Abstract Verapamil is a chiral drug that is marketed in its racemic form, but because of the pharmacological effects due to molecule’s chirality, one of the enantiomers is more potent, and the other exhibits different activities of therapeutic interest. The preparative separation of the verapamil enantiomers was performed using a continuous Varicol unit operated on a scale of 1 g/day. Amylose tris(3,5-dimethylphenylcarbamate) functioned as the stationary phase, and n-hexane/isopropanol/ethanol mixtures were used as the mobile phase. Diethylamine was used as the additive. The enantiomeric purities were 93.0% for S-(-)-verapamil and 92.0% for R-(+)-verapamil in the raffinate and extract streams, respectively. The unit provided productivities of 0.18 kg of raffinate per day per kg of adsorbent and 0.20 kg of extract per day per kg of adsorbent when using a feed concentration of 12.5 g L-1.

AbstractWater-in-oil (W/O) emulsions are complex mixtures generally found in crude oil production in reservoirs and processing equipment. Sedimentation studies of water-oil emulsions enable the analysis of the fluid dynamic behavior concerning separation of this system composed of two immiscible liquids. Gravitational settling was evaluated in this article for a model emulsion system consisting of water and a Brazilian crude oil diluted in a clear mineral oil as organic phase. The effects of water content and temperature were considered in the study of sedimentation velocity of water-oil emulsions. Water contents between 10% and 50 % and temperatures of 25, 40 and 60 ºC were evaluated, and a Richardson-Zaki type correlation was obtained to calculate settling velocities as a function of the process variables investigated. Water contents and average droplet sizes were monitored at different levels in the settling equipment, thus enabling identification of the effect of these variables on the phenomena of sedimentation and coalescence of the emulsions studied. The results showed that the emulsion stability during sedimentation was governed by the emulsion water content, which yielded high settling velocities at low water contents, even when very small droplets were present. A quantitative analysis of the combined effects of drop size and droplet concentration supports the conclusion that a stronger effect is produced by the higher concentration of particles, compared with the relatively smaller effect of increasing the size of the droplets.

Biodegradable polymeric materials can be used as temporary implants and may be able to carry out specific functions for a pre-determined period prior to their degradation in vivo. In order to be used they must present characteristics of biocompatibility. When a material comes into contact with blood, the instantaneous adsorption of protein occurs on its surface. Coverage of the surface by γ-globulins causes the adhesion of platelets and, consequently, provokes the process of blood coagulation. In this context, the objective of the present paper was to quantify the adsorption of human Immunoglobulin G (HIgG) to poly ( β-hydroxybutyrate) (PHB), poly (L-lactic acid) (PLLA) and PHB/PLLA blends using the FTIR/ATR technique. The results showed the occurrence of HlgG adsorption for all three systems, PHB having the highest adsorption density, about Γmax =2.57 µg/cm², followed by PHB/PLLA blends (Γmax=0.85 µg/cm²) and PLLA with the lowest values (Γmax=0.25 µg/cm²).

Crystallization is an important industrial-scale process for the purification of enantiomers that depends on a phase diagram. In this work, the ternary phase diagram of R- and S-ketamine in ethanol was determined. The eutectic point indicated that crystallization of pure enantiomers from solutions containing more than 75% of the desired enantiomer is feasible. Solubility studies showed the feasibility of using temperature control to conduct the process. Batch crystallization of ketamine (S/R:80/20) solutions at 25ºC provided the isolation of S-ketamine (purity of 100%) with a yield from 65 to 70% and a productivity of 6.5 g/(lh).

Chitosan microspheres with a mean size of 140 ± 119 µm were produced by the spray and coagulation methods. The microspheres were chemically modified using the following routes: a) crosslinking with glutaraldehyde b) crosslinking with epychlorohydrin and c) acetylation. For investigation of their ability as adsorbents, the following standard proteins were chosen as adsorbates: bovine serum albumin - BSA (pI = 4.8 and MW = 66 kDa) and lysozyme (pI = 11 and MW = 14 kDa). The adsorption experiments were performed using a static method. The adsorption media and equilibrium concentration of adsorbates were varied in the ranges of pH 4-11 and 0.07-0.70 mg.ml-1, respectively. The maximum adsorption capacities (q m) and the constant of the Langmuir model (Ks) were shown to be dependent on charge interactions and on the kind of treatment performed on chitosan microspheres. The satisfactory fit of a kinetic model to the experimental data shows that the step that controls the adsorption kinetics is probably the initial adsorbate transport.

A model is derived for the change with time of the concentration of a surface-active component in the liquid pool of a semi-batch foam fractionation process. The transport of surface-active material to the gas-liquid interface was assumed to be limited by the mass transfer rates, and the concentration of the adsorbed material at the interface was assumed to be in equilibrium with the concentration of liquid adjacent to the bubble gas surface. This model was compared to experimental data obtained for semi-batch foam fractionation of aqueous solutions of bovine serum albumin and cetyltrimetylammonium bromide.

The design of novel applications for the use of new high-density adsorbents in the direct recovery of proteins requires analysis of the fluid dynamics and mass transfer characteristics of the column used with the solid-liquid system. In this article we describe the operating parameters related to the use of a high-density, hydrophobic resin (Streamline® Phenyl) for the recovery of alpha-lactalbumin from cow milk whey in an expanded-bed adsorption mode of operation. The adsorption isotherm, kinetic curves and chromatographic curves for adsorption and elution were determined for alpha-lactalbumin recovered from whole whey. The experiments were used to confirm the theoretical model that involves the combination of resistance to the mass transfer in the liquid phase and diffusivity in the adsorbent resin pores. The model solution was obtained through the orthogonal collocation method. A nonlinear multivariable optimization method was used to fit the model to experimental results. A purity of 79% was obtained with the adsorption/elution protocol prior to any polishing procedure.

The two enantiomers that constitute a racemate have different activities when employed as pharmaceuticals. Due to this fact, fully recognized today, the pharmaceutical industry has been forced to market pure enantiomers instead of the racemic mixture whenever a chiral compound is involved. The simulated moving bed (SMB) is a chromatographic process that, unlike traditional HPLC systems, operates continuously without losing the enantiomeric purity of the outlet streams. The present work describes the enantioseparation of the anesthetic ketamine in a semipreparative-scale SMB unit. The chiral stationary phase employed was the microcrystalline cellulose triacetate. The outlet streams were analyzed by an on-line system, composed by an UV/VIS meter and a polarimeter, and also by HPLC. The analysis indicated purity values up to 100% for the stream of interest and up to 97.7% for the other stream.