Fine Chemical Technologies

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Vol 10, No 1 (2015)
View or download the full issue PDF (Russian)
4-12 277
The article is devoted to the history of the construction of the physicochemical building of the Moscow Higher Women's Courses (1907-1908) on Malaya Tsaritsinskaya street, now the MITHT named after M. V. Lomonosov building on Malaya Pirogovskaya street.


13-28 223
In this paper were analyzed the prognostic opportunity of some semi-empirical methods (additive, additive-correlation, QSPR-methods) used to calculate enthalpies of vaporization (298.2K) acyclic oxygen-containing compounds. Used literature data and our own experimental research by the author in the development of the concept of molecular connectivity based on the index approach is proposed QSPR-method for the calculation of enthalpies of vaporization (298.2K) with high accuracy for the esters and ethers, aldehydes, ketones, alcohols and carboxylic acids.
29-33 230
The thermodynamic efficiency of the rectification process as quoted in various credible scientific sources is estimated to be 5-15%. An evaluation of the rectification process efficiency was proposed where consideration is given to the expenses of heat in the boiler and to the difficulty and the quality of the separation process.
34-38 174
On example of the А+В↔С reaction which is situated in zeotropic mixture the different variants of separation unit design are suggested. Presented separation unit includes both two simple distillation columns and one side stream column. The separation unit allows obtaining high values of reagents conversion. The reactive distillation flow sheets are suggested also. Obtained results are confirmed by numerical simulation.and the quality of the separation process.
39-44 180
The analysis of splitting diagrams of multicomponent multiphase systems was made. Euler characteristics was considered as topological invariant of phase diagram of liquid-liquid equilibrium. It was established that a certain value of the Euler characteristics corresponds to each type of splitting diagram and a geometrical image of heterogeneous area was determined. The suggested method is universal and can be applied to systems with any number of splitting binary constituents and with different structure of binodal variety.


45-49 198
The synthesis of a series of N-substituted arylheteraaliphatic amino amides was carried out to determine their antiarrhythmic activity. Styrene oxide was the initial compound for the synthesis. Its oxirane ring was opened with N,N-dialkylaminoethanols in the presence of alcoholates. It was found that the opening of the oxirane ring was carried out mainly according to the Krasusky rule on the bond between the oxygen atom and the less substituted carbon atom. A mixture of two products with the predominance of the secondary amino alcohol was created. The main product was separated by multiple vacuum distillations. 2-[2-(Dialkylamino) ethoxy]-1-phenylethanols were obtained and used in the Ritter reaction for the alkylation of benzonitrile in the presence of sulfuric acid to give N-{2-[2-(dialkylamino)ethoxy]-1-phenylethyl} benzamides. Biological tests of the obtained compounds were carried on the aconitine arrhythmia model out in rats. Procainamide, Quinidine, Lidocaine and Ethacyzin were used as the drugs. The findings in this study indicate that most of the obtained compounds have a low toxicity and expressed antiarrhythmic activity.
50-55 494
In this paper we studied the effect of melatonin at three concentrations on the formation of 8-oxo-2'-dioxyguanosine (8-oxo-dG) under the conditions of the Fenton reaction. Reproducible kinetic curve of 8-oxo-dG accumulation in this reaction was obtained by the method of reversedphase high performance liquid chromatography with amperometric detection. When adding melatonin in all three concentrations studied, there was a noticeable change in the shape of the kinetic curve with a significant decrease in the amount of detected 8-oxo-dG in most of its control points. This suggests the melatonin inhibition of 8-oxo-dG formation in the reaction and confirms the hypothesis of a direct, non-hormonal, antioxidant effect of melatonin. However, the dependence of the inhibitory effect of melatonin on its concentration is not a straight line. The higher of the studied concentrations of melatonin (60 mg/ml) gave the least pronounced effect.
56-59 196
This article describes a new method of determining concentration of active ingredient in diclofenac-loaded polymer microspheres by using HPLC analysis. Proposed method showed better repeatability than more commonly used UV-Vis spectrometry. Isocratic liquid chromatograph with Luna C18 (2) Phenomenex column and UV detector (254 nm) was employed. Various parameters, such as specificity, repeatability, limit of quantification and stability, were measured to validate the method. Chromatogram showed only diclofenac-related peaks, which means specificity was adequate. Recovery was determined using 5 standard diclofenac solutions with known concentration. Repeatability and reproducibility were calculated based on data from two series of microspheres. LOQ was found using standard curve. Stability was observed during 30 days since sample preparation. Based on these results, suggested method successfully passed the validation process and can be used for quality control of diclofenac-loaded microspheres.
60-65 208
Methods for creations of oxaliplatin liposomal form in laboratory scale are discussed in this mini-review. Analysis of existed methods has been carried out, and the estimation of their usage in pharmaceutical industry view has been given. Oxaliplatin is one of the modern anticancer medicines, which is used both in monotherapy and in combination with other anticancer agents. One of the disadvantages of oxaliplatin as an anticancer drug is high neuro- and cardiotoxicity, which can be reduced by the creation of its liposomal form. In most methods, PEG-conjugated lipids were used as a part of phospholipids’ bilayer. Cationic liposomes modified with DSPE (distearoyl phosphatidyl ethanolamine)-PEG2000, with composition PC (phosphatidyl choline)/ Chol (cholesterol)/DSPE-PEG2000 (2/1/0.2 molar ratio) showed in vivo higher efficiency against human carcinoma SW480 line on mice both in comparison with a control group and with a free oxaliplatin treated group. Moreover, the absence of cachexia, in case of liposomal oxaliplatin was noted. Also, the influence of Chol on liposomes stability was studied. It was discovered that addition of 40% mol of Chol to liposomes with HSPC (hydrogenated soybean PC)/DSPCPEG 2000 increased encapsulation by 8% within 24 h at 37°C. Comparison of trehalose and L-arginine for liposomes HSPC/Chol/PEG2000 was carried out. Both cryoprotectors showed appropriate stability results in a ratio of 1 : 4 to lipids. As a conclusion, liposomal oxaliplatin is a prospective medicine with less toxicity and higher efficiency against tumors in comparison with a free oxaliplatin.


66-71 224
We present the synthesis of new biuret complexes NH2CONHCONH2 (BU), PrBr3·2BU·4H2O (I) and HoBr3·2BU·4H2O (II), and the results of X-ray diffraction analysis. In the crystals of I and II we find complex cations [Ln(H2O)4(BU)4]3+ (Ln = La, Gd) and uncoordinated halogenide ions existing in the external sphere. Biuret molecules serve as bidentate ligands (through the oxygen atoms) and are transformed from the original trans- to cis-configuration. The coordination polyhedron is a distorted square antiprism. These compounds have one or two non-coordinated molecules of water and one non-coordinated BU molecule (II) existing in the external sphere, which are joined with the halogenide ions by hydrogen bonds.
72-75 189
Liquid extraction is a promising method of aluminum extraction from potassium bittern (mother liquors) solutions. Extractants are nitrogen containing chelating phenol type compounds, namely: N-(2-hydroxy-5-nonylbenzyl)-β,β-dihydroxyethylamine (NBEA-0) and N-(2-hydroxy- 5-nonylbenzyl)-β-hydroxyethylmethylamine (NBEA-2) dissolved in a mixture containing 75% vol. of octane + 25% of octanol. The most effective extraction parameters are as follows: extraction time 15 min, contamination of K2CO3 350 grams per liter, alkali concentration 4.5 M, concentration of the extractants more than 0.3 M. Under given conditions metal: extractant ratio is 1:1. The back-extraction was presumed to be performed using 3.5 М alkaline solutions. It was determined that results obtained when NBEA-0 was used as an extractant are insignificantly better in comparison with using NBEA-2.
76-82 228
Niobium and tantalum methylates with common formula M2(OMe)10 , where M - Nb,Ta, have been synthesized as precursors by electrochemical synthesis for obtaining niobium and tantalum oxides. Ultradispersed and nanosized oxides TT (δ)-Nb2O5 and T (γ)-Ta2O5 were obtained by supercritical fluid technology. The samples are characterized by different methods (chemical analysis, DTA-DTG, XRD, IR-spectroscopy, grain size analysis). It is shown that under the experimental conditions amorphous particles of niobium and tantalum pentoxides are formed, which react to form the crystalline state at temperatures of 600°C and 750°C respectively. Crystallization temperature of T(γ)-Ta2O5 obtained by SAS-technology significantly lower than the crystallization temperature of the same tantalum pentoxide obtained by heterophasic method (900°C). The particle size of the annealed tantalum pentoxide is in the range of nanosized materials, particle size of the annealed niobium pentoxide qualifies them as ultradispersed.


83-89 151
Dissipative effects are investigated by means of relaxation spectrometry in films of polyvinyl alcohol with various molecular weight and hydration degree. Peaks of mechanical loss reveal two relaxation transitions (α- and β-peaks) and one first order phase transition (δ-peak). It is found that decrease of hydration degree and increase of crystallinity degree in polyvinyl alcohol essentially increases temperature of α-transition. The α-peak shifts to the higher temperatures area with growth of the molecular weight. Situation of the β-peak does not depend on molecular weight but changes depending on hydration degree. Change of oscillation frequency is noted in area of α- and β-transition, which is indicative of shear modulus defect.

ISSN 2410-6593 (Print)
ISSN 2686-7575 (Online)