Solution- and crystal-phase covalent modification of lysozyme by a purpose-designed organoruthenium complex. A MALDI-TOF MS study of its metal binding sites

Study of the reaction between the transition organometallic complex 4-ruthenocenyl 2,6-dimethylpyrylium tetrafluoroborate and the enzyme hen egg white lysozyme (HEWL) in solution and by diffusion in crystals was performed by use of a combination of spectroscopic and chromatographic methods. Conjugation involving the lysine residues of lysozyme appeared to occur readily, yielding very stable ruthenocenyl pyridinium adducts with average degrees of incorporation ranging from 0.2 to 1.8 metal complexes per protein molecule, depending on reaction conditions. Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) revealed that the protein conjugates were in fact mixtures of unmodified, mono-, di- and sometimes tripyridinium adducts. In combination with reversed-phased HPLC, we were able to show that six different monoruthenocenyl pyridinium adducts were formed in solution. This result was confirmed by trypsin digestion of a ruthenocenyl pyridinium conjugate and MALDI-TOF MS analysis of the peptide mixture, which showed that lysines 1, 13, 33, 96, 97 and 116 were involved in the reaction with the pyrylium complex, lysines 13, 33 and 116 being the major binding sites. In the tetragonal crystal state, no binding of the ruthenium complex was shown to occur at lysine 116, owing to steric hindrance at this particular position.     

Background voltage distortion influence on power electric systems in the presence of the Steinmetz circuit

In traction systems, it is usual to connect reactances in delta configuration with single-phase loads to reduce voltage unbalances and avoid electric system operation problems. This set is known as Steinmetz circuit. Parallel and series resonances can occur due to the capacitive reactance of the Steinmetz circuit and affect power quality. In this paper, the series resonance “observed” from the supply system is numerically located. The study of this resonance is important to avoid problems due to background voltage distortion. Experimental measurements are also presented to validate the obtained numerical results.     

Entrapment of Phenytoin into Microspheres of Oleaginous Materials: Process Development and in Vitro Evaluation of Drug Release

A novel multiparticulate preparation of the antiepileptic agent phenytoin (1) was developed and evaluated in vitro. The preparation consists of gastroresistant microparticulate drug delivery system formulated with oleaginous material (lipospheres) to minimize unwanted effects of l on gastric apparatus. The drug was dispersed in a spherical micromatrix consisting of a mixture of stearyl alcohol and glycerol esters of various fatty acids. The best mixture to obtain discrete, reproducible, free-flowing lipospheres consisted of glyceryl monostearate dilaurate and stearyl alcohol (ratio 3: 17). The lipospheres were obtained by a technique involving melting and dispersion of drug-containing oleaginous material in aqueous medium. The oily droplets of the resulting emulsion after cooling under rapid stirring were transformed into solid. About 99% of the lipospheres were of particle size range 100-800 pm. The lipospheres were analyzed to determine the drug content in various particle sizes and to characterize the in vitro release profile. The average drug content was 23.8% w/w. Drug encapsulation efficiency was about 93.6% and the yield of production ranged from 94 to 98%. The drug discharge pattern from the microparticulate system in the intestinal environment was evaluated. Kinetic results were analyzed to distinguish between various release models. The matrix diffusion-controlled equation was the most appropriate one in describing drug release.     

Towards identifying the roll motion parameters of a motorcycle simulator

This study aimed at identifying the roll motion parameters of a motorcycle simulator prototype. Experienced motorcyclists tuned the angular physical movement of the mock-up and that of the visual scene to achieve an optimal riding experience during curves. The participants exceeded the rolling angles that would be required in real-world riding, while avoiding leaning the mock-up beyond 10°. In addition, they were more influenced by the speed of the virtual motorcycle than by road curvature, especially in a wide field of view. Heterogeneity was found in the roll applied to the visual scene. The overall patterns suggest that at least when washout is not applied to remove the side forces that in real-world riding are compensated by a centrifugal force, greater roll of the visual at the expense of the mock-up is mandatory to avoid performance biases that might be enhanced due to fear of falling off the simulator. Future roll motion models must take into consideration factors such as riding postures, which might not only influence the forces operating on the rider-motorcycle system, but also how motorcyclists perceive the visual world.     

Composition, yield, and functionality of reduced-fat Oaxaca cheese: effects of using skim milk or a dry milk protein concentrate

The effect of adding either skim milk or a commercial dry milk protein concentrate (MPC) to whole milk on the composition, yield, and functional properties of Mexican Oaxaca cheese were investigated. Five batches of Oaxaca cheeses were produced. One batch (the control) was produced from whole milk containing 3.5% fat and 9% nonfat solids (SNF). Two batches were produced from milk standardized with skim milk to 2.7 and 1.8% fat, maintaining the SNF content at 9%. In the other 2 batches, an MPC (40% protein content) was used to standardize the milk to a SNF content of 10 and 11%, maintaining the milk fat content at 3.5%. The use of either skim milk or MPC caused a significant decrease in the fat percentage in cheese. The use of skim milk or MPC showed a nonsignificant tendency to lower total solids and fat recoveries in cheese. Actual, dry matter, and moisture-adjusted cheese yields significantly decreased with skim milk addition, but increased with MPC addition. However, normalized yields adjusted to milk fat and protein reference levels did not show significant differences between treatments. Considering skim milk-added and control cheeses, actual yield increased with cheese milk fat content at a rate of 1.34 kg/kg of fat (R = 0.88). In addition, cheese milk fat and SNF:fat ratio proved to be strong individual predictors of cheese moisture-adjusted yield (r² ≈ 0.90). Taking into account the results obtained from control and MPC-added cheeses, a 2.0-kg cheese yield increase rate per kg of milk MPC protein was observed (R = 0.89), with TS and SNF being the strongest predictors for moisture adjusted yield (r² ≈ 0.77). Reduced-fat Oaxaca cheese functionality differed from that of controls. In unmelted reduced-fat cheeses, hardness and springiness increased. In melted reduced-fat cheeses, meltability and free oil increased, but stretchability decreased. These changes were related to differences in cheese composition, mainly fat in dry matter and calcium in SNF.     

Optimization of MRI Acquisition and Texture Analysis to Predict Physico-chemical Parameters of Loins by Data Mining

The main objective of this study was to configure the acquisition and analysis of low-field magnetic resonance imaging (MRI) to predict physico-chemical characteristics of Iberian loin, evaluating the use of different MRI sequences (spin echo, SE; gradient echo, GE; turbo 3D, T3D), computational texture feature methods (GLCM, NGLDM, GLRLM, GLCM + NGLDM + GLRLM), and data mining techniques (multiple linear regression, MLR; isotonic regression, IR). Moderate to very good correlation coefficients and low mean absolute error were found when applying MLR or IR on any method of computational texture features from MRI acquired with SE or GE. For T3D sequence, accurate results are only obtained by applying IR on GLCM or GLCM + NGLDM + GLRLM methods. Considering not only the accuracy of the methodology but also consumed time and required resources, the use of SE sequences for MRI acquisition, GLCM method for MRI texture analysis, and MLR could be indicated for prediction physico-chemical characteristics of loin.     

Benefit of Microscopic Diffusion Measurement for the Characterization of Nanoporous Materials

Detailed knowledge of the transport properties of nanoporous materials is a prerequisite for their complete characterization and optimum technological exploitation. One of the best ways to attain this information is provided by the “microscopic” techniques of diffusion measurement, in particular by the pulsed field gradient technique of NMR and by interference microscopy and IR microscopy. Starting with the measuring principles, the various types of evidence as accessible by these techniques are illustrated. A large variety of host‐guest systems with both ordered and random pore networks have been studied, from microporous up to macroporous materials. The information obtained concerns diffusivities in the various pore domains, extra resistances at the interfaces between them and the associated exchange rates.     

Some implications of nanoscience in food dispersion formulations containing phospholipids as emulsifiers

This contribution is concerned with phospholipid films in relation to food dispersions such as emulsions and foams. Structural, morphological and surface rheological characteristics of dipalmitoyl phosphatidylcholine (DPPC) and dioleoyl phosphatidylcholine (DOPC) monolayers were determined at the air–water interface at 20 °C and at pH 5, 7, and 9, by means of surface pressure (π)–area (A) isotherms coupled with Brewster angle microscopy (BAM), atomic force microscopy (AFM) and surface dilatational and shear rheometry. From the π–A isotherms it was deduced that DPPC monolayers show structural polymorphism at the air–water interface. DOPC monolayers formed a liquid-expanded (LE) structure under all experimental conditions, a consequence of the weak molecular interactions due to the double bond in the hydrocarbon chain. Electrostatic interactions between film-forming components influence the monolayer structure. BAM and AFM images corroborate, at a microscopic and at nanoscopic level respectively, the structural polymorphism deduced from the π–A isotherm for DPPC monolayers as a function of surface pressure and the pH of the aqueous phase. However, the homogeneous morphology of DOPC monolayers at a microscopic level, as observed by BAM, shows structural heterogeneity at a nanoscopic level when observed by AFM. The relative monolayer thickness increases with surface pressure and is a maximum at the collapse point, especially for DPPC monolayers. The results confirm that the interfacial rheological characteristic measured under dilatation and shear conditions are very dependent on the structural characteristics and morphology of the phospholipids (DPPC and DOPC) monolayers.