Chitosan-based magnetite nanocomposites were synthesized using a versatile ultrasound assisted in situ method involving one quick step. This synthetic route approach results in the formation of spheroidal nanoparticles (Fe3O4) with average diameter between 10 and 24nm, which were found to be superparamagnetic with saturation magnetization (Ms) ranges from 32-57emug(-1), depending on the concentration. The incorporation of Fe3O4 into chitosan matrix was also confirmed by FTIR and TG techniques. This hybrid nanocomposite has the potential application as electrochemical sensors, since the electrochemical signal was excepitionally stable. In addition, the in situ strategy proposed in this work allowed us to synthesize the nanocomposite system in a short time, around 2min of time-consuming, showing great potential to replace convencional methods. Herein, the procedure will permit a further diversity of applications into nanocomposite materials engineering.
In this communication, lipase A from Candida antarctica (CALA) was immobilized by covalent bonding on magnetic nanoparticles coated with chitosan and activated with glutaraldehyde, labelled CALA-MNP, (immobilization parameters: 84.1% ± 1.0 for immobilization yield and 208.0 ± 3.0 U/g ± 1.1 for derivative activity). CALA-MNP biocatalyst was characterized by X-ray Powder Diffraction (XRPD), Fourier Transform Infrared (FTIR) spectroscopy, Thermogravimetry (TG) and Scanning Electron Microscope (SEM), proving the incorporation of magnetite and the immobilization of CALA in the chitosan matrix. Besides, the immobilized biocatalyst showed a half-life 8–11 times higher than that of the soluble enzyme at pH 5–9. CALA showed the highest activity at pH 7, while CALA-MNP presented the highest activity at pH 10. The immobilized enzyme was more active than the free enzyme at all studied pH values, except pH 7.
Residual oil from babassu (Orbignya sp.), a low-cost raw material, was used in the enzymatic esterification for biodiesel production, using lipase B from Candida antarctica (Novozym® 435) and ethanol. For the first time in the literature, residual babassu oil and Novozym® 435 are being investigated to obtain biodiesel. In this communication, response surface methodology (RSM) and a central composite design (CCD) were used to optimize the esterification and study the effects of four factors (molar ratio (1:1–1:16, free fatty acids (FFAs) /alcohol), temperature (30–50 °C), biocatalyst content (0.05–0.15 g) and reaction time (2–6 h)) in the conversion into fatty acid ethyl esters. Under optimized conditions (1:18 molar ratio (FFAs/alcohol), 0.14 g of Novozym® 435, 48 °C and 4 h), the conversion into ethyl esters was 96.8%. It was found that after 10 consecutive cycles of esterification under optimal conditions, Novozym® 435 showed a maximum loss of activity of 5.8%, suggesting a very small change in the support/enzyme ratio proved by Fourier Transform Infrared (FTIR) spectroscopy and insignificant changes in the surface of Novozym® 435 proved by scanning electron microscopy (SEM) after the 10 consecutive cycles of esterification.
In this work, chitosan/magnetite nanoparticles (ChM) were quickly synthesized according to our previous report based on co-precipitation reaction under ultrasound (US) irradiation. Besides ChM was in-depth structurally characterized, showing a crystalline phase corresponding to magnetite and presenting a spheric morphology, a “nanorod”-type morphology was also obtained after increasing reaction time for eight minutes. Successfully, both morphologies presented a nanoscale range with an average particle size of approximately 5–30 nm, providing a superparamagnetic behavior with saturation magnetization ranging from 44 to 57 emu·g−1. As ChM nanocomposites have shown great versatility considering their properties, we proposed a comparative study using three different amine-based nanoparticles, non-surface-modified and surface-modified, for removal of azo dyes from aqueous solutions. From nitrogen adsorption–desorption isotherm results, the surface-modified ChMs increased the specific surface area and pore size. Additionally, the adsorption of anionic azo dyes (reactive black 5 (RB5) and methyl orange (MO)) on nanocomposites surface was pH-dependent, where surface-modified samples presented a better response under pH 4 and non-modified one under pH 8. Indeed, adsorption capacity results also showed different adsorption mechanisms, molecular size effect and electrostatic attraction, for unmodified and modified ChMs, respectively. Herein, considering all results and nanocomposite-type structure, ChM nanoparticles seem to be a suitable potential alternative for conventional anionic dyes adsorbents, as well as both primary materials source, chitosan and magnetite, are costless and easily supplied.
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