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See detailChemical composition analysis and structural features of banana rachis lignin extracted by two organosolv methods
Tiappi Deumaga, Mathias ULiege; villani, Nicolas; Aguedo, Mario et al

in Industrial Crops and Products (2019)

Two organosolv methods involving Formic acid/Acetic (FA) acid and Sulphuric acid/Ethanol (SE) solvent mixtures were investigated for lignin extraction from banana rachis biomass residues. Different ... [more ▼]

Two organosolv methods involving Formic acid/Acetic (FA) acid and Sulphuric acid/Ethanol (SE) solvent mixtures were investigated for lignin extraction from banana rachis biomass residues. Different heating methods were also applied during each extraction process, respectively direct conduction heating and microwave heating. The chemical composition and structural features of the extracted lignin fractions were further analyzed by ATRFTIR, TGA, elemental analysis and 13C NMR methods. SE extraction method showed a higher extraction yield (58.7%) and allowed also to obtain a lignin fraction with higher purity (76.5% Vs 71.0% for FA lignin). In addition, SE extraction method allowed a higher pulp yield which meant a better selectivity for lignin extraction thanks to the microwave heating method. SE lignin also showed a higher thermal stability due to its higher purity and higher density. The higher molecular weight found for FA lignin residues (7622.7g/mol Vs 5957.7g/mol for SEL) was suspected to be due to co-extracted carbohydrate residues bounded to extracted lignin macromolecules. These results allowed us to establish the SE extraction method (Sulphuric acid/Ethanol/water solvent with microwave heating) as effective for lignin extraction from banana rachis straw. [less ▲]

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See detailEssential oil chemical diversity of Tunisian Mentha spp. collection
Soilhi, Zayneb; Rhimi, Awatef; Heuskin, Stéphanie et al

in Industrial Crops and Products (2019), 131

Mints are perennial herbs that are cultivated for medicinal and aromatic purposes. They are highly polymorphic and their taxonomy is difficult. Sixty mint accessions, representing seven Mentha species (M ... [more ▼]

Mints are perennial herbs that are cultivated for medicinal and aromatic purposes. They are highly polymorphic and their taxonomy is difficult. Sixty mint accessions, representing seven Mentha species (M. aquatica L., M. longifolia L., M. piperita L., M. pulegium., M. rotundifolia L., M. spicata L. and M. spicata var. crispa 'moroccan'), were collected at full flowering from 51 Tunisian localities. Essential oil yields were found to vary from 0.45 to 2.5%, (w/w). Analyses of these oils by GC/FID and GC/MS and their subsequent classification by statistical analysis resulted in six clusters with significant variations in their terpenoid compositions: i) ulegone/isomenthone/ menthone; ii) isomenthone/pulegone; iii) menthone/pulegone ; iv) piperitenone oxide; v) linalool/ linalyl acetate/1,8 cineol/myrcene; and vi) carvone/limonene/1.8 cineol. M. pulegium accessions grouped two chemotypes: one rich in pulegone and the second rich in isomenthone. M. longifolia grouped one chemotype rich in pulegone and a second rich in menthone. M. spicata grouped one chemotypes characterized by a moderate to high carvone content and the second pulegone-rich. M. rotoundifolia accessions were piperitone oxide-rich. M. aquatica and M. piperita have linalool and linalyl acetate as major compounds. These results clearly indicate that there were a large biochemical diversity among the investigated Tunisian Mentha spp. accessions. Genetic and ecological diversities may explain this chemical diversity. [less ▲]

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See detailEffect of steam explosion treatment on chemical composition and characteristic of organosolv fescue lignin
Maniet, Guillaume ULiege; Schmetz, Quentin ULiege; Jacquet, Nicolas ULiege et al

in Industrial Crops and Products (2017), 99

Tall fescue, a grass currently grown as forage, presents a good potential as a feedstock in the developmentof biorefining. In this study, combination of steam explosion and an acetic/formic acid ... [more ▼]

Tall fescue, a grass currently grown as forage, presents a good potential as a feedstock in the developmentof biorefining. In this study, combination of steam explosion and an acetic/formic acid “organosolv”pretreatments are applied on raw fescue to optimize lignin extraction yields and obtain specific products.In a first step, fescue is pretreated by steam explosion under severity factors from 1.4 to 4.2. Thesetreatments allow hemicelluloses solubilization and open the lignocellulosic structure. Steam explodedsolid residues are then treated with an acetic acid (50%)/formic acid (30%)/water (20%) mixture. Extractedlignins are precipitated and characterized by size exclusion chromatography (SEC),31P NMR and HSQCNMR. Results show that acetic and formic acids extracted lignins present G, H and S units with ferulate andp-coumarate. Lignin typical linkages identified are of -O-4 and spirodienone substructures. Combinationof steam explosion and acetic and formic acid pretreatments increases extraction yields from 30% to100%. Moreover, an increase of the steam explosion treatment intensity induces chemical modificationsin lignin structure such -O-4 and spirodienone substructure degradations, increase of free COOH andphenolic OH bonds, decrease of aliphatic OH ferulate and p-coumarate bonds and changes in G/H/S unitsproportions. Steam explosion intensity affects also lignin molecular weights. [less ▲]

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See detailComprehension of an organosolv process for lignin extraction on Festuca arundinacea and monitoring of the cellulose degradation
Schmetz, Quentin ULiege; Maniet, Guillaume ULiege; Jacquet, Nicolas ULiege et al

in Industrial Crops and Products (2016), 94

It is commonly accepted that the current society needs to partially substitute fossil resources by renewable ones. Among many solutions, one approach consists in the development of biorefinery involving ... [more ▼]

It is commonly accepted that the current society needs to partially substitute fossil resources by renewable ones. Among many solutions, one approach consists in the development of biorefinery involving lignocellulosic biomass to produce bio-based materials and fuels. This study focuses on the comprehension of an organosolv treatment designed to break the complex lignocellulosic structure for high purity lignin extraction from tall fescue (Festuca arundinacea Schreb.). This grass benefits from an increasing interest in Western Europe and has been suggested as feedstock for biorefinery. However, its use as material for high purity lignin production has not been determined yet. Ethanol/water, 92/8% [v/v] with H2SO4 0.32 M was investigated at pilot scale under conventional heating (5 °C min−1 during 30 min and stabilized at 148 °C for 5 min). Precipitated lignin were analyzed as well as the composition of side-stream products (recovered cellulosic pulp and the aqueous hydrolysate). Lignin has been recovered at a purity level of 90% with a yield of 60%. The main contaminants were nitrogen containing compounds and degraded hemicelluloses. 2D-HSQC NMR (Two Dimension-Heteronuclear Single Quantum Correlation Nuclear Magnetic Resonance) revealed a co-extraction of ferulates and coumarates function as well as arabinoxylan. Cellulose was recovered at 53% purity with 60% yield. The conditions appear to be too harsh for tall fescue and led to significant amount of cellulose degradation. A process using a lower alcohol concentration will be developed to provide better yields of both cellulose and lignin. [less ▲]

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See detailUse of wheat bran arabinoxylans in chitosan-based films: Effect on physicochemical properties
Costa, Maria J.; Cerqueira, Miguel A.; Ruiz, Héctor A. et al

in Industrial Crops and Products (2015), 66

tThe aim of this work was to evaluate physicochemical properties of chitosan-based films with differentfractions of arabinoxylans (AXs). Five fractions composed by AXs or mixtures of AXs and arabino-xylo ... [more ▼]

tThe aim of this work was to evaluate physicochemical properties of chitosan-based films with differentfractions of arabinoxylans (AXs). Five fractions composed by AXs or mixtures of AXs and arabino-xylo-oligosaccharides (AXOS) obtained through three different processes were added to chitosan-based films.These films were obtained by solvent casting and characterized in terms of water vapor permeability(WVP), opacity, thickness, moisture content and mechanical properties (i.e., tensile strength – TS andelongation at break – EB), being the chemical interactions evaluated by FTIR.Moisture content values ranged between 20 and 30% for all five studied films being the lowest valueobserved for chitosan films with the fraction F1 of AX/AXOS (21.1%). The films with incorporation of F3a,F3b and F4 AXs fraction were more opaque (>10%) than the other studied films. Regarding mechanicalproperties CH films presented EB and TS values of 31.26% and 8.25 MPa, respectively, both these valuesremain statistically equal with the incorporation of AX/AXOS except for films containing the fractionF1 and F2. For films with the F2 fraction were obtained higher values of EB (41.31%) while for CH filmscontaining the F1 fraction the TS values (13.07 MPa) increased.In conclusion, wheat bran AXs can be successfully incorporated into chitosan-based edible films pro-viding, together with chitosan, an extra functional value to films, due their health benefits. [less ▲]

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See detailOak barks as raw materials for the extraction of polyphenols for the chemical and pharmaceutical sectors: a regional case study
Dedrie, Maxime; Jacquet, Nicolas ULiege; Bombeck, Pierre-Louis ULiege et al

in Industrial Crops and Products (2015), 70

Despite their potential for chemical recycling, residues from forest harvesting and wood processing are mostly used for industrial applications with low added value (energy, paper pulp, panels). Bark of ... [more ▼]

Despite their potential for chemical recycling, residues from forest harvesting and wood processing are mostly used for industrial applications with low added value (energy, paper pulp, panels). Bark of both oak species, Quercus robur L. 1753, Quercus petraea (Matt.) Liebl. 1784 is a by-product from sawmill and pulp mill activities. Bark is mainly used as a fuel for the same wood plants. The aim of this study is to look at the feasibility of enhancing the value of this material through the extraction of bioactive molecules such as polyphenols (i.e. catechin, gallic and ellagic acids). First, the effect of industrial storage of logs and bark on their polyphenol content was explored. Then, referring to the selection of tan oaks in the past, the question of an optimum harvesting age is addressed in order to maximize the polyphenol content of the barks. In the end, molecular diversity of bark is examined through the identification of molecules of interest, using different chromatographic analyses. The results show an effect of the industrial context and an effect of the raw material age on the chemical properties of the bark. First investigations also highlight molecules of interest and the molecular diversity, which needs to be further explored. [less ▲]

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See detailFast and high yield recovery of arabinose from destarched wheat bran
Aguedo, Mario ULiege; Vanderghem, Caroline ULiege; Goffin, Dorothée ULiege et al

in Industrial Crops and Products (2013), 43

Enzymatically destarched wheat bran (DWB) contained 13.8% of arabinose and 23.1% xylose. Up to a maximum of 70% of the arabinose was progressively released from DWB when heated at 80 or 100°C in media ... [more ▼]

Enzymatically destarched wheat bran (DWB) contained 13.8% of arabinose and 23.1% xylose. Up to a maximum of 70% of the arabinose was progressively released from DWB when heated at 80 or 100°C in media acidified with HCl. Whereas microwave irradiation at higher temperatures in pressure vessels could lead to higher yields of extraction. A Box-Behnken experimental design established an efficient model describing the effects of temperature, irradiation duration and pH on arabinose extraction. The pH appeared as the most important factor of the process. 4-5 min of microwave heating at 150ºC and pH 1 appeared as a fast and highly efficient method to recover more than 90% of the arabinose of DWB. When plotting the percentages of arabinose against the combined severity factors LogR’0 (calculated from the temperature/duration/pH conditions applied), two different fitting profiles were obtained for both the heating techniques. Under microwave heating, high free xylose’s release could also occur. The experimental design led to a quadratic model predicting the release of xylose from DWB. A range of conditions enabled to minimize xylose and hydrolyze around 50% of the total arabinose, yielding a high purity fraction. An alternative would be to release more than 90% of both arabinose and xylose, for further arabinose purification or for a common valorization of both pentoses. [less ▲]

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See detailEffects of extraction solvents on phenolic contents and antioxidant activities of Tunisian date varieties (Phoenix dactylifera L.)
Kchaou, W; Abbès, F; Blecker, Christophe ULiege et al

in Industrial Crops and Products (2013), 45

Second-grade dates (Phoenix dactylifera L.), with hard texture, from six Tunisian cultivars were analysed for their composition and antioxidant activities. Results showed predominance of total sugars and ... [more ▼]

Second-grade dates (Phoenix dactylifera L.), with hard texture, from six Tunisian cultivars were analysed for their composition and antioxidant activities. Results showed predominance of total sugars and a relatively low content of protein, fat andash. On the other hand, optimisation of extraction of antioxidant was carried using five different solvents. The highest level of phenolic compounds for all dates varieties was found in the 70% acetone extract. This level ranged from 199.43 to 576.48 mg of GAE/100 g fresh weight. However, extraction into 50% methanol gave the highest antioxidant activity from 89.55 to 109.67 mg equivalents of ascorbic acid/g fresh weight. For both two olvents, Bejo exhibited the highest phenolic content and total antioxidant activity, while Baydh El Hamam presented the owest. A positive linear correlation between total antioxidant activity and phenolic contents was observed (R2 = 0.83; R2 = 74 for acetone/H2O and methanol/H2O, respectively). The antioxidant activity of acetone/H2O and methanol/H2O extracts was carried using DPPH radical-scavenging activity and reducing power. These results showed that dates had strongly scavenging activity on DPPH reaching 90.12% in methanol/H2O from Deglet Nour. Whereas, acetone/H2O showed the best reducing power which Bejo was significantly higher than the other varieties. This study demonstrates the potential antioxidant activity with Tunisian date, that we can use these natural extracts as food additives in replacement of synthetic compounds. [less ▲]

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See detailEffect of processing conditions on phenolic compounds and antioxidant properties of date syrup
Abbès, F.; Kchaou, W.; Blecker, Christophe ULiege et al

in Industrial Crops and Products (2013), 44

Commercial hydrolytic enzymes (pectinase and cellulase) were investigated for their influence on phenolics and antioxidant activities of date syrup. Content of total phenolics, flavonoids and carotenoids ... [more ▼]

Commercial hydrolytic enzymes (pectinase and cellulase) were investigated for their influence on phenolics and antioxidant activities of date syrup. Content of total phenolics, flavonoids and carotenoids contents were determined spectrophotometrically. Polyphenols composition was examined using HPLC. Seven phenolic compounds (catechin, vanillic acid, caffeic acid, syringic acid, p-coumaric acid, ferulic acid and sinapic acid) were detected in all date syrup extracts. p-Coumaric acid was the major compound of all date syrup extracts, representing 49.223-63.397%. The antioxidant activity of date syrup was evaluated by various antioxidant assays, including total antioxidant, DPPH scavenging test, FRAP, hydrogen peroxide scavenging activity and metal chelating activity.Results showed that the date syrup prepared after extraction with pectinase and cellulase mixture gave the lowest phenolic and flavonoid contents. For same variety, date syrup prepared after extraction with pectinase and cellulase mixture gave the highest carotenoids amounts. The antioxidant activity, determined by several methods, was significantly affected by the extraction method as well as date varieties. In fact, the date syrup prepared after extraction with pectinase and cellulase mixture gave the lowest antioxidant activity. A good correlation between the antioxidant activity and total phenolic content and flavonoid was observed. The discovery of our research is very important to scientists as well as to the fruit-processing industry to produce juice and syrup with high antioxidant activity. © 2012 Elsevier B.V. [less ▲]

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See detailOptimization of formic/acetic acid delignification of Miscanthus ×giganteus for enzymatic hydrolysis using response surface methodology
Vanderghem, Caroline ULiege; Brostaux, Yves ULiege; Jacquet, Nicolas ULiege et al

in Industrial Crops and Products (2012), 35

A Box–Behnken experimental design and response surface methodology were employed to optimize the pretreatment parameters of a formic/acetic acid delignification treatment of Miscanthus ×giganteus for ... [more ▼]

A Box–Behnken experimental design and response surface methodology were employed to optimize the pretreatment parameters of a formic/acetic acid delignification treatment of Miscanthus ×giganteus for enzymatic hydrolysis. The effects of three independent variables, namely cooking time (1, 2 and 3 h), formic acid/acetic acid/water ratio (20/60/20, 30/50/20 and 40/40/20) and temperature (80, 90 and 107 ◦C) on pulp yield, residual Klason lignin content, concentration of degradation products (furfural and hydroxymethylfurfural) in the black liquor, and enzymatic digestibility of the pulps were investigated. The major parameter influencing was the temperature for pulp yield, delignification degree, furfural production and enzymatic digestibility. According to the response surface analysis the optimum conditions predicted for a maximum enzymatic digestibility of the glucan (75.3%) would be obtained using a cooking time of 3 h, at 107 ◦C and with a formic acid/acetic acid/water ratio of 40/40/20%. Glucan digestibility was highly dependent on the delignification degree. [less ▲]

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See detailSeed and juice characterization of pomegranatenext term fruits grown in Tunisia: Comparison between sour and sweet cultivars revealed interesting properties for prospective industrial applications
Hasnaoui, Nejib ULiege; Mars, Messaoud; Ghaffari, Sana et al

in Industrial Crops and Products (2011), 33(2), 374-381

Tunisian previous termpomegranatenext term genetic resources consist of sweet and sour cultivars, showing large morphometric variability. In the present work we characterized seeds and juice contents of ... [more ▼]

Tunisian previous termpomegranatenext term genetic resources consist of sweet and sour cultivars, showing large morphometric variability. In the present work we characterized seeds and juice contents of sugars and organic acids of 5 sour and 7 sweet previous termpomegranatenext term cultivars. Results showed that citric acid was predominant in sour previous termpomegranatesnext term, while malic acid was the most prevalent in sweet ones. Paradoxically, sour cultivars have higher sugar content than the sweet ones. A strong correlation was found between sourness and citric acid content, which is assumed to be the major factor that determines sour taste in previous termpomegranatenext term fruits. Besides, some of the seed parameters showed a significant positive correlation with acidity. Sweet cultivars were appropriate for fresh consumption and juice production due to several attributes in addition to their sweetness. Equally, sour previous termpomegranatenext term showed several characteristics that could be of great interest for food and nutraceutical industries. [less ▲]

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See detailNew developments on the ring opening polymerisation of polylactide
Jacobsen, Sven; Fritz, Hans-Gerhard; Degée, Philippe et al

in Industrial Crops and Products (2000), 11

Polylactides (PLA), biodegradable aliphatic polyesters, produced solely from renewable resources may substitute petrochemically based polymers in a broad range of applications in the near future, if we ... [more ▼]

Polylactides (PLA), biodegradable aliphatic polyesters, produced solely from renewable resources may substitute petrochemically based polymers in a broad range of applications in the near future, if we manage to produce them at lower cost and higher efficiency as nowadays. Possible applications include food packaging for meat and soft drinks, films for agro-industry and non-wovens in hygienic products. The authors developed, based on a new catalytic system, a reactive extrusion polymerisation process, which can be used to produce PLA continuously in larger quantities and at lower costs than before. This extrusion polymerisation process has been developed and tested with laboratory scale machines and the possibilities to extend this polymerisation process to lactide based blockcopolymers have been investigated. [less ▲]

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See detailApproach to the use of immobilizer sulfatase for analytical purposes and for the pràoduction of desulfo-glucosinolates
Wathelet, Jean-Paul ULiege

in Industrial Crops and Products (1998), 7

A commercial crude sulfatase from snail (Helix pomatia) was purified by ion exchange affinity, HPLC, gel-filtration chromatography. The enzyme isolated. which was ca. 37-folcl more active than the ... [more ▼]

A commercial crude sulfatase from snail (Helix pomatia) was purified by ion exchange affinity, HPLC, gel-filtration chromatography. The enzyme isolated. which was ca. 37-folcl more active than the commercial one was covalently immobilizcd on nyon 6.6 by the cross linking method. Immobilized sulfatase was usecl to produce some desulfo-glucosinolates (DSGLs) on the gram-scale. starting fiom glucotropaeolin. glucoraphenin ancl épiprogoitrin ancl for HPLC analyses of glucosinolates (GLs) containecl in cruciferous material and rapeseecl in particular. The immobilized enzyme as well as allowing the standarclization of the HPLC methocl for GLs analysis seems to be an efflcient system for producing DSGLs which are interesting starting materials to prepare bio-active structures through further chemical modilications. [less ▲]

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