Effect of extraction procedures on the chemical structure, antitumor and anticoagulant properties of ulvan from Ulva lactuca of Tunisia coast.

The effect of extraction procedures on chemical composition, structural, antitumor and anticoagulant properties of the sulphated polysaccharide 'ulvan' from the green seaweed Ulva lactuca were investigated. The structural features of ulvans were carried out by FTIR and by one- and two- dimensional 1H and 13C NMR spectroscopic. The ulvans were mainly composed of rhamnose, xylose, and uronic acid. Chemical and spectroscopic analyses demonstrated that ulvans were constituted of (1→4)-ß-glucuronic acid, (1→3,4)-α-L-rhamnose-3-sulphate and (1→4)-α-xylose. The extraction procedures effect were observed in chemical structure, Mw and biological activities. Cytotoxic activity of enzymatic-chemical extract on cervical cancer cells (HeLa) (IC50 = 1000 µg/mL) was higher than on normal peripheral blood lymphocytes cells (PBL). Acid extracts promoted to reduce HeLa cells and to grow PBL cells. At high concentrations, acid extracts showed the highest APTT and TT clotting time. Antitumoral and anticoagulant activities of ulvans from Ulva lactuca promote their use as effective therapeutic agent.

Smart ulvan films responsive to stimuli of plasticizer and extraction condition in physico-chemical, optical, barrier and mechanical properties.

Smart films were produced with ulvan extracted from the green seaweed Ulva. lactuca at different extraction conditions, by varying the glycerol or sorbitol in specific plasticizer concentration. Chemical composition and molecular weight characteristics of ulvans were carried out by GLC and HPSEC analysis, respectively. Regardless of the extraction procedure, the investigation revealed that ulvans were selected as reproducible and suitable materials of stimuli-responsive due to its peculiar chemical composition and self-aggregation molecular behavior. When using the terminology of stimuli-responsive system, we declare that the physico-chemical, barrier, optical, and mechanical characteristics of ulvan films system are strongly responsive to extraction conditions and to plasticizer type and concentration. As plasticizer concentration increased, thickness, moisture content (MC), water solubility, water vapor permeability (WVP), transparency, elongation at break (EAB), usually UV and visible light protection of ulvan films increased, while, their tensile strength (TS) decreased significantly. The films prepared with glycerol exhibited better solubility, transparency and mechanical properties, than those with sorbitol. However, the films formed with sorbitol had the greatest moisture resistance and more effective vapor, visible and UV light barrier as well as the lowest solubility. The FTIR spectra evidenced the expected outcome of the chemical interaction and miscibility kind between polysaccharides and plasticizers.

Effects of extraction procedures and plasticizer concentration on the optical, thermal, structural and antioxidant properties of novel ulvan films.

Active films were produced with sulphated polysaccharides "ulvan", extracted from the green seaweed Ulva lactuca with different extraction procedures, by varying the glycerol or sorbitol plasticizer concentration at 1% and 2% (w/v). The surface charge and glass transition temperature (Tg) of ulvans were carried out by zeta (ζ)-potential and DSC analysis, respectively. The investigation revealed that ulvans were anionic stable polymers and they had great Tg values. Regardless of the extraction procedure, ulvans can give successful films formulations. However, the optical, thermal, structural and antioxidant characteristics of ulvan films were strongly affected by extraction conditions and by the variation of the type and concentration of plasticizer. In general, as plasticizer concentration increased, ferrous chelating activity and compact structure increased as well, while, Tg, lightness and DPPH radical-scavenging activity decreased. Interestingly, the films plasticized with glycerol exhibited better compact structure, more negative temperature of transition, and greater free radical scavenging ability than with sorbitol. However, the films prepared with sorbitol had the highest L* values and chelating ability. The current study revealed a high correlation between zeta (ζ)-potential of ulvans and their Tg (R2 = 0.98), as well as with scavenging activity of ulvan films (R2 = 0.8-0.99).

Effect of extraction procedures on structural, thermal and antioxidant properties of ulvan from Ulva lactuca collected in Monastir coast.

The present work aims to evaluate the effect of an acid extraction as well as a combined enzymatic-chemical extraction on structural, thermal and antioxidant properties of the sulphated polysaccharide 'ulvan' from the green seaweed Ulva lactuca. Structural characterization by FTIR and NMR spectroscopies showed the typical peaks of ulvan, namely, uronic acids, rhamnose and sulphate. FTIR analysis revealed that the extraction procedures were able to maintain ulvan structure. Despite differences in the extraction procedures, 13C NMR spectra were globally similar, proving a comparable chemical structure of ulvans. A major difference has been observed in signal intensity which reflected the resonance of glucose or xylose. Thermal characterization proved that ulvans were thermally stable until approximately 180°C. Antioxidant properties of ulvans were evaluated in vitro through different antioxidant assays. Ulvan, which is extracted at pH 1.5 and 90°C, exhibited the greatest scavenging activity (IC50=13.56µg/ml) towards DPPH radical. Result indicated that Mw has influenced inhibitory effect on DPPH radical of ulvan. The current study revealed also a high correlation between sulphate contents of ulvans and their reducing power (R2=-0.89) and their metal scavenging activity (R2=0.97). Overall, ulvans have peculiar structural, thermal and antioxidant properties which promote their use in food or pharmaceutical products as natural ingredient.

Effect of extraction conditions on the yield and purity of apple pomace pectin precipitated but not washed by alcohol.

A study of the influence of extraction conditions (pH: 1.5 to 2; temperature: 80 to 90 degrees C; extraction time: 1 to 3 h), on the yield and purity of apple pomace pectin without elimination of impurities by alcohol washing was carried out. The alcohol precipitate yields varied from 2.9% to 8.9% depending on the pH. At pH 1.5, these yields were higher than those obtained at pH 2 contrary to the galacturonic acid purity (%w/w). Compounds other than pectins were solubilized from the cell walls of apple pomace at pH 1.5, and they were precipitated with alcohol. The apple pectins obtained from the different extraction procedures were highly methylated (54.5% to 79.5%), especially when the conditions (temperature, pH) were drastic. Similar conclusions can be drawn for the neutral sugar content that decreased at pH 1.5 (arabinose, xylose, and galactose) or at the highest temperatures and extraction times (arabinose and galactose). The phenomenon of demethylation and pectin degradation of neutral sugars chains can be observed at acid pH, and for long extraction times. The presence of high quantities of mannose or fructose, glucose, and xylose in the alcohol precipitate showed that pectin precipitation with ethanol was not specific.

New method for a two-step hydrolysis and chromatographic analysis of pectin neutral sugar chains.

A new method for the determination of the main neutral sugars in pectin has been developed. The sample preparation involves a mild chemical attack followed by an enzymatic hydrolysis. The completeness and nondestructive character of the method are demonstrated by comparison of the results obtained with different acids such as H2SO4, HCl, and trifluoroacetic acid (TFA) at different concentrations (2, 1, or 0.2 M) at two temperatures (80 or 100 degrees C). The chemical hydrolysis of pectin neutral sugar chains with strong acid (1 or 2 M) and high temperature (100 degrees C) shows that the liberation of the pectin sugars is not realized at the same rate for each sugar. Different optimum conditions are thus obtained. However, the chemical pectin hydrolysis with 0.2 M TFA at 80 degrees C is characterized by the liberation of pectin neutral sugar side chains without any degradation within 72 h of hydrolysis. Under these conditions, the liberation of some pectin sugars, essentially galactose, glucose, and rhamnose, was not complete. An enzymatic hydrolysis is necessary to obtain a complete release of all the sugars. The combination of the two treatments, a chemical hydrolysis realized with diluted acid (0.2 M) for 72 h at low temperature (80 degrees C) on one hand and an enzymatic hydrolysis on the other hand, allow a total liberation of pectin sugars. The quantitative analysis of the carbohydrates is realized with accuracy, high selectivity, and sensitivity with high-performance anion-exchange chromatography with pulsed-amperometric detection. The sugars can be analyzed without any derivatization with a limit of quantification of 0.1 mM.