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Vol 72, No 6 (2017)

Article

Gradient HPLC Separation of Alkylphosphonic Acids on a Hypercarb Porous Graphitic Carbon Adsorbent with an Aqueous Formic Acid Solution as the Mobile Phase

Goncharova E.N., Semenova I.P., Statkus M.A., Tsysin G.I.

Abstract

An approach to the gradient HPLC separation of alkylphosphonic acids on a Hypercarb porous graphitic carbon adsorbent with an aqueous formic acid solution as a mobile phase is proposed. Analytes were detected using a quadrupole mass spectrometer. To increase the retention of the analytes, the chromatographic column was washed with water before the injection of a sample solution. This procedure results in a three- to fourfold increase in the retention factors of alkylphosphonic acids in comparison with the analogs described in the publications.

Moscow University Chemistry Bulletin. 2017;72(6):255-259
pages 255-259 views

Kinetics of Extraction of Biologically Active Substances from Medicinal Plant Raw Materials using Different Techniques

Milevskaya V.V., Butylskaya T.S., Temerdashev Z.A., Statkus M.A., Kiseleva N.V.

Abstract

The problems and peculiarities of obtaining the kinetic characteristics of extraction of biologically active substances (BAS) from a plant matrix are discussed. The establishment of kinetic characteristics of the extraction of BAS under various extraction conditions is studied on the example of samples of Hypericum perforatum and Salvia officinalis. The lowest value of the average rate constant of the extraction of BAS from the materials examined is characteristic of a variant of static extraction with an aqueous alcohol extractant under heating. The methods of static extraction under heating (according to the requirements of pharmacopoeia articles) and ultrasonication, as well as using double ultrasonication differ little from each other in their kinetic efficiency. The method of dynamic extraction of BAS at an elevated temperature and pressure is characterized by the highest values of the rate constant, which leads to an acceleration of the diffusion of the BAS into the extractant’s medium. It is noted that the extraction processes and chemical transformations of some BAS (hyperforin, carnosic acid, etc.) occur simultaneously as confirmed by the decrease in their concentrations in the extractant during the extraction from plant samples.

Moscow University Chemistry Bulletin. 2017;72(6):260-266
pages 260-266 views

Synthesis of Copper Nanoparticles by Thermal Decomposition of Anhydrous Copper Formate

Vernaya O.I., Epishev V.V., Markov M.A., Nuzhdina V.A., Fedorov V.V., Shabatin V.P., Shabatina T.I.

Abstract

Highly dispersed anhydrous copper formate obtained by cryochemical synthesis is subjected to thermal decomposition in an atmosphere of hydrogen. X-ray diffraction, PAM, UV-spectroscopy, and lowtemperature adsorption of argon show that the obtained powder contains only copper nanoparticles with a size of 50–200 nm.

Moscow University Chemistry Bulletin. 2017;72(6):267-268
pages 267-268 views

Comparative Analysis of Data Obtained by Immunofluorescence Estimation of ERCC1 Expression using Different Clones of Monoclonal Antibodies 8F1 and FL297

Bogush T.A., Mamichev I.A., Kaliuzhny S.A., Polotskii B.E., Zarkua V.T., Tjulandina A.S., Bogush E.A., Davydov M.M.

Abstract

In the present research, we compared two datasets obtained from the quantitative estimation of ERCC1 protein using two monoclonal antibodies—8F1 and FL29. Quantitative evaluation of immunofluorescence parameters was performed by flow cytometry on ovarian cancer biopsy specimens (n = 53). Agreement between two different assays was estimated by correlation analyses and Bland–Altman plots. It was shown that, despite of large spread of differences etween two measurements obtained by 8F1 and FL297, both clones may be used for estimation of ERCC1 expression level (i.e., the number of positively stained cells) in tumor.

Moscow University Chemistry Bulletin. 2017;72(6):269-274
pages 269-274 views

Quantum Chemical Study of Regularities of Electrophilic Substitution in the Synthesis of Pyrroloquinolines

Boyarkina O.V., Tomilin O.B., Yamashkin S.A.

Abstract

It has been shown that the cyclization of the indolylenaminoketones prepared from substituted 5-aminoindoles, which is carried out according to the mechanism of electrophilic substitution, is an orbitally controlled interaction. The formation of pyrroloquinolines with a linear or angular structure is determined by the values of the electronic populations of the frontier orbitals of the interacting atoms.

Moscow University Chemistry Bulletin. 2017;72(6):275-281
pages 275-281 views

2-Mercaptobenzotellurazole Derivatives Obtained Using a Mercapto Group

Ali A.M., Ramazanova P.A., Khibiev K.S., Salim A.S., Tarakanova A.V., Anisimov A.V.

Abstract

Novel 2-mercaptobenzotellurazole derivatives with different functional groups were obtained using its mercapto group.

Moscow University Chemistry Bulletin. 2017;72(6):282-288
pages 282-288 views

Methods for Preparing High Performance Stationary Phases for Anion-Exchange Chromatography

Zatirakha A.V., Uzhel A.S., Smolenkov A.D., Shpigun O.A.

Abstract

The development of new high-performance anion-exchange stationary phases is one of the priority tasks of modern ion chromatography (IC). Most of the research in this field is aimed at improving the selectivity of anion exchangers and increasing the sensitivity, efficiency, and rapidity of the analysis. The selectivity of the stationary phases is largely determined by the chemistry of the adsorbent surface; therefore, it is particularly important to understand the relationship between the structure of the functional layer of the anion exchanger and its chromatographic properties. This review is devoted to methods for modifying polymer matrices in order to obtain highly efficient anion exchangers for the separation of inorganic and organic anions.

Moscow University Chemistry Bulletin. 2017;72(6):289-302
pages 289-302 views

The Use of Microemulsions for the Extraction and Simultaneous Preconcentration of Maltenes as Potential Chemical Markers to Identify Hydrocarbon Deposits

Levkina V.V., Petruk E.S., Popik M.V., Pirogov A.V., Shpigun O.A.

Abstract

The possibility of using microemulsions as extractants during the extraction of chemical markers from oil samples and their subsequent preconcentration by the decomposition of microemulsions and determination of oil components by the gas chromatography-mass-spectrometry method is shown. Due to hydrophobicity, oil components pass into the organic phase after the decomposition of microemulsions and become concentrated due to the reduction of the volume of one of the phases. It is shown that as the preconcentration of the precipitant increases, the preconcentration coefficient of the chemical markers grows to 8–10. The method itself is characterized by low detection limits, good selectivity, and reproducibility.

Moscow University Chemistry Bulletin. 2017;72(6):303-306
pages 303-306 views

A Potentiometric Multisensor System of Anion-Selective Electrodes Based on Ionic Liquids

Shvedene N.V., Rzhevskaia A.V., Aksenova V.A., Pletnev I.V.

Abstract

The possibility of using solid-state and liquid PVC-membrane electrodes based on ionic liquids to design a potentiometric multisensor system is assessed. Ionic liquids with 1,3-dihexadecylimidazolium cation and chloride, bromide, iodide, and nitrate anions are used. The sensitivity parameters of the sensors are determined. A multisensor array is applied to detect chloride and iodide anions in the multicomponent mixture. The designed system is used to discriminate between mineral waters of different compositions by applying the method of principal component analysis (PCA).

Moscow University Chemistry Bulletin. 2017;72(6):307-314
pages 307-314 views

Direct Analysis of Natural Waters by Electron Spray Ionization and High-Resolution Time-of-Flight Mass Spectrometry Detection. Determination of Pesticides of Various Classes

Amelin V.G., Saun’kina M.A., Andoralov A.M.

Abstract

The possibility of directly determining 36 pesticides (derivatives of urea, triazines, triazoles, imidazoles, carbamates, triazinones, benzamides, and pyridazinones and organophosphorus pesticides) by electrospray ionization with high-resolution quadrupole time-of-flight mass spectrometry in natural waters is demonstrated. A significant matrix effect is observed in the determination of pesticides in natural waters, and the use of the standard addition method is proposed for their determination in test samples, both undiluted and diluted with deionized water. The analytical range of the analytes was 0.5–50 ng/mL. The relative standard deviation of the results does not exceed 10%; the time required for the analysis is 10–15 min.

Moscow University Chemistry Bulletin. 2017;72(6):315-321
pages 315-321 views

Development and Validation of the Quantification of GML-1 Compound (N-benzyl-N-methyl-1-phenylpyrrolo[1,2-A] pyrazine- 3-carbamide) in the Blood Plasma of Rats by HPLC–MS

Novitskiy A.A., Bochkov P.O., Litvin A.A., Zherdev V.P., Blynskaya E.V.

Abstract

The technique of quantitative determination of a new compound, possessing anxiolytic activity, GML-1 in the blood plasma of rats is developed and validated. The analysis is performed by HPLC–MS. The method is linear in the range of 50–1000 ng/mL. 83.63% of GML-1 was recovered. The detection limit was 25 ng/mL.

Moscow University Chemistry Bulletin. 2017;72(6):322-324
pages 322-324 views

Gradient Lateral Flow Immunoassay of Human Chorionic Gonadotropin

Serebrennikova K.V., Samsonova J.V., Osipov A.P.

Abstract

A new format for the express method of visual semiquantitative analysis based on the principle of gradient lateral flow immunoassay with gold nanoparticles as a label is proposed. Several test bands with an increasing concentration of specific antibodies immobilized on the membrane are formed in the analytic zone of the test strip. The antigen content is semiquantitatively evaluated visually by counting the number of visible colored bands in the analytic zone. By the example of the human chorionic gonadotropin hormone, the possibility of noninstrumental semiquantitative determination of the antigen in the range from 50 to 10000 mU/mL for 5–10 min was shown in five concentration ranges: under 100, 100–300, 300–500, 500–800, and above 800 mU/mL. The developed semiquantitative express method allows visually determining the concentration range of human chorionic gonadotropin in the urine by the number of colored bands for diagnosing pregnancy and its course.

Moscow University Chemistry Bulletin. 2017;72(6):325-327
pages 325-327 views

Determination of Codeine Phosphate in the Culture Fluid of Rhodococcus by High-Performance Liquid Chromatography

Plotnikov A.N., Karpenko Y.N., Vikhareva E.V., Tyumina E.A., Richkova M.I., Selyaninov A.A.

Abstract

The conditions for the quantitative determination of codeine phosphate in the culture fluid of Rhodococcus by reversed-phase high-performance liquid chromatography (RP-HPLC) are established. The specificity, linearity, precision, and accuracy of the method are confirmed by the validation procedure.

Moscow University Chemistry Bulletin. 2017;72(6):328-332
pages 328-332 views