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Volume 74, Nº 2 (2019)

Article

Digital Colorimetry: Analytical Possibilities and Prospects of Use

Schults E., Monogarova O., Oskolok K.

Resumo

We analyze and systematize publications in the field of digital colorimetry over the past 15 years. Different versions and possibilities of the method are considered; the fields of its application and the prospects for use in chemical analysis are noted. Colorimetric units based on household optical gadgets (smartphones, office flatbed scanners, etc.) that enable the obtaining of raster images are described.

Moscow University Chemistry Bulletin. 2019;74(2):55-62
pages 55-62 views

Sample Preparation, Identification, and Determination of Twelve Macrolides in Raw Food Materials and Food Products Using High-Resolution Mass Spectrometry

Amelin V., Bol’shakov D.

Resumo

A simple technique for the isolation, identification, and determination of 12 macrolide antibiotics (azithromycin, roxithromycin, josamycin, spiramycin I–III, tilmicosin, tylosin, erythromycin, clarithromycin, tylvalosine, and tulathromycin) in raw food materials and food products is developed based on high-resolution time-of-flight mass spectrometry. The range of the detected macrolide content is 1–400 ng/g, the limits of detection are 0.01–0.50 ng/g, and the limits of quantification are 0.04–2 ng/g. A scheme for identification and quantification of the detected antibiotics using the standard addition method is proposed. The relative standard deviation of the analysis does not exceed 21%. The duration of the sample screening is 40 min and the time required for quantification of the detected antibiotics is 1.0–1.5 h.

Moscow University Chemistry Bulletin. 2019;74(2):63-69
pages 63-69 views

Mechanism of the C=C Bond’s Migration in Allyl Phenyl Sulfide during Catalysis by Methanesulfonic Acid

Mityagin D., Gabbasova I., Anisimov A., Kantor E.

Resumo

The mechanism of the C=C bond’s migration in allyl phenyl sulfide in the presence of methanesulfonic acid is analyzed by quantum chemistry using the density functional theory in the B3PW91/6-31G** approximation. The reaction proceeds through the formation of 1-(phenylthio)prop-2-ylium and 2-methyl-1-phenylthiiranium. The calculations show the possibility of the protonation of allyl phenyl sulfide and deprotonation of the resulting cation to phenyl propenyl sulfide. The possibility of the opening of the thiiranium cation under the action of methyl sulfonate to form a complex of phenyl propenyl sulfide with methanesulfonic acid is also shown. Comparison of the results of calculations with and without a solvent shows that the energy profile of the reaction (ΔG2980, and ΔEtotZPE) is practically preserved.

Moscow University Chemistry Bulletin. 2019;74(2):70-73
pages 70-73 views

Synthesis of the 1,3-Benzotellurazole-2-Thiol Derivatives Alkylated in the Thiol Group

Ali A., Ramazanova P., Tafeenko V., Aslanov L., Tarakanov A., Anisimov A.

Resumo

The structure of 1,3-benzotellurazole-2-thiol derivatives was determined by IR and NMR spectroscopy, mass spectrometry, and X-ray diffraction.

Moscow University Chemistry Bulletin. 2019;74(2):74-78
pages 74-78 views

The Study of the Stability of Colloid Dispersions of Copper Nanoparticles Based on Sodium Dodecyl Sulfate

Begletsova N., Selifonova E., Zakharevich A., Chernova R., Sevostyanov V., Glukhovskoy E.

Resumo

Methods for the synthesis of copper nanoparticles in a micellar solution of an anionic surfactant, sodium dodecyl sulfate, are improved by optimizing the molar ratios of the precursor and the reductant, Cu(II): N2H4 of 1 : 4, 1 : 8, 1 : 20, 1 : 40, 1 : 100, and 1 : 150 at a pH of 11.1 and pH values of the reaction medium of 10.9, 11.0, 11.2, and 11.9 at the optimum Cu(II): N2H4 molar ratio of 1 : 150. The effect of increasing the Cu(II) : N2H4 molar ratio on the growth in the absorbance of suspensions of copper nanoparticles is established. The stability of solutions over time is studied using the spectrophotometric analysis of colloidal dispersions of copper nanoparticles obtained at a Cu(II) : N2H4 molar ratio of 1 : 150 and values of pH of 10.9, 11.0, 11.2, and 11.9. The process of the aggregation of copper particles accompanied by a hypsochromic shift of the absorption band of surface plasmon resonance towards larger wavelengths is studied by dynamic light scattering. Scanning electron microscopy has shown that copper particles obtained at a Cu(II) : N2H4 molar ratio of 1 : 150 and pH values of 10.9, 11.0, and 11.2 have a spherical shape with dimensions in the range from 12 to 176 nm.

Moscow University Chemistry Bulletin. 2019;74(2):79-87
pages 79-87 views

Adsorption of Nitrophenols from Aqueous Media by N-Vinylpyrrolidone-Based Polymeric Adsorbents

Sukhanov P., Kushnir A.

Resumo

The adsorption of nitrophenols by N-vinylpyrrolidone-based polymeric adsorbents is studied under static conditions. The adsorption constants and energy characteristics are calculated. The adsorption mechanism and correlations between partition coefficients and adsorbate hydrophobicity are revealed. The contribution of hydrophobic and specific interactions to the adsorption mechanism is substantiated. The studied polymers are recommended for concentrating and extracting nitrophenols from aqueous solutions.

Moscow University Chemistry Bulletin. 2019;74(2):88-92
pages 88-92 views

Study on the Solubility of Ketoprofen From Solid Dispersions with Polyvinylpyrrolidone

Beliatskaya A., Krasnyuk I., Krasnyuk I., Stepanova O., Abgaryan Z., Kudinova T., Vorob’yov A., Nesterenko I.

Resumo

The solubility of ketoprofen (nonsteroidal anti-inflammatory drug) from solid dispersions based on polyvinylpyrrolidone (PVP-10000, PVP-12600 and PVP-24000) is studied. The use of solid dispersions (SDs) increases the solubility and dissolution rate. The solubility of ketoprofen from SD increases by 1.5–2.6 times. The rate of dissolution from SDs increases by 1.5–3.2 times. The studies conducted by a complex of physical and chemical methods suggest that an improved release of ketoprofen from SDs is due to the generation of solid solution of the active substance in the polymer, the formation of intermolecular hydrogen bonds of the active substance with polyvinylpyrrolidone and the solubilizing effect of the polymer during the dissolution of ketoprofen. The results obtained can be used in the development of fast-dissolving solid dosage forms of ketoprofen with enhanced bioavailability.

Moscow University Chemistry Bulletin. 2019;74(2):93-99
pages 93-99 views