Biotin-Containing Third Generation Glucoheptoamidated Polyamidoamine Dendrimer for 5-Aminolevulinic Acid Delivery System

Polyamidoamine PAMAM dendrimer generation 3 (G3) was modified by attachment of biotin via amide bond and glucoheptoamidated by addition of α-D-glucoheptono-1,4-lacton to obtain a series of conjugates with a variable number of biotin residues. The composition of conjugates was determined by detailed 1-D and 2-D NMR spectroscopy to reveal the number of biotin residues, which were 1, 2, 4, 6, or 8, while the number of glucoheptoamide residues substituted most of the remaining primary amine groups of PAMAM G3. The conjugates were then used as host molecules to encapsulate the 5-aminolevulinic acid. The solubility of 5-aminolevulinic acid increased twice in the presence of the 5-mM guest in water. The interaction between host and guest was accompanied by deprotonation of the carboxylic group of 5-aminolevulinic acid and proton transfer into internal ternary nitrogen atoms of the guest as evidenced by a characteristic chemical shift of resonances in the ¹H NMR spectrum of associates. The guest molecules were most likely encapsulated inside inner shell voids of the host. The number of guest molecules depended on the number of biotin residues of the host, which was 15 for non-biotin-containing glucoheptoamidated G3 down to 6 for glucoheptoamidated G3 with 8 biotin residues on the host surface. The encapsulates were not cytotoxic against Caco-2 cells up to 200-µM concentration in the dark. All encapsulates were able to deliver 5-aminolevulinic acid to cells but aqueous encapsulates were more active in this regard. Simultaneously, the reactive oxygen species were detected by staining with H2DCFDA in Caco-2 cells incubated with encapsulates. The amount of PpIX was sufficient for induction of reactive oxygen species upon 30-s illumination with a 655-nm laser beam.     

Flame retardant and durable chloroprene rubber and styrene-butadiene rubber blends crosslinked with copper(I) oxide

The purpose of this work was to investigate the effect of application of copper(I) oxide (Cu₂O) as an unconventional crosslinking agent of chloroprene (CR) and styrene-butadiene (SBR) rubber compositions. The use of Cu₂O arises from the need to limit the application of ZnO as a CR crosslinking agent. The obtained results indicate that CR/SBR blends crosslinked with Cu₂O are characterized by good mechanical properties and a high degree of crosslinking The results show that the proportion of both processing rubbers, as well as the amount of copper(I) oxide, influence the crosslinking of CR/SBR blends and the properties of the vulcanizates. Performing FTIR analysis has allowed the development of a crosslinking mechanism. Crosslinking presumably takes place according to the mechanism of Friedel–Crafts alkylation reaction. Silica, chalk, china clay and nanofiller (montmorillonite modified with quaternary ammonium salt containing hydroxyl groups) were applied as fillers. Among the fillers, silica had the greatest impact on improving the properties. It is arisen from silica activity, unlike other used fillers. The AFM analysis allowed us to determine the miscibility of the rubbers and dispersion of fillers. Thermal analysis was performed to determine the changes occurring as a result of material heating. The low intensity of the peaks corresponding to the crosslinking of the CR/SBR blends may indicate a small amount of bonds formed during heating, or possibility is the formation of connections between chains with a low binding energy. The use of chalk, china clay or silica increases the thermal stability of the vulcanizates. Obtained vulcanizates were characterized by increased incombustibility. The study of combustion time in the air showed that the prepared vulcanizates did not support the burning.

     

Indirect Determination of MCPD Fatty Acid Esters in Lipid Fractions of Commercially Available Infant Formulas for the Assessment of Infants’ Health Risk

Food Analytical Methods - MCPD esters are intensively investigated food lipid contaminants for over a decade. Concern related to their presence in various types of food products is related to the...     

Antioxidant capacity of rapeseed meal and rapeseed oils enriched with meal extract

Response surface methodology (RSM) was used to evaluate the quantitative effects of two independent variables: solvent polarity and temperature of the extraction process on the antioxidant capacity (AC) and total phenolics content (TPC) in meal rapeseed extracts. The mean AC and TPC results for meal ranged between 1181–9974 µmol TE/100 g and 73.8–814 mg sinapic acid/100 g of meal. The experimental results of AC and TPC were close to the predicted values calculated from the polynomial response surface models equations (R² = 0.9758 and 0.9603, respectively). The effect of solvent polarity on AC and TPC in the examined extracts was about 3.6 and 2.6 times greater, respectively, than the effect of processing temperature. The predicted optimum solvent polarity of ε = 78.3 and 63.8, and temperature of 89.4 and 74.2°C resulted in an AC of 10 014 µmol TE/100 g and TPC of 863 mg SAE/100 g meal, respectively. The phenolic profile of rapeseed meal was determined by an HPLC method. The main phenolics in rapeseed meal were sinapine and sinapic acid. Refined rapeseed oils were fortified with an extract – rich in polyphenols – obtained from rapeseed meal. The supplemented rapeseed oil had higher AC and TPC than the refined oil without addition of meal extracts. However, AC and TPC in the enriched oils decreased during storage. The TPC in the studied meal extracts and rapeseed oils correlated significantly (p<0.0000001) positively with their AC (R² = 0.9387). Practical applications: Many bioactive compounds extracted from rapeseed meal provide health benefits and have antioxidative properties. Therefore, it seems worth to consider the application of antioxidants extracted from the rapeseed meal for the production of rapeseed oils with potent AC. Moreover, antioxidants extracted from the rapeseed meal were added to refined rapeseed oil in order to enhance its AC. AC was then tested by FRAP assay. FRAP method is based on the reduction of the ferric tripyridyltriazine (Fe³⁺‐TPTZ) complex to the ferrous tripyridyltriazine (Fe²⁺‐TPTZ), and it is simple, fast, low cost, and robust method. FRAP method does not require specialized equipment and can be performed using automated, semi‐automatic, or manual methods. Therefore the proposed FRAP method can be employed by the fat industry laboratories to asses the AC of rapeseed oils and meal.     

Rational Design,Synthesis, and Potency of N‐Substituted Indoles,Pyrroles, and Triarylpyrazoles as Potential Fructose 1,6‐Bisphosphatase Inhibitors

By using computer modeling and lead structures from our earlier SAR results, a broad variety of pyrrole‐, indole‐, and pyrazole‐based compounds were evaluated as potential fructose 1,6‐bisphosphatase (FBPase) inhibitors. The docking studies yielded promising structures, and several were selected for synthesis and FBPase inhibition assays: 1‐[4‐(trifluoromethyl)benzoyl]‐1H‐indole‐5‐carboxamide, 1‐(α‐naphthalen‐1‐ylsulfonyl)‐7‐nitro‐1H‐indole, 5‐(4‐carboxyphenyl)‐3‐phenyl‐1‐[3‐(trifluoromethyl)phenyl]‐1H‐pyrazole, 1‐(4‐carboxyphenylsulfonyl)‐1H‐pyrrole, and 1‐(4‐carbomethoxyphenylsulfonyl)‐1H‐pyrrole were synthesized and tested for inhibition of FBPase. The IC₅₀ values were determined to be 0.991 and 1.34 μM , and 575, 135, and 32 nM , respectively. The tested compounds were significantly more potent than the natural inhibitor AMP (4.0 μM ) by an order of magnitude; indeed, the best inhibitor showed an IC₅₀ value toward FBPase more than two orders of magnitude better than that of AMP. This level of activity is virtually the same as that of the best currently known FBPase inhibitors. This work shows that such indole derivatives are promising candidates for drug development in the treatment of type II diabetes.     

A new method of preparing Ni/YSZ cermet materials

Ceramic–metal composites (cermets) containing yttria-stabilized zirconia(YSZ) and Ni particles as anode materials in solid oxide fuel cells were prepared by a new method. The method encompasses nickel oxalate dihydrate precipitation on the nanometre YSZ powder, and decomposition at 633 K in inert atmosphere. The composite powders containing 30, 40, and 50% Ni manufactured by the oxalate method were compacted into disk pellets, and sintered in Ar containing 10% H₂. The structure of the cermet materials was characterized by means of X-ray diffractometry (XRD), scanning electron microscopy (SEM), and mercury porosimetry. The thermal expansion coefficient (TEC) was determined by the dilatometric method. Electrochemical impedance spectroscopy (EIS) was used to determine electrical conductivity. The oxalate method leads to obtaining the Ni/YSZ anodes with the Ni content reduced to 40 wt% and well obeying based requirements for anode material in SOFCs.     

Patient dose measurements in diagnostic radiology procedures in Montenegro

It was the aim of the study presented here to estimate for the first time patient dose levels in conventional diagnostic radiology in Montenegro. Measurements of patient dose in terms of entrance surface air kerma (ESAK) and kerma-area product (KAP) were performed on at least 10 patients for each examination type, in each of five randomly selected health institutions in Montenegro, so that a total of 872 patients for 16 different examination categories were included in the survey (817 patients for 1049 radiographies and 55 fluoroscopy patients). Exposure settings and individual data were recorded for each patient. Mean, median and third quartile values ESAK of patient doses are reported. The estimated mean ESAK values obtained are as follows: 4.7 mGy for pelvis anteroposterior (AP), 4.5 mGy for lumbar spine AP, 7.8 mGy for lumbar spine lateral (LAT), 3.1 mGy for thoracic spine AP and 4.3 mGy for thoracic spine LAT. When compared with the European diagnostic reference values, the mean ESAK for all studied examination types are found to be below the reference levels, except in chest radiography. Mean ESAK values for chest radiography are 0.9 mGy for posteroanterior (PA) projection and 2.0 mGy for LAT. The results exhibit a wide range of variation. For fluoroscopy examinations, the total KAP was measured. The mean KAP value per procedure for barium meal is found to be 22 Gy cm(2), 41 Gy cm(2) for barium enema and 19 Gy cm(2) for intravenous urography. Broad dose ranges for the same types of examinations indicate the necessity of applying practice optimisation in diagnostic radiology and establishment of national diagnostic reference levels.     

Engineering of bone fixation metal implants biointerface—Application of parylene C as versatile protective coating

The tribological and protective properties of parylene C coatings (2–20 μm) on stainless steel 316L implant materials were investigated by means of electrochemical measurements and wear tests. The thickness and morphology of the CVD prepared coatings were characterized by scanning electron and laser confocal microscopy. The stability of the coatings was examined in contact with Hanks' solution and H₂O₂ (simulating the inflammatory response). It was concluded that silane–parylene C coating with the optimum thickness of 8 μm exhibits excellent wear resistance properties and limits the wear formation. The engineered versatile coating demonstrates sufficient elastomer properties, essential to sustain the implantation surgery strains and micromotions during long-term usage in the body.     

Mitigation of Sn Whisker Growth by Composite Ni/Sn Plating

Tin (Sn) is a key industrial material in coatings on various components in the electronics industry. However, Sn is prone to the development of filament-like whiskers, which is the leading cause of many types of damage to electronics reported in the last several decades. Due to its properties, a tin-lead (Sn-Pb) alloy coating can mitigate Sn whisker growth. However, the demand for Pb-free surface finishes has rekindled interest in the Sn whisker phenomenon. In order to achieve properties similar to those naturally developed in a Sn-Pb alloy coating, we carried out a study on deposited films with other Sn alloys, such as tin-bismuth (Sn-Bi), tin-zinc (Sn-Zn), and tin-copper (Sn-Cu), electrodeposited onto a brass substrate by utilizing a pulse plating technique. The results indicated that the Sn alloy films modified the columnar grain structure of pure Sn into an equiaxed grain structure and increased the incubation period of Sn whisker growth. The primary conclusions were based on analysis of the topography and microstructural characteristics in each case, as well as the stress distribution in the plated films computed by x-ray diffraction, and the␣amount of Sn whisker growth in each case, over 6 months under various environmental influences.