysaccharides (fucoidans, alginates, glucosamines, inulins, laminarins, ulvans, and pectins), and secondary metabolites (polyphenols (phlorotannins, lignins, polyphenols), alkaloids, and flavonoids) also present. The production technology, the mechanism, the opportunity, and the challenge of antioxidants functional food also present in the current chapter. The current chapter also gives the production process of functional-antioxidant food composed of the capsule, the tablet, tube, the pills, the powder, and the effervescent tablet.

The grape berry is composed of skin, flesh (pulp) and seeds. After destemming (Chapter 13), the grapes are sent on for crushing. On crushing, the thick walls of the skin, including the waxy cuticle, are broken. Crushing the grapes (Figure 16.1) is a question of quantity. Small quantities are handled differently than large. The skins, including the contaminants thereon, as well as the majority of the materials discussed above for the individual grapes (i.e., phenols, anthocyanins, tanins, some acids, terpenes, pyrazines, and some carbohydrates including those attached to the anthocyanidins, forming anthocyanins) therein, are released. The cells of the pulp are also broken and released into the juice on crushing. This berry cell juice is mainly water (70–80% by weight) which contains the mixture of sugars (mostly glucose and fructose, but small concentrations of many other carbohydrates are also present), carboxylic acids (mostly tartaric and malic, but additional members of the tricarboxylic acid cycle, oxalic, glucuronic, etc. are also present), complex cross-linked polysaccharides from cell walls (pectins), some phenols and proteins (as well as the peptides and simple amino acids from which they are constructed), and minerals, including oxides of iron (Fe), phosphorus (P), and sulfur (S), as well as salts of potassium (K) and sodium (Na) brought up in the xylem to the growing berry. The seeds have their cellulose carbohydrate-based exterior coatings, which are also rich in complexed polyphenols (tannins). Additionally, amino acids, generally found as constituents of peptides, proteins, and enzymes, and their cofactors needed for all life, nucleic acids and their attached sugars needed for the next generation, are all present too. Thus, overall, the result of crushing the berries is a mixture consisting of skins, seeds, and fruit juice (the must = Latin vinum mustum = young wine). This mixture may, if the grapes were “white,” be cooled and the cap on the must—sometimes called the pomace (the solid portion of the must) removed early or late (usually between 12 and 24 hours) by the vintner. Most of the flavoring constituents are quickly extracted, and brightly colored phenols, tannins, anthocyanins, etc.