Stereoselective sodium borohydride reductions of cyclopentanones: influence of ceric chloride on the stereochemistry of reaction

In this paper we describe the reduction by NaBH4 of some cyclopentanones containing an oxygenated function at the side chain position beta to the carbonyl group, both in the presence and in the absence of CeCl3. Some suggestions for the rationalization of the results are discussed, considering the stereochemical course of the reactions.

Complications following an accidental sodium hypochlorite extrusion: A report of two cases

Sodium hypochlorite (NaOCl) is the most commonly used solution in root canal treatments, as it is a low-cost method that displays a very effective antimicrobial activity against microbiota of infected root canals. However, this solution can cause complications especially due to its cytotoxic features. When this solution is injected into the adjacent tissues, the patient usually experiences intense pain, and an urgent treatment should be implemented in order to prevent a long-term sequelae. This paper describes the clinical features of two patients that experienced an accidental extrusion of NaOCl after endodontic treatment of varying severity and with different treatments. Furthermore, it shows the long-term neurologic injuries that this type of accidents may cause and a treatment protocol for these situations will be suggested.

A Novel Missense Mutation, I890T, in the Pore Region of Cardiac Sodium Channel Causes Brugada Syndrome

Brugada syndrome (BrS) is a life-threatening, inherited arrhythmogenic syndrome associated with autosomal dominant mutations in SCN5A, the gene encoding the cardiac Na₊ channel alpha subunit (Naᵥ1.5). The aim of this work was to characterize the functional alterations caused by a novel SCN5A mutation, I890T, and thus establish whether this mutation is associated with BrS. The mutation was identified by direct sequencing of SCN5A from the proband’s DNA. Wild-type (WT) or I890T Naᵥ1.5 channels were heterologously expressed in human embryonic kidney cells. Sodium currents were studied using standard whole cell patch-clamp protocols and immunodetection experiments were performed using an antibody against human Naᵥ1.5 channel. A marked decrease in current density was observed in cells expressing the I890T channel (from -52.0 ± 6.5 pA/pF, n=15 to 35.9 ± 3.4 pA/pF, n = 22, at -20 mV, WT and I890T, respectively). Moreover, a positive shift of the activation curve was identified (V½ =-32.0 ± 0.3 mV, n = 18, and -27.3 ± 0.3 mV, n = 22, WT and I890T, respectively). No changes between WT and I890T currents were observed in steady-state inactivation, time course of inactivation, slow inactivation or recovery from inactivation parameters. Cell surface protein biotinylation analyses confirmed that Nav1.5 channel membrane expression levels were similar in WT and I890T cells. In summary, our data reveal that the I890T mutation, located within the pore of Nav1.5, causes an evident loss-of-function of the channel. Thus, the BrS phenotype observed in the proband is most likely due to this mutation

Effect of reducing and replacing pork fat on the physicochemical, instrumental and sensory characteristics throughout storage time of small caliber non-acid fermented sausages with reduced sodium content

The effect of pork fat reduction (from 44% to 20% final fat content) and its partial substitution by sunflower oil (3% addition) on the physicochemical, instrumental and sensory properties throughout storage time of small caliber non-acid fermented sausages (fuet type) with reduced sodium content (with partial substitution of NaCl by KCl and K-lactate) and without direct addition of nitrate and nitrite (natural nitrate source used instead), was studied. Results showed that sausages with reduced fat (10% initial fat content) and with acceptable sensory characteristics can be obtained by adding to the shoulder lean (8% fat content) during the grinding, either 3.3% backfat (3% fat content) or 3% sunflower oil, both previously finely comminuted with lean. Furthermore, sunflower oil showed to be suitable for partial pork backfat substitution in very lean fermented sausages, conferring desirable sensory properties similar to those of sausages with standard fat content. The sensory quality of the sausages was maintained after three-month cold storage in modified atmosphere.

Influence of the temperature and type of salt on the phase equilibrium of peg 1500 + potassium phosphate and peg 1500 + sodium citrate aqueous two-phase systems

The present work analyzed the effect of the temperature and type of salt on the phase equilibrium of aqueous two-phase systems (ATPS) formed by poly (ethylene glycol) (PEG) 1500 + potassium phosphate, from (278.15 to 318.15) K, and PEG 1500 + sodium citrate, from (278.15 to 298.15) K. The rise of the temperature normally increased the slope of the tie line (STL). With respect to the influence of the type of salt, sodium citrate showed better capability to induce phase separation, when compared to potassium phosphate.

High encapsulation efficiency of sodium alendronate in eudragit S100/HPMC blend microparticles

The hydrophilic drug sodium alendronate was encapsulated in blended microparticles of Eudragit® S100 and Methocel® F4M or Methocel® K100LV. Both formulations prepared by spray-drying showed spherical collapsed shape and smooth surface, encapsulation efficiencies of 85 and 82% and mean diameters of 11.7 and 8.4 µm, respectively. At pH 1.2, in vitro dissolution studies showed good gastro-resistance for both formulations. At pH 6.8, the sodium alendronate release from the microparticles was delayed and was controlled by Fickian diffusion. In conclusion, the prepared microparticles showed high encapsulation efficiency of sodium alendronate presenting gastro-resistance and sustained release suitable for its oral administration.

Rapid and accurate hplc-dad method for the determination of the herbicide bispyribac-sodium in surface water, and its validation

A new method is described for the determination of the herbicide bispyribac-sodium in surface water, especially from river and irrigated rice water samples. The method involves extraction in solid phase and quantification by high performance liquid chromatography with diode array detection (HPLC-DAD). After optimization of the extraction and separation parameters, the method was validated. The method presented average recoveries of 101.3 and 97.7%, under repeatability and intermediate precision conditions, respectively, with adequate precision (RSD from 0.9 to 7.5%). The method was applied for the determination of bispyribac-sodium in surface water samples with a limit of detection of 0.1 μg L-1.

Thermodynamic study of the solubility of sodium naproxen in some ethanol + water mixtures

By using the van't Hoff and Gibbs equations the apparent thermodynamic functions Gibbs energy, enthalpy, and entropy of solution for sodium naproxen in ethanol + water cosolvent mixtures, were evaluated from solubility data determined at temperatures from (278.15 to 308.15) K. The drug solubility was greatest in neat water and lowest in neat ethanol at all the temperatures studied. By means of non-linear enthalpy-entropy compensation analysis, it follows that the dissolution process of this drug in ethanol-rich mixtures is entropy-driven, whereas, in water-rich mixtures the process is enthalpy-driven.

Evaluation of chitosan microparticles containing curcumin and crosslinked with sodium tripolyphosphate produced by spray drying

The aim of this study was to encapsulate curcumin into chitosan, using sodium tripolyphosphate (TPP) as an ionic crosslinker by the spray drying method. The influence of TPP on the properties of the final product, such as solubility, morphology, loading efficiency, thermal behavior, swelling degree and release profiles, was evaluated. The microparticles had a spherical morphology (0.5-20 µm) with no apparent porosity or cracks. Results indicated the formation of a polymeric network, which ensures effective protection for curcumin. Controlled-release studies were carried out at pH 1.2 and 6.8, to observe the influence of pH on curcumin release while the mechanism was analyzed using the Korsmeyer-Peppas equation.

Application of ftir in the determination of acrylate content in poly(sodium acrylate-co-acrylamide) superabsorbent hydrogels

Hydrogels have been prepared by free-radical solution copolymerization of acrylamide and sodium acrylate (NaAc), with molar ratio ranging from 25/75 to 80/20, respectively, using methylene bisacrylamide as the crosslinking agent. A FTIR spectroscopy procedure to determine the acrylate/acrylamide ratio in these hydrogels was proposed based on absorbance at 1410 cm-1 (nCOO-) and 2940 cm-1 (nCH and nCH2). A straight line with a good linear correlation coefficient (0.998) was obtained by plotting the acrylate content (Ac%) versus relative absorbance (Arel = A1410/A2940). Results were confirmed by the amount of sodium cation released in acid medium determined by atomic absorption spectrometry.

Sodium dodecyl sulfate coated γ-alumina support modified by a new Schiff base for solid phase extraction and flame-AAS determination of lead and copper ions

A simple and fast approach for solid phase extraction is herein described, and used to determine trace amounts of Pb2+ and Cu2+ metal ions. The solid phase support is sodium dodecyl sulfate (SDS)-coated γ-alumina modified with bis(2-hydroxy acetophenone)-1,6-hexanediimine (BHAH) ligand. The adsorbed ions were stripped from the solid phase by 6 mL of 4 M nitric acid as eluent. The eluting solution was analyzed by flame atomic absorption spectrometry (FAAS). The sorption recovery of metal ions was investigated with regard to the effects of pH, amount of ligand, γ-alumina and surfactant and the amount and type of eluent. Complexation of BHAH with Pb2+ or Cu2+ ions was examined via spectrophotometry using the HypSpec program. The detection limit for Cu2+ was 7.9 µg L-1 with a relative standard deviation of 1.67%, while that for Pb2+ was 6.4 µg L-1 with a relative standard deviation of 1.64%. A preconcentration factor of 100 was achieved for these ions. The method was successfully applied to determine analyte concentrations in samples of liver, parsley, cabbage, and water.

Synthesis and thermal studies of solid state 2-chloro-benzylidenepyruvic acid and its compounds with sodium, aluminium (III), gallium (III) and indium (III) cations

The synthesis of sodium 2-chlorobenzylidenepyruvate and its corresponding acid as well as binary, binary together with it's acid or hydroxo-2-chorobenzylidenepyruvate of aluminium (III), gallium (III) and indium (III), were isolated. Chemical analysis, thermogravimetry, derivative thermogravimetry (TG/DTG), simultaneous thermogravimetry-differential thermal analysis (TG-DTA) and X-ray powder diffractometry have been employed to characterize and to study the thermal behaviour of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition.

Thermal behavior of alginic acid and its sodium salt

An evaluation of hydration and thermal decomposition of HAlg and its sodium salt is described using thermogravimetry (TG) and differential scanning calorimetry (DSC). TG curves in N2 and air, were obtained for alginic acid showed two decomposition steps attributed to loss of water and polymer decomposition respectively. The sodium alginate decomposed in three steps. The first attributed to water loss, followed by the formation of a carbonaceous residue and finally the Na2CO3. DSC curves presented peaks in agreement with the TG data. In the IR alginic acid presented bands at 1730 and 1631 cm-1, while sodium alginate presented a doublet at 1614 e 1431 cm-1, evidencing the presence of salified carboxyl groups.

Comparison of Potassium and Sodium Content in Diet and Non-Diet Soft Drinks by Using Capillary Electrophoresis with Capacitively Coupled Contactless Conductivity Detection

Capillary electrophoresis (CE) with capacitively coupled contactless conductivity detection (C4D) was used for determination of sodium and potassium concentrations in diet and non-diet soft drinks. Higher sodium concentrations were found in the diet samples due to the utilization of sodium salts of cyclamate and saccharine as sweeteners. The CE-C4D method can be used by food industries and health regulatory agencies for monitoring sodium and potassium content, not only in soft drink but in many others food products.