Nuclear Magnetic Resonance and Calorimetric Investigations of Extraction Mode on Flaxseed Gum Composition.

We discussed about the influence of extraction mode on the flaxseed gums composition and their thermal stabilities. In order to do so, flaxseed gum was extracted by both classical magnetic stirring method and ultrasonic-assisted extraction (UAE). As a function of time, protein content, gum yield, pH values were evaluated and samples were characterized by 1H and 13C nuclear magnetic resonance (NMR) experiments as well as scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The flaxseed gum extracted in aqueous solution correspond to a mixture of different components, including polysaccharides, proteins and sometimes lignan derivatives. It is found that the protein and gum contents increase with the extraction duration for both the ultrasonic assisted and the traditional extraction while the pH decreases at the same time. As expected, compared to traditional magnetic stirring method, ultrasonic assisted extraction method can significantly enhance the yield of polysaccharides, lignans and proteins. The variation of pH is correlated to the increase of lignan molecules in the extracted samples. For thermic methods, SEM experiments showed that lignan derivatives which ester-bonded to polysaccharides associated to proteins are responsible to the formation of globular aggregates. Supplementary rod-like molecular organization were obtained from UAE and questions on the nature of the amphiphilic mesogen carbohydrate structures.

Mixed Oxides Issued from Hydrotalcite Precursors for Toluene and CO Total Oxidation: Comparison of Preparation Method.

Catalytic total oxidation is an effective technique for the treatment of industrial VOCs. This emission is generally accompanied by the presence of other products like CO, NOx or other VOC. In this paper, the development of catalysts for the total oxidation of CO and toluene mixture is performed. For this study, Mg6Al2HT hydrotalcites precursors were synthesized by three different methods: co-precipitation, microwaves and ultrasound assisted method. Hydrotalcite precursors have been used in order to develop mixed oxides after calcination for the catalytic oxidation test. Hydrotalcite structure as well as the mixed oxides obtained after calcination was studied, by several techniques: XRD, TEM, DTA/TG, BET, N2 sorption, H2-TPR. The physico chemical studies revealed modification in the structural characteristics (surface area, porosity) as well as in reducibility properties of the formed mixed oxides. The nanocatalyst issued from microwaves synthesis was the most active in these studied reactions for the total oxidation of the mixture. Moreover, addition of CO on the reaction mixture allows obtaining a beneficial effect on the toluene oxidation.

Efficient synthesis of 4-substituted-ortho-phthalaldehyde analogues: toward the emergence of new building blocks.

4-Methoxy-ortho-phthalaldehyde and 4-hydroxy-ortho-phthalaldehyde are potentially useful molecules for fluorimetric analysis of a variety of amines and for the elaboration of complex molecular architectures. Nevertheless, literature generally describes their synthesis in very low yield (below 5%), mainly due to the inefficiency of the last oxidation step. In this paper, we report a reliable synthesis of 4-substituted-ortho-phthalaldehyde analogues in 51% overall yield owing to the addition of a protecting step of the unstable key intermediate 4,5-dihydroisobenzofuran-5-ol. Oxidation and deprotection steps were also studied in order to provide an effective availability of these two dialdehyde compounds that may increase their future applications.

Cyclodextrins: A promising drug delivery vehicle for bisphosphonate.

Bisphosphonates are well established pharmaceutical drugs with wide applications in medicine. Nevertheless, the side chain and the nature of phosphorous groups could induce a poor aqueous solubility and act on their bioavailability. At the same time, cyclodextrins are cage molecules that facilitate transport of hydrophobic molecules to enhance the intestinal drug absorption of these molecules by forming inclusion complexes. Here we demonstrate that cyclodextrins could be used as a bisphosphonate carrier. The formation of cyclodextrins-bisphosphonate complexes was characterized by 1D and 2D NMR spectroscopy, Isothermal Titration Calorimetry and UV-vis spectroscopy. The results revealed that only the side chain of bisphosphonate was involved in the inclusion phenomenon and its length was a crucial parameter in the control of affinity. Findings from this study suggest that cyclodextrin will be a useful carrier for bisphosphonates.

Recognition of iron ions by carbazole-desferrioxamine fluorescent sensor and its application in total iron detection in airbone particulate matter.

This work reports on an efficient microwave irradiation synthesis of a new fluorescent chemosensor based on desferrioxamine B (DFO-B) and carbazole moiety. Furthermore, this novel chemosensor was employed for a comparative study of real environmental samples of airbone particulate matter collected from Dunkirk (Northern of France). Among selected relevant metal cations present in its airbone particulate matter, such as Na(+), K(+), Mg(2+), Ca(2+), Al(3+), Cr(3+), Mn(2+) and Zn(2+), this molecular device proved to be outstandingly sensitive toward Fe(3+) with a limit of detection of 1.49 ppb (2.1×10(-8) M) in methanol allowing the estimation of total iron in atmospheric particles.

Polydisperse methyl ß-cyclodextrin-epichlorohydrin polymers: variable contact time (13)C CP-MAS solid-state NMR characterization.

The polymerization of partially methylated ß-cyclodextrin (CRYSMEB) with epichlorohydrin was carried out in the presence of a known amount of toluene as imprinting agent. Three different preparations (D1, D2 and D3) of imprinted polymers were obtained and characterized by solid-state (13)C NMR spectroscopy under cross-polarization magic angle spinning (CP-MAS) conditions. The polymers were prepared by using the same synthetic conditions but with different molar ratios of imprinting agent/monomer, leading to morphologically equivalent materials but with different absorption properties. The main purpose of the work was to find a suitable spectroscopic descriptor accounting for the different imprinting process in three homogeneous polymeric networks. The polymers were characterized by studying the kinetics of the cross-polarization process. This approach is based on variable contact time CP-MAS spectra, referred to as VCP-MAS. The analysis of the VCP-MAS spectra provided two relaxation parameters: T CH (the CP time constant) and T 1ρ (the proton spin-lattice relaxation time in the rotating frame). The results and the analysis presented in the paper pointed out that T CH is sensitive to the imprinting process, showing variations related to the toluene/cyclodextrin molar ratio used for the preparation of the materials. Conversely, the observed values of T 1ρ did not show dramatic variations with the imprinting protocol, but rather confirmed that the three polymers are morphologically similar. Thus the combined use of T CH and T 1ρ can be helpful for the characterization and fine tuning of imprinted polymeric matrices.

Synthesis and inclusion ability of anthracene appended ß-cyclodextrins: unexpected effect of triazole linker.

A new fluorescent ß-cyclodextrin has been synthesized by coupling an anthracene moiety to the cyclic oligosaccharide via click chemistry. The influence of the triazole spacer was compared to the simple amino and amido linkers. While a sensing ability toward adamantan-1-ol was observed with the latter two spacers, the absence of inclusion capacity prevents the triazole modified cyclodextrin from showing any fluorescence variations. The difference in the binding behaviors studied by Isothermal Titration Calorimetry, UV-vis and fluorescence spectroscopies, was highlighted by the NOESY NMR spectra of the modified cyclodextrins: whereas a free cavity was observed for the amino and amido linkers, an important obstruction was obtained in the case of the triazole.