PHYSICAL CHEMISTRY
The nanoparticles of (Mg, Zn)xFe3–xO4 (x ≤ 0.3) solid solutions have been prepared by coprecipitation with Na2CO3 from solutions of salts. For a number of compositions (Mg0,1Fe2,9O4, Mg0,05Zn0,1Fe2,85O4, Zn0,18Fe2,82O4), an increase of saturation magnetization has been detected, as compared to non-substituted magnetite (MS = 64 emu/g). This can be explained by the tendency of zinc and small amounts of magnesium ions to occupy preferentially tetrahedral sites of the magnetite lattice. In the case of zinc and magnesium joint substitution in the (Mg, Zn)xFe3–xO4 system up to x = 0.3, the values of saturation magnetization decrease slightly comparing to that of magnetite, but remain constant (MS ≈ 58 emu/g). By ultrasound assisted dispersion of nanopowders into polyelectrolyte aqueous solutions, colloidal solutions of non-agglomerated nanoparticles have been prepared. Тhe nanoparticles modified with a layer of positively charged polyelectrolyte demonstrate the best sedimentation stability up to 45 days. Their hydrodynamic diameter is lower than 200 nm, with predominance of the fraction with the size of 40–80 nm.
COLLOIDAL CHEMISTRY
Stability of water dispersions of a polyorganosiloxane and TiO2 or mica both in presence of surfactants and without them has been studied at pH 6.7 and 8.7 by nephelometry and granulometry. Aggregate stability of latex-TiO2 system increases with disperse phase concentration, while decreasing for the latex-mica system. Introduction of anionic and nonionic surfactants into mixed dispersions (pH 6.7) leads to increase. Increase of dispersant pH significantly improves dispersancy of powders in the latex without dispersing agent.
ANALYTICAL CHEMISTRY
The membrane composition of molybdate-selective electrodes based on higher quaternary ammonium salts (QAS) has been optimized. It has been found that electrodes with the best analytical characteristics are based on 2,3,4-tris(dodecyloxy) benzyltrimethylammonium bromide (TM), with 4-trifluoroacetylbenzoic acid heptyl ester (HE) as the solvating additive. Their analytical characteristics, such as lower detection limits (5·10−6mol/l); selectivity coefficients to interfering chloride (2·10−3), sulfate (9·10−3), oxalate (2·10−2) and tungstate (5·10−3) ions; working pH range (7.5−8.5); and the slope of the electrode function (28 mV/pC) have been determined. Sodium molybdate aqueous solutions have been studied with FT-IR spectrometry method at various pH, and it has been shown that at pH above 7.5 hydrolysis is not significant. However, for molybdateselective electrodes it is better to use freshly prepared solutions, as it increases the reproducibility of the experimental results.
Method for determination of 69 pesticides from different classes (amides, anilinopyrimidines, dinitroanilines, imidazoles, carbamates, carbanilates, morpholines, neonicotinoids, organodithiophosphates, organothiophosphates, pyrethroids, simmtriazines, esters, strobilurins, thiocarbamates, triazoles, etc.) in winter wheat grain by gas chromatography with mass spectrometric detection has been developed and validated by experimental data. The developed extraction method of sample preparation is simple, quick, consumes only cheap and rather common reagents and provides extracts clean enough to obtain reproducible quantitative results without cleaning of injector liner at least for 200 injections. The recovery values of studied pesticides from winter wheat grain were between 76 and 118 % with RSD values below 9 % at 10.0, 20.0 and 200 µg·kg–1 spiking levels. Detection limits were less or equal to 0.01 mg·kg−1 for all the studied pesticides. The obtained limits of quantification were below or equal to the maximum residue levels (MRLs) which are set by Belarus and the European Union for the corresponding pesticides in cereal grains. The linear range used in the calibration curves was from 50 to 3000 µg·L–1 with the values of the determination coefficients R2 more than 0.997. The developed method was successfully used for the analysis of cereal grains for the residues of the pesticides, which were under registration trials held in Belarus in 2015.
ORGANIC CHEMISTRY
BIOORGANIC CHEMISTRY
Human glutathione S-transferase P1-1 (GSTP1-1) is an important enzyme in clinical diagnostics since its overexpression in solid tumours and lymphomas largely contributes to multiple drug resistance of cancer cells. Small amounts of the enzyme can also be isolated from erythrocytes. However, known isolation methods are disadvantageous and do not allow to obtain the purified enzyme in good yield and with high specific activity (≥ 100 U/mg protein). In order to elaborate more effective purification procedure for the erythrocyte GSTP1-1, we have for the first time synthesized and investigated glutathione-containing affinity membranes based on chemically modified cellulose paper. The membranes have been shown to successfully replace conventional glutathione-agarose affinity gels in the enzyme purification. To isolate and purify GSTP1-1 from erythrocyte hemolysate, a novel two-step method has been developed involving preliminary hemoglobin removal on a small anion exchange column and further affinity chromatography on the cartridge with glutathione-containing membranes. In terms of activity yield (76.5%), purification factor (23589-fold), and specific activity of the purified enzyme (104.5 U/mg), the method is notably superior to previously published procedures. Gel electrophoretic and MALDI-TOF mass spectrometric analyses reveal apparent homogeneity (≥ 95%) of the obtained preparation. Steady-state kinetic parameters have been determined for the purified GSTP1-1 in the conjugation reaction between glutathione and 1-chloro-2,4-dinitrobenzene at pH 6.5 and 25 °С: for the former substrate, Km = 0.19 mМ, kcat = 47.8 s–1; for the latter, Km = 0.68 mМ, kcat = 54.3 s–1. The results of the present work may be useful for screening new enzyme inhibitors with possible antitumour activity. The affinity membranes may also find application in isolating native and recombinant glutathione S-transferase (GST) isoforms from various sources, as well as fusion proteins with GST tag.
TECHNICAL CHEMISTRY AND CHEMICAL ENGINEERING
ОБЗОРЫ
SCIENTISTS OF BELARUS
ISSN 2524-2342 (Online)