Synthesis of Galactosylhydroxylysine and its Analogs

Synthesis of (--)-galactosylhydroxylysine (GHL, I), and its analogs (+)-2 and (+)-3, which are essential for development of assays for osteoporosis, is described starting from (2S,5R)-(+)-hydroxylysine (4).     

Detection and characterization of silver nanoparticles in chicken meat by asymmetric flow field flow fractionation with detection by conventional or single particle ICP-MS

A method of analysis of silver nanoparticles (AgNPs) in chicken meat was developed. The homogenized chicken meat sample, which was spiked with AgNPs, was subjected to enzymolysis by Proteinase K for 40 min at 37 °C. Transmission electron microscopy and inductively coupled plasma mass spectrometry (ICP-MS) in single particle mode were used to characterize the number-based size distribution of AgNPs in the meat digestate. Because similar size distributions were found in the meat digestate and in the aqueous suspension of AgNPs used for spiking the meat, it was shown that no detectable dissolution of the AgNPs took place during the sample preparation stage. The digestate was injected into the asymmetric flow field flow fractionation (AF⁴) -ICP-MS system, which enabled fractionation of nanoparticles from the remaining meat matrix, and resulted in one large peak in the fractograms as well as two smaller peaks eluting close to the void volume. The recovery of silver contained in the large AgNP peak was around 80 %. Size determination of AgNPs in the meat matrix, based on external size calibration of the AF⁴ channel, was hampered by non-ideal (early elution) behavior of the AgNPs. Single particle ICP-MS was applied for determination of the number-based particle size distribution of AgNPs in collected fractions. The presented work describes for the first time the coupling of AF⁴ and ICP-MS for AgNP separation in a food matrix.     

Method development for simultaneous analysis of HBCD,TBBPA, and dimethyl-TBBPA in marine biota from Greenland and the Faroe Islands

The brominated flame retardants hexabromocyclododecane (HBCD) and tetrabromobisphenol A (TBBPA) are high-production-volume chemicals. In recent years, their presence has been reported in sediment and biota from the marine environment. In this study, an analytical method was developed for the simultaneous determination of HBCD, TBBPA, and the possible metabolite dimethyl-TBBPA. The method was applied in a preliminary screening of egg, liver, and adipose tissue of marine biota from Greenland and the Faroe Islands. α-HBCD was detected in 35 of 36 analysed samples from the Arctic, indicating a ubiquitous presence of α-HBCD in the environment. β- and γ-HBCD were found in 10 and 14 samples, respectively. TBBPA and dimethyl-TBBPA were not detected in any of the samples indicating limited or no transport of these compounds to remote areas.     

Nanoparticles from conventional cellulose esters: evaluation of preparation methods

Nano-scaled particles were obtained from two different cellulose acetates, cellulose acetate propionate, and cellulose acetate butyrate using the emulsification solvent evaporation procedure and the low energy methods of solvent displacement (dialysis and controlled precipitation). The relationship between the formulation parameters and the particle properties were evaluated in case of the emulsification-evaporation technique. For the solvent displacement procedures, the influence of the formulation parameters, and the intrinsic polymer properties like the hydrophilic-hydrophobic balance was evaluated. Comparing the methods, it could be shown that large amounts of small and uniform nanoparticles can be obtained by the emulsification solvent evaporation procedure. The solvent displacement techniques turned out to be very easy to use and to yield narrowly distributed particles as well.     

Polymer Chain Conformation on Deuterated Polystyrene Nanoparticles Investigated by SANS

We previously reported that grafted polystyrene (PS) chains on silica nanoparticles at a low grafting density show similar conformations to free PS chains in the same solvent, THF (diameter ?50 nm, Colloid.poly.Sci. (2013), 291, 9, 2087–2099). As an extension of our previous study we choose an organic nanoparticle (deuterated polystyrene, dPS) instead of inorganic nanoparticle to see the impact of the substrate material on chain conformation. Additionally, a wider range of molecular weights were prepared to investigate the conformation feature of grafted PS chains more in detail. Small angle neutron scattering (SANS) experiments were performed to characterize PS grafted dPS particles in good solvent condition, with deuterated toluene and deuterated THF as solvent. To get insight into the conformation of the grafted PS layer we apply a scaling law describing the dimension of free PS polymer in good solvent condition to the obtained thickness of the grafted PS layer. We find an overall agreement with the scaling law where the thickness of the grafted PS layer is slightly larger than 2R_g of the free polymer chains in the respective solvent giving hint for semi dilute polymer brush (SDPB) situation.     

Size does matter! Label-free detection of small molecule–protein interaction

This review is focused on methods for detecting small molecules and, in particular, the characterisation of their interaction with natural proteins (e.g. receptors, ion channels). Because there are intrinsic advantages to using label-free methods over labelled methods (e.g. fluorescence, radioactivity), this review only covers label-free techniques. We briefly discuss available techniques and their advantages and disadvantages, especially as related to investigating the interaction between small molecules and proteins. The reviewed techniques include well-known and widely used standard analytical methods (e.g. HPLC-MS, NMR, calorimetry, and X-ray diffraction), newer and more specialised analytical methods (e.g. biosensors), biological systems (e.g. cell lines and animal models), and in-silico approaches.     

Microwave-Assisted One-Pot Lipid Extraction and Glycolipid Production from Oleaginous Yeast Saitozyma podzolica in Sugar Alcohol-Based Media

Glycolipids are non-ionic surfactants occurring in numerous products of daily life. Due to their surface-activity, emulsifying properties, and foaming abilities, they can be applied in food, cosmetics, and pharmaceuticals. Enzymatic synthesis of glycolipids based on carbohydrates and free fatty acids or esters is often catalyzed using certain acyltransferases in reaction media of low water activity, e.g., organic solvents or notably Deep Eutectic Systems (DESs). Existing reports describing integrated processes for glycolipid production from renewables use many reaction steps, therefore this study aims at simplifying the procedure. By using microwave dielectric heating, DESs preparation was first accelerated considerably. A comparative study revealed a preparation time on average 16-fold faster than the conventional heating method in an incubator. Furthermore, lipids from robust oleaginous yeast biomass were successfully extracted up to 70% without using the pre-treatment method for cell disruption, limiting logically the energy input necessary for such process. Acidified DESs consisting of either xylitol or sorbitol and choline chloride mediated the one-pot process, allowing subsequent conversion of the lipids into mono-acylated palmitate, oleate, linoleate, and stearate sugar alcohol esters. Thus, we show strong evidence that addition of immobilized Candida antarctica Lipase B (Novozym 435^®), in acidified DES mixture, enables a simplified and fast glycolipid synthesis using directly oleaginous yeast biomass.     

Preparation and dielectric properties of the lead-free BaFe<Subscript>1/2</Subscript>Nb<Subscript>1/2</Subscript>O<Subscript>3</Subscript> ceramics obtained from mechanically triggered powder

In the paper the influence of mechanical activation of the powder on the final dielectric properties lead-free Ba(Fe_1/2Nb_1/2)O₃ (BFN) ceramic was examined. The BFN ceramics were obtained by 3-steps route. Firstly, the substrates were pre-homogenized in a planetary ball mill. Than, the powder was activated in vibratory mill (the shaker type SPEX 8000 Mixer Mill) for different duration between 25 h and 100 h. The influence of the milling time on the BFN powder was monitored by X-ray diffraction. The diffraction data confirmed that the milling process of the starting components is accompanied by partial synthesis of the BFN materials. The longer of the high-energy milling duration the powders results in increasing the amount of amorphous/nanocrystalline content. The mechanically activated materials were sintered in order to obtain the ceramic samples. During this temperature treatment the final crystallisation of the powder appeared what was confirmed by XRD studies. The performed dielectric measurements have revealed the reduction of the dielectric loss of the BFN ceramics compared to materials obtained by classic methods.