Rapid dissolution of vitamin E by using sodium N-lauroylsarcosinate ionic surfactant

Vitamin E is widely used in pharmaceutical, food and cosmetic preparations. This paper discusses methods of preparing a vitamin E emulsion by using sodium N-lauroylsarcosinate (SNLS) ionic surfactant. The amount of vitamin E dissolved in water was analyzed by turbidity and UV absorption measurements. The emulsion droplet size was determined by laser light scattering. Microemulsions with small particle size and high resistance to oxidation in air can be obtained by solubilizing vitamin E in SNLS solution. The dissolution is rapid and the surfactant solution has high solubilization power. At 0.7% surfactant concentration, the saturation value is 1 g vitamin E per gram of surfactant. The micellar dissociation concentration (MDC) of the surfactant can be estimated from a vitamin saturation—surfactant concentration curve. Dissolution mechanisms at different surfactant concentrations are interpreted by use of the MDC and CMC (critical micellar concentration) concepts.     

A new dissolution microcalorimeter: calibration and test

A new batch microcalorimetric vessel for the determination of enthalpies of dissolution of small amounts of easily or slightly soluble solids was developed at University of Lund, Sweden and was tested at University of Porto, Portugal.The vessel forms part of a series of twin heat conduction microcalorimeters. In a series of consecutive dissolution steps up to four samples, each 0.1-3 mg, can be injected into a solvent chamber of the vessel, volume 20 ml. The high stability of the baseline allows solution experiments to be extended over several hours.All measurements reported were conducted at 298.15 K and with water as the solvent. The calorimeter was calibrated chemically by dissolution of potassium chloride. The performance of the instrument was further tested by measurements of the enthalpies of dissolution of acetanilide and adenine, 18.25±0.56 and 31.78±0.64 kJ mol⁻¹, respectively. No concentration dependence was found. The results are in good agreement with values in the literature.     

A new method for alkaline dissolution of uranium metal foil

In order to develop a production process of ⁹⁹Mo by fission of low-enriched uranium, the first purification step, which consists of dissolution of a uranium metal foil target, was studied. It was found that alkaline NaClO gave good results, reaching the dissolution of up to 300 m of uranium foil. The different conditions for the dissolution were studied and the optimum ones were found. The influence of NaClO and NaOH concentration, temperature, dissolving solution volume per unit of surface and dissolution time were investigated. During this step, a gas, identified as H₂, was generated, and a precipitate characterized as Na₂U₂O₇ was observed. A stoichiometric reaction for this uranium dissolution is proposed.     

Kinetics of carbon steel dissolution in ammonium chloride solution containing sodium thiosulfate

The dissolution behavior of carbon steel in ammonium chloride (NH₄Cl) solution containing sodium thiosulfate (Na₂S₂O₃) of various concentrations (0.01 and 0.1 M) was investigated using electrochemical impedance spectroscopy (EIS) and other nonelectrochemical techniques. The weight loss and polarization measurements indicate a significant increase in the NH₄Cl corrosion rate of carbon steel on addition of Na₂S₂O_3. The EIS measurements exhibited two capacitive loops at multiple direct current (dc) potentials for both the concentrations. Electrical equivalent circuit (EEC) and reaction mechanism analysis (RMA) were employed to analyze the impedance data. A four-step mechanism with two intermediate adsorbate species of same charge was proposed to explain the dissolution behavior of carbon steel in the given system. The surface coverage values enumerated that the surface was entirely covered with adsorbed species unlike in the pure NH₄Cl system. Charge transfer resistance and polarization resistance values estimated from RMA parameters indicate the increase in a dissolution rate with dc potential. The surface morphology was inspected via field emission scanning electron microscopy, and the corrosion products including surface state of carbon steel electrode were analyzed using energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy.     

A micellar liquid chromatographic method for quality control of pharmaceutical preparations containing tricyclic antidepressants

Summary Micellar liquid chromatography methods for quality control of pharmaceutical preparations (capsules, pills, tablets, injections) containing the tricyclic antidepressants amineptine, amitriptiline, clomipramine, doxepin, imipramine, melitracen and nortriptyline alone or together with other CNS drugs like diazepam, medazepam and perphenazine are described. The methods using micellar solutions of cetyltrimethylammonium bromide as mobile phases and UV detection are rapid and reproducible. Due to the versatility of interactions in micellar liquid chromatography, it is possible determine highly hydrophobic compounds such as TCAs in a short time using mobile phases containing low organic solvent concentrations and usual flow rates, in contrast with the RP-HPLC methods proposed for these compounds. Samples preparation only requires solution and adequate dilution with the mobile phase before injection into the chromatographic system.     

A new liquid membrane electrode for determination of vitamin B1 in multivitamin preparations

Summary A new liquid membrane electrode was developed which is highly selective and sensitive for vitamin B₁. It is based on the thiamine-picrolonate ion-pair complex as an electroactive material in nitrobenzene solvent. The electrode has a remarkable selectivity for vitamin B₁ in the presence of vitamins B₂, B₆, B₁₂ and nicotinamide. The results obtained for the determination of vitamin B₁ in various multivitamin preparations at levels as low as 1 g/ml show an average recovery of 98% (mean standard deviation 1.8%) and are favourably compared with those obtained by the official methods.

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Neue Flüssig-Membranelektrode zur Bestimmung von Vitamin B₁ in Multivitaminpräparaten

Zusammenfassung Eine neue, für Vitamin B₁ hochselektive Flüssig-Membranelektrode wurde entwickelt. Sie beruht auf dem Thiamin-Picrolonat-Ionenpaarkomplex als elektroaktives Material im Lösungsmittel Nitrobenzol. Die Elektrode besitzt eine beachtliche Selektivität für Vitamin B₁ in Gegenwart der Vitamine B₂, B₆, B₁₂ und Nicotinamid. Bei Bestimmungen in verschiedenen Multivitaminpräparaten mit Konzentrationen bis herab zu 1 g/ml erhielt man eine durchschnittliche Wiederfindung von 98% (mittlere Standardabweichung 1,8%). Die erhaltenen Resultate zeigen gute Übereinstimmung mit den nach amtlichen Methoden erhaltenen Werten.

     

Behaviors of sodium glycochenodeoxycholate and sodium glycoursodeoxycholate in binary mixed micelles of bile salt and nonionic surfactant

The behavior of sodium glycochenodeoxycholate (NaGCDC) and sodium glycoursodeoxycholate (NaGUDC) in binary mixed micelles consisting of bile salt and octaoxyethylene glycol mono n-decyl ether (C₁₀E₈) has been studied on the basis of micellar compositions, polarities of the interior of intramicelles, mean aggregation numbers and ¹H NMR measurements. Micellar compositions for both NaGCDC---C₁₀E₈ and NaGUDC---C₁₀E₈ systems showed a tendency to change from C₁₀E₈-rich micelles to bile-salt-rich micelles with an increase on the mole fraction of bile salts from the results of both theoretical calculations using the critical micelle concentration and the micellar polarity. The microenvironment of intramicelles for the NaGCDC---C₁₀E₈ system was found to be more hydrophobic than that for the NaGUDC---C₁₀E₈ system. Mean aggregation numbers of mixed micelles for both systems decreased abruptly with an increase in the mole fraction of bile salts in the range of low mole fraction, but those for NaGCDC were larger than those for NaGUDC. Furthermore, from the results of ¹H NMR measurements, the motions of the methyl group protons in the 18 position of the molecular structure of NaGCDC were slightly restricted with an increase in the mole fraction of NaGCDC. In contrast, the methyl group protons in the 18 and 19 positions of the molecular structure of NaGUDC became freer with an increase in the mole fraction of NaGUDC.     

A new method for the preparation of solution of sodium pentaphosphacyclopentadienide

Heating of a mixture of white phosphorus and sodium in diethylene glycol dimethyl ether in the presence of catalytic amounts of dibenzo-18-crown-6 affords a pure solution of sodium pentaphosphacyclopentadienide NaP₅. One of the intermediate products is trisodium heptaphosphide Na₃P₇. The influence of the nature of a metal (Li, Na, K) on the formation of the pentaphosphacyclopentadienide anion was studied. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1249–1251, July, 2006.     

A new enzymatic method for determination of E. coli

Inthispaper,arapid,sensitiveandsimpleenzymaticmethodfordetectingtheE.coltcellshasbeenestablished.P-GalactosidaseisakindofendoenzymeexistingintheE.coltcells.Itcanbereleasedfromthecellsbythepore-formingactionofcolicinEI,andcanbedetectedrapidlybyenZymatic..thodl.Colici.,areplasmid-encodedproteins,bindspecificallytoparticularreceptorsontheoutermembraneofsensitivecellsan.dactmainlythroughtwopathways'.Beca.s.theycanformporesinthemembrane,colicinshavebeenwidelyusedastoolstostudythebiologicalandphy…     

Analysis of vitamin E in food and phytopharmaceutical preparations by HPLC and HPLC-APCI-MS-MS

Summary The analysis of α, β, γ, δ-tocopherols, trienols, α-tocopheryl acetate and nicotinate (vitamin E) in complex matrices was carried out using a new liquid chromatographic (HPLC) method giving better separation efficiency, selectivity and sensitivity than that described in the literature. The use of normal-phase (NP)-HPLC on silica gel with issoctane-diisopropylether-1,4-dioxane as optimized mobilepphase yielded higher resolution than conventional reversed-phase (RP)-HPLC using methanol mobile phase. Identification of peaks was by UV-absorbance at 295 nm, diode array, or fluorescence detection (λ _ex = 295 nm,λ _ex = 330 nm). The latter was found to be more selective and ten times more sensitive than UV-absorbance detection. A quadrupole, ion-trap mass spectrometer with an atmospheric-pressure ionization (APCl) interface was used to detect vitamin E constituents in the femtomole range. With collision-induced dissociation (CID) in the ion source, which gave characteristic fragmentation, the identity of the investigated compounds could be confirmed. Plots of peak area versus amount injected allowed quantitation of α, β, γ, δ-tocopherols and-trienols, α-tocopheryl acetate and nicotinate in real samples such as peanut, almond, spinach, spelt grain bran, latex and tablets. The method described offers fast identification and quantitation of vitamin E constituents of complex biological origin. Dedicated to Professor Dr. Heinz Engelhardt on the occasion of his 65^th birthday.     

A new model for nanoscale enamel dissolution

The dissolution kinetics of human tooth enamel surfaces was investigated using nanomolar-sensitive constant composition (CC) and in situ atomic force microscopy (AFM) under simulated caries formation conditions (relative undersaturation with respect to hydroxyapatite = 0.902, pH = 4.5). Scanning electron microscopic (SEM) examination of the resulting etched enamel surfaces showed that deminerzalization, initiated at core/wall interfaces of rods, developed anisotropically along the c-axes. After an initial rapid removal of surface polishing artifacts, the dissolution rate decreased as the reaction proceeded in accordance with our recently proposed crystal dissolution model, resulting in hollow enamel cores and nanosized remaining crystallites, resistant to further dissolution. Generally, dissolution of minerals is regarded as a spontaneous reaction in which all the solid phase can be dissolved in undersaturated solutions. However, the dissolution of some biominerals may be suppressed when the crystallites approach nanometer size. This study shows that CC demineralization of enamel in acidic medium follows this new model that can be used to mimic carious lesion formation. In dissolution studies, nanosized enamel crystallites exhibit a remarkable degree of self-preservation in the fluctuating physiological milieu.     

A new method for dissolution of silica gel in a pentafluoropropionyl fluoride—tertiary amine system

A new procedure for the preparation of amino complexes of silicon tetrafluoride was proposed. For this purpose, silica gel is dissolved in a fluoroanhydride—methanol system at room temperature followed by the precipitation of SiF₄ solvate that was formed with tertiary amine (pyridine, 1,10-phenanthroline, 2,2′-bipyridyl). The yields of the formed complexes are 69–83%. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 421–423, March, 2007.     

A new method for testing polymer gear wear rate and performance

This paper provides details of a new test rig design and methodology intended for, and successfully applied to, measuring the gear wear rate and performance of polymer composite gears under both dry and lubricated conditions. One of its unique contributions is that it continuously measures the gear wear rate, a feature essential for understanding polymer gear behaviour. While sharing some concepts with the traditional back-to-back test configuration used for steel gears, the new method introduces a rotary freedom to the block supporting the polymer gears under test. This block rotates if the gear tooth thickness is reduced, which aids control of the test load. The gear surface wear rate is recorded continuously by using a capacitance transducer to measure the pivot block motion. A second unique contribution of the new test method involves splitting the support block so that controlled misaligned gear engagements (not reported in other designs) can be introduced and subsequent changes to wear behaviour studied. The paper first outlines the test rig concepts and design before discussing in more detail the gear wear rate measuring principles, the methods of centre distance adjustment and the achievement of virtually constant gear loading. Finally, a selection test results are presented in summary to further validate the new test method and illustrate potential applications.     

Unifying criteria for dissolution kinetics of various hydroxyapatite preparations

A powder suspension method has been used to study the dissolution rate behavior of various hydroxyapatite (HAP) preparations in acidic media containing different levels of calcium and phosphate. Despite the reported variabilities in the properties among differently prepared samples, the present study indicates that, with regard to the dissolution rate behavior, there is an important common characteristic dissolution rate component. There appears to be a dissolution site common to most HAP preparations that may be associated with the predominant surface of the HAP crystal. Also, an attempt is made to correlate the dissolution rate data with the study of Young and Holcomb on the properties of different HAP preparations.     

A new spectrophotometric method for the determination of promethazine-HCl from pure and pharmaceutical preparations

Promethazine-HCl reacts with potassium persulphate to give a pinkish red color complex exhibiting maximum absorbance at 515 nm. The reaction is selective for promethazine-HCl, with 1 μg/mL as visual limit of identification and provides a basis for a new spectrophotometric determination method. The color forming reaction obeys Beer's Law from 0.001 to 0.125 mg/mL of promethazine-HCl. The relative standard deviation does not exceed 0.005 mg/mL. The method is successfully applied to pure and pharmaceutical formulations of promethazine-HCl. The quantitative assessment of tolerable amounts of possible interferants was also studied. The results are reproducible within ±1% and in good agreement with those obtained by the standard procedure.