NMR-study of the stereochemistry and dynamic behaviour of thioacrylamides

Several model thioacrylamides, Me₂N CH = C(R) C(S) NMe₂ (R = H, Ph — 2a, b ) and (p)MeO C₆H₄ NH CHC(R) C(S) NMe₂ (R = H, Ph — 3a, b ) have been synthesized. The ¹H-n.m.r. spectra have been taken for discussing the E/Z-isomerism of the thioacrylamides and the assignment further strengthened by an added LIS-study. The 2-unsubstituted compounds have been found to exist exclusively in preferred configurations/conformations: 2a — E(s-cis); 3a — Z(s-cis); the 2-phenylsubstituted analogs are of divergent behaviour: in 2b the C(S) NMe₂ moiety is found to be twisted out of the common plane, and 3b prefers the flat s-trans conformations (E(s-trans) ⇌ Z(s-trans)). The compounds show restricted rotations about C¹, N- and C³, N-partial double bonds. The corresponding rotational barriers, determined as ΔG-values by dynamic n.m.r. spectroscopy, are discussed with respect to (i) the resonance branch at C¹, (ii) the influence of substituents, and (iii) the effect of steric hindrance in the thioacrylamide moiety generally.     

SnO<Subscript>2</Subscript>-core/SiO<Subscript>x</Subscript>-shell coaxial whiskers with a needle-like morphology

Needle-shaped structures of tin oxide (SnO₂) were coated with a shell layer of SiO_x via a sputtering method. The diameters of the SiO_x-coated structures gradually became thinner, leading to the formation of sharp tips. The whiskers consisted of a crystalline SnO₂ core surrounded by an amorphous SiO_x shell. The photoluminescence (PL) spectrum with a Gaussian fitting exhibited yellow-green and orange light emission bands, and the overall shape and intensity of the PL spectrum were not changed by the SiO_xcoating. The results of this study suggest that sputtering can be employed to achieve the layered growth of shell layers on a variety of nanostructures.     

Studies on the mashing conditions of teff (Eragrostis tef) malt as a raw material for lactic acid‐fermented gluten‐free beverage

Formation of extracts and fermentable sugars during mashing can be limited by incomplete starch gelatinisation. The aim of this research was to develop mashing programme for 100% teff malt as a potential raw material for gluten‐free lactic acid‐fermented beverage. Isothermal mashing at temperatures ranging between 60 and 84 °C was conducted, and the highest extract (85%) was observed for the wort samples produced at temperatures higher than 76 °C. Sixty‐minute rest at 71 °C resulted in higher fermentable sugars than other tested conversion rest temperatures. Inclusion of lower mashing‐in temperature in the mashing programme also substantially improved the concentrations of free amino nitrogen (128 mg L^?1) and fermentable sugar (58 g L^?1) in the final wort. Therefore, 30‐min rest at 40 °C followed by 60‐min rest at 71 °C and 10‐min rest at 78 °C was found to be a suitable mashing programme for teff malt.     

Donor–acceptor interaction between non-aqueous solvents and I2 to generate I3, and its implication in dye sensitized solar cells

The spectrophotometric properties of I⁻, I₂ and the I⁻/I₂ mixture were studied in 1,2-dichloroethane (DCE), acetone (AC), acetonitrile (ACN), ethanol (EtOH), methanol (MeOH), tertiary-butanol (t-BuOH), dimethylformamide (DMF), propylenecarbonate (PC), 3-methoxypropionitrile (MePN), dimethylsulfoxide (DMSO), dioxane (DIO) and pyridine (PY) solutions. From the investigation it has been realized that in DCE, I⁻, I₂ and I⁻/I₂ mixture have the same absorption peak at 500 nm. I⁻ gives rise to the absorption spectra at about 220, 290 and 360 nm in t-BuOH and in PY solutions. However, in all other solvents the I⁻ generates peaks only around 220 nm. Similarly I₂ and the I⁻/I₂ mixture in all solvents except DCE have indicated similar absorption peaks around 220, 290 and 360 nm. On the other hand, except in PC and DMF, I₂ shows the additional peaks in the range of 380–500 nm which are assigned to the formation of a I₂–solvent complex. The peaks around 290 and 360 nm indicate the presence of I⁻₃ and around 220 nm is the peak of I⁻. The spectral shift of the I₂ solutions in the visible region is interesting and is the core of this report. It points to the importance of donor–acceptor interaction between solvents and iodine. The data obtained in these solvents were well correlated to the donor number (DN) of the solvents. From this correlation the DN of MePN was estimated to 14.6. The absorption peak of I₂ in DCE(DN=0.0) is 500 nm and in PY(DN=33.1) is 378 nm. This peak shift due to solvent effects corresponds to an energy difference close to 0.8 eV. The absorption peak shift due to addition of the 0.0080 vol%. PY(1 mM) in 1 mM I₂-ACN solutions corresponds to ca. 0.6 eV. The blue shift of I₂ absorption in basic solvents indicates the tendency to form a complex. The increase of the efficiency of the dye-sensitized solar cell by addition of PY to I⁻/I⁻₃ ACN solution is suggested to be due to the formation of the dipyridine complex, PY₂I⁺. Such complex formation decreases the amount of I₂ which is expected to be an electron scavenger. We also propose that the more bulky complex, PY₂I⁺ has a slower kinetics with the conduction band electrons, and thus decrease the losses of photocurrent and photopotentials in the solar cell.     

Prevalence and antimicrobial susceptibility of Salmonella isolated from a variety of raw meat sausages in Gaborone (Botswana) retail stores

The objective of the study was to provide baseline data on the prevalence and antimicrobial susceptibility of Salmonella in different types of raw meat sausages directly accessible to the consumers in Gaborone, Botswana. A total of 300 raw sausages comprising 79 beef, 78 pork, 72 chicken, and 71 mutton samples were concurrently analyzed for the presence of Salmonella using a conventional culture method and a validated PCR method. The PCR assay results were in full concordance with those of the conventional culture method for the detection of Salmonella. Sixty-five (21.7%) of 300 samples were positive for Salmonella by both the conventional culture method and PCR assay. Even though more chicken samples contained Salmonella than did any other sausage type, the difference in the presence of Salmonella among the four sausages types was not significant. Eleven serotypes were identified, and Salmonella enterica subsp. salamae II was most prevalent in all the sausage types. Beef sausages generally had higher mesophilic bacterial counts than did the other three sausage types. However, higher microbial counts were not reflective of the presence of salmonellae. Susceptibility of the Salmonella enterica serotypes to 20 antimicrobial agents was determined, and Salmonella Muenchen was resistant to the widest array of agents and was mostly isolated from chicken sausages. Regardless of the meat of origin, all 65 Salmonella isolates were resistant to at least four antimicrobial agents: amikacin, gentamicin, cefuroxime, and tombramycin. This resistance profile group was the most common in all four sausage types, comprising 90% of all Salmonella isolates from beef, 71% from pork, 63% from mutton, and 35% from chicken. These results suggest that raw sausages pose a risk of transmitting multidrug-resistant Salmonella isolates to consumers.     

Reduction of Furan Formation by High-Pressure High-Temperature Treatment of Individual Vegetable Purées

The present study addressed the need for furan mitigation measures at the level of food production, where the effects of extrinsic (process-related) and intrinsic (product-related) properties on furan formation in vegetable-based systems were investigated. For the first time in the literature, the effect of high-pressure high-temperature (HPHT) processing on the formation of furan was demonstrated. HPHT processing was proven to be an interesting alternative for furan reduction in vegetable-based systems, when aiming for sterilization intensities. Following HPHT treatment, the furan concentrations of a wide range of individual vegetable purées dropped to levels close to the analytical limits (1–2 ng/g purée). A higher processing cost might limit the use of HPHT processing to high-value added products, which means that for many other conduction-heated food products, conventional heating would remain the standard technology. As a first step towards control of furan formation in the latter products, a mixed model regression was used to identify the major precursors in vegetable-based systems. Significant correlations were observed for vitamin C and sugars, which were attributed to the efficiency of the conversion and high concentrations, respectively. Next to furan, the HPHT- and thermally treated purées were analyzed for 2- and 3-methylfuran, which are likely to undergo the same metabolic fate as furan. For most of the vegetables tested, the total amount of methylfuran found in the thermally treated purées could not be ignored. Similarly to furan, there was a clear reduction in the concentrations found in the HPHT-treated purées.     

ZnO sputter coating on SnO2 nanowires: Effects of thin coating and subsequent thermal annealing

The structural and optical properties of SnO₂–ZnO core–shell nanowires were studied and the effects of thermal annealing were investigated. As-prepared SnO₂–ZnO core–shell nanowires exhibited a smooth and continuous shell layer along the nanowire, with a thickness in the range of 5–10 nm. While the thin ZnO shell layer disappeared after annealing at 800 °C, this did not occur after annealing at 600 °C. The as-fabricated SnO₂–ZnO core–shell nanowires exhibited yellow emission, presumably from the core SnO₂ nanowires. The UV emission from ZnO shell layer was obtained by annealing at 600 °C, whereas it was removed by annealing at 800 °C.     

Optimization of nuclear magnetic resonance and gas chromatography-mass spectrometry-based fingerprinting methods to characterize goat milk powder

This study is the first to provide a comprehensive characterization of the liquid and volatile fractions of whole goat milk powder (GMP). Robust nuclear magnetic resonance (NMR)- and gas chromatography-mass spectrometry (GC-MS)-based chemical fingerprinting methods were optimized and implemented. The untargeted ¹H-NMR analysis resolved 44 metabolites in the liquid fractions of GMP. The NMR fingerprinting technique effectively identified metabolites coming from the aliphatic, sugar, and aromatic regions that can be important in defining the technological properties and quality of the GMP. The untargeted headspace gas chromatography-mass spectrometry fingerprinting was able to detect a total of 50 volatiles including alkanes, ketones, alcohols, aromatics, alkenes, aldehydes, esters, acid, and sulfur compounds. The GMP was dominated by volatiles in the alkane group, while only a few esters were detected. Goat milk is a premium product and vulnerable to fraudulent activities such as adulteration or counterfeit. Therefore, proper characterization and identification is a crucial first step to verify its authenticity and quality.