Synthesis and characterization of cellulose acetate from royal palm tree agroindustrial waste

This study provides a novel value‐added utilization of the agroindustrial waste of royal palm tree leaf sheath to produce cellulose acetate. One of the motivations of this work was the fact that Brazil is one of the largest heart of palm producers in the world. However, as a result of extraction and processing, tons of waste are generated and discharged to the environment. Such waste is rich in lignocellulosic material, which could be reused to obtain derivatives of interest and commercial value. The synthesis of cellulose acetate was performed through a homogeneous acetylation reaction. Three different conditions were tested for delignification of the raw material, which resulted in a reduction in lignin content from 17.75 to 7.72%. The highest yield of cellulose acetate reached 99.5%, with degree of substitutions ranging between 2.08 and 2.82, which indicates satisfactory conversion. The Fourier transform infrared spectrum showed that practically all hydroxyl groups were replaced by acetate groups; this was also confirmed by nuclear magnetic resonance analysis. X‐ray diffraction analysis showed that the cellulose acetate crystallinity index was 8.9%. This demonstrates the viable potential of cellulose acetate production with low cost and use of highly available agroindustrial waste. POLYM. ENG. SCI., 59:891–898, 2019. © 2018 Society of Plastics Engineers     

Absence of ferromagnetism in ferroelectric Mn-doped BaTiO3 nanofibers

Pure and Mn-doped barium titanate nanofibers were synthesized by the electrospinning method. The morphology, microstructure and crystal structure of as-spun and annealed composite nanofibers were characterized by scanning electron microscopy and transmission electron microscopy. After annealing at 850°C, we obtain nanofibers a few μm long, formed by nanoparticles of irregular shape with sizes around 100 nm. X-ray diffraction and Raman spectroscopy show that a partial phase transition from tetragonal to hexagonal takes place for BaTi_0.90Mn_0.10O₃. Vibrational phonon modes were calculated for BaTiO₃ within the density functional theory (DFT) framework. Ferroelectricity has been probed on pure and Mn-doped BaTiO₃ nanofibers, by means of piezoresponse force microscopy in an atomic force microscope, confirming the polar domain switching behavior of the fibers. The measured piezoelectric coefficient d₃₃ were 31 and 22 pm/V for BaTiO₃ and BaTi_0.90Mn_0.10O₃. Magnetic properties of the samples were probed in a superconducting quantum interference device. Diamagnetic and paramagnetic behaviors were found in pure and Mn-doped samples, respectively.     

Examination of organic coatings on metallic substrates by scanning electrochemical microscopy in feedback mode: Revealing the early stages of coating breakdown in corrosive environments

Scanning electrochemical microscopy in feedback mode was used to monitor changes in the surface state of a polymeric film applied on a metallic substrate when exposed to an aqueous electrolytic environment. The protected metal consisted of a carbon steel substrate coated with a polyurethane-based polymeric film. SECM measurements performed in the presence and absence of chloride anions permitted a specific effect caused by Cl⁻ anions at early exposures to be detected. Significant surface roughening is observed for immersion times shorter than 1 day when the electrolyte contains chloride ions. Additionally, the growth of an individual blister could also be investigated.     

Adsorption and photocatalytic degradation of phenol and 2,4 dichlorophenoxiacetic acid by Mg–Zn–Al layered double hydroxides

Mg–Zn–Al layered double hydroxides (LDHs) with varying amounts of zinc were prepared by the coprecipitation method. Solids were analyzed by XRD and N₂ physisorption, confirming the formation of pure LDH phase; and the production of mixed oxides with high specific surface areas (182–276 m² g⁻¹) after calcination. Band gap energy was also determined, presenting the expected decreasing tendency on increasing zinc amounts. These mixed oxides were tested both for the adsorption of 2,4 dichlorophenoxiacetic acid (2,4-d) and for the photocatalytic degradation of 2,4-d and phenol. Nearly total (97%) degradation of initial 1.45 mmol L⁻¹ of 2,4-d, with 1 g calcined LDH per liter, was accomplished in 9 h, while phenol half-life was as short as 3.5 h, with the catalyst with lowest zinc amount (5 wt.%). Langmuir adsorption isotherms are presented. Solids were also characterized by XRD and FTIR analysis after photocatalytic and adsorption activity, to determine the presence of 2,4-d. The versatility of LDH decomposition products in the elimination of different contaminants by different mechanisms puts them forward as a viable alternative for environmental remediation.     

Evolution of the nutritional status of Chilean children from preschool to school age: anthropometric results according to the source of the data

Because the results of the nutritional status released by Chilean institutions which collect anthropometric data on their population under control, show different increments in the prevalence of obesity between preschoolers and children in 1st grade, we decided to verify the real magnitude of this increase. This study is based on a longitudinal investigation which began in 2006 and included 1100, three-year old children, which we evaluated when they were 4, 5 and 6 y. The nutritional status was determined according to BMI Z and WHO References 2006/2007. The information was also used to determine the concordance between the anthropometric data collected on first graders by teachers from public schools in 2009 (JUNAEB data set) and the same children assessed in parallel by INTA (INTA data set). The sample included 474, six-year olds. No differences were found between the average BMI Z and HAZ of the two data sets, and the degree of concordance between the BMI Z's was good (rho = 0.73), however there were differences in the nutritional status, since the prevalence of low weight was significantly greater when assessed with JUNAEB's data (9.5% vs. 3.6% ), while that for obesity was lower with INTA's data, 17.5% vs. 19.2% (not significantly different). At 4 and 5 y, obesity prevalence of the children was 13.3% and 15.7% respectively (INTA's data). Considering the observed nutritional trajectory, it is likely that the rise in obesity between 4 and 6 y of age, was 4 percentage points and not 6, as was determined with INTA's data.     

Effects of Seed Color and Growing Locations on Fatty Acid Content and Composition of Two Chia (Salvia hispanica L.) Genotypes

The objective of this study was to investigate the effect of chia (Salvia hispanica L.) seed coat color on oil content and fatty acid composition, as well as the effect of different growing areas on chemical variation. This study was carried out using white and black-spotted chia seeds grown together at five locations of Ecuador. Oil content was not significantly (P < 0.05) different for any of the comparative analyses performed between white and black-spotted seeds at all, although significant differences in oil content among locations were detected. The seeds from the San Pablo location showed the highest oil concentration (34.5%). No significant differences among fatty acids at any of the location were detected between white and black-spotted seeds; however, significant differences in fatty acids composition between sites were found. Overall, significant (P < 0.05) differences in palmitic, oleic, linoleic, and α-linolenic fatty acid compositions among oils from seeds grown in different locations were detected. In conclusion, this paper shows that the larger differences found in oil content and fatty acid composition are due to location (because of the environmental differences) rather than chia seed coat color.     

Rare Glutamic Acid Methyl Ester Peptaibols from Sepedonium ampullosporum Damon KSH 534 Exhibit Promising Antifungal and Anticancer Activity

Fungal species of genus Sepedonium are rich sources of diverse secondary metabolites (e.g., alkaloids, peptaibols), which exhibit variable biological activities. Herein, two new peptaibols, named ampullosporin F (1) and ampullosporin G (2), together with five known compounds, ampullosporin A (3), peptaibolin (4), chrysosporide (5), c(Trp-Ser) (6) and c(Trp-Ala) (7), have been isolated from the culture of Sepedonium ampullosporum Damon strain KSH534. The structures of 1 and 2 were elucidated based on ESI-HRMSⁿ experiments and intense 1D and 2D NMR analyses. The sequence of ampullosporin F (1) was determined to be Ac-Trp¹-Ala²-Aib³-Aib⁴-Leu⁵-Aib⁶-Gln⁷-Aib⁸-Aib⁹-Aib¹⁰-GluOMe¹¹-Leu¹²-Aib¹³-Gln¹⁴-Leuol¹⁵, while ampullosporin G (2) differs from 1 by exchanging the position of Gln⁷ with GluOMe¹¹. Furthermore, the total synthesis of 1 and 2 was carried out on solid-phase to confirm the absolute configuration of all chiral amino acids as L. In addition, ampullosporin F (1) and G (2) showed significant antifungal activity against B. cinerea and P. infestans, but were inactive against S. tritici. Cell viability assays using human prostate (PC-3) and colorectal (HT-29) cancer cells confirmed potent anticancer activities of 1 and 2. Furthermore, a molecular docking study was performed in silico as an attempt to explain the structure-activity correlation of the characteristic ampullosporins (1–3).     

Bacterial inactivation and organic oxidation via immobilized photo-Fenton reagent on structured silica surfaces

A woven inorganic silica fabric loaded with Fe-ions (EGF-Fe) was tested under simulated solar light during hydroquinone degradation. The abatement of hydroquinone was observed to attain about 80% within 3 h. The photo-catalyst was also tested to inactive Escherichia coli K12 at “natural” pH and in the presence of a low concentration of H₂O₂. Addition of H₂O₂ (10 mg L⁻¹) did not by itself to bacterial inactivation. Total bacterial inactivation was mediated by EGF-Fe fabrics in the presence of H₂O₂ (10 mg L⁻¹) under solar light irradiation. A sample containing active (culturable) bacteria (10⁵ CFU mL⁻¹) decreased to values <1 CFU mL⁻¹ within 3 h reaction. Fe-mediated homogeneous process decreased the bacterial CFU content by about two orders of magnitude within 4 h. During the degradation of hydroquinone only a small amount of iron ions were found in solution of about 1.2 mg L⁻¹, within 90 min decreasing to values ≤0.5 mg L⁻¹ after 180 min. The leaching of Fe-ions did not affect the photo-catalyst performance since EGF-Fe fabric did not deactivate after five or more cycles. The Fe-ions founds in solution mineralized hydroquinone to levels below 37% of its initial content. The present study presents the first report on the beneficial role of a heterogeneous iron supported catalyst leading to efficient bacterial inactivation in aqueous solution with iron leaching <0.1 mg L⁻¹, the detection limit for Fe-analysis in solution. No bacterial re-growth was observed during a post-irradiation period up to 24 h in the dark.     

Synthesis and Properties of Novel Antifungal Gemini Compounds Derived from <Emphasis Type="Italic">N</Emphasis>-Acetyl Diethanolamines

A series of new N-acetylated non-ionic and cationic gemini surfactants (3a–f) having dimeric structures derived from primary and tertiary amines with variably long tails (C₈–C₁₂–C₁₈) were synthesized. In addition, N-acetylated monomeric analogues 6a and 6b were prepared and their antifungal potency and surface properties were also determined. Critical micelle concentration (CMC), effectiveness of surface tension reduction (γ_CMC), surface excess concentration (Γ), and area per molecule at the interface (A) were also determined and the resulting values indicate that the cationic series is characterized by good surface-active and self-aggregation properties. For the first time, all surfactants were tested to evaluate their antifungal properties using the method for the broth macrodilution test (M27-A2, NCCLS). Four microbial strains were used to perform the study: Candida parapsilosis (ATCC 22019), C. albicans (ATCC 64548), and a wild-type strain of C. parasilosis and Saccharomyces cerevisiae (ATCC 9763). The antimicrobial activity was measured by yeast growth inhibition expressed as minimum inhibitory concentration (MIC) values. Results were compared to those obtained for their monomeric analogues and for a commercially available reference compound (Fluconazole). Gemini 3b, 3e and 3f were found to be the most potent compounds. The results show S. cerevisiae as the most sensitive strain. In contrast, the wild strain of C. parapsilosis was resistant.