


Vol 79, No 9 (2024)
REVIEWS
Methods of organic compounds isolation from solid samples. 2. Extraction under sub- and supercritical conditions. Matrix solid-phase dispersion. The QuEChERS method
Abstract
The second and final part of the review. General information is provided on extraction under sub- and supercritical conditions (liquid extraction under pressure, subcritical water extraction, supercritical fluid extraction), the matrix solid-phase dispersion method and the QuEChERS method. Based on the analysis of the review papers, information on the specifics of sample preparation using these methods is systematized, experimental parameters affecting the extraction efficiency are considered, examples of the use of these methods for the isolation of organic compounds in the analysis of solid environmental objects, food and plants are given.



ORIGINAL ARTICLES
Digital colorometric analysis of aqueous and water-organic systems using hydrophilic crosslinked polyvinyl alcohol–magnetite composite films
Abstract
The use of the crosslinked polyvinyl alcohol–magnetite composite films as sensitive elements for determining the composition of aqueous solutions by digital colorimetry is described. A new approach to the production of composite materials of the composition hydrophilic polymer–magnetite by precipitation of Fe3O4 particles in ammonia vapor is proposed. The sensor films obtained in this way were used to determine the volume fraction of alcohol in products with a high alcohol content. The limit of ethanol determination was 63 vol.% isopropanol – 24 vol.%. The proposed sensory materials have been tested in the analysis of liquid hand antiseptics.



Fluorescent azolotriazines-based test systems based for the diagnosis of endometritis in cows on site conditions
Abstract
The results of an experiment on testing the possibility of using solutions of 6-oxo-2-phenylimidazo[1,2-b]pyrido[4,3-e][1,2,4]triazine-7(6H)-yl)acetic acid on tablets and cellulose carriers to register the excessive, relatively biologically normal, content of volatile organic compounds that accompany inflammation of the endometrium have been considered. The fluorescent properties of the dye were studied using gynecological mucus of cows taken at different periods (before and after parturition) and nasal mucus of newborn calves. The response of the test systems was compared with clinically established diagnoses of cows and the results of microbiological studies. False-positive (no more than 11%) and false-negative (2%) responses, other characteristics (specificity, correctness, precision) of test systems based on 6-oxo-2-phenylimidazo[1,2-b]pyrido[4,3-e][1,2,4]triazin-7(6H)yl) acetic acid were evaluated. The possibility of using this fluorophore for the express diagnosis of endometritis inflammation in cows in the “on-site” mode is considered.



Experimental and theoretical study of the manifestation of the main background single- harge arid ions ArM+ in the inductively coupled plasma mass spectrometry method
Abstract
Single-charge background argid ions ArH+, ArN+, ArO+ and Ar2+ create very strong spectral interference in elemental and isotope analysis by inductively coupled plasma mass spectrometry (ICP-MS). The behavior of these basic background argid ions under ICP-MS conditions is experimentally investigated depending on the high-frequency plasma power and the velocity of the argon transporting stream. Theoretically, the behavior of these argid ions has been studied by thermodynamic modeling with varying plasma temperature and velocity of the transporting argon stream. The general patterns of changes in the intensity of the main background argid ions and the efficiency of their formation with varying operational parameters of inductively coupled plasma are noted. A good coincidence of the experimental and theoretical dependences obtained has been achieved.



Determination of trace element composition and u-pb dating of apatite by inductively coupled plasma mass spectrometry and laser ablation on NexION 300S with NWR 213 accessory
Abstract
The trace element composition and isotope ratios of Pb/U, Pb/Th and Pb/Pb in apatite were determined by inductively coupled plasma mass spectrometry and laser ablation (LA) on a NexION 300S device with a NWR 213 laser ablation accessory, and the procedure for processing experimental data was described. The optimal performance parameters of the mass spectrometer and the laser attachment were determined, including in determining the trace element composition and U/Pb dating from a single crater with a size of 50 μm or more. Standard synthetic glasses NIST SRM-612, -610 were used to determine the trace element composition of apatite; reference samples (RS) were used to measure isotope ratios – Durango, Mun Mad and Mud Tank apatites analyzed in laboratories in different countries. According to scanning electron microscopy data, the shape of laser ablation craters in apatite RS grains was analyzed; significant grain heterogeneity in the content of matrix and impurity elements was shown. The metrological characteristics of the methods for the measurement period 2021-2023 are presented. The repeatability of measuring the isotope ratios of 206Pb/238U and 208Pb/232Th is 0.54 and 0.72, 7.5 and 14.3, 1.5 and 4.4% for Mun Mad, Durango, Mud Tank, respectively. The variations in REE content in the reference samples (sr) are 11-24, 5-13, 0.3–7% for Mun Mad, Durango, Mud Tank, respectively. The dating of apatite OS within the limits of uncertainty corresponds to those obtained in world laboratories. The methods were tested in the analysis of a number of apatite samples from Ural sites.



Application of a composite based on magnetite nanoparticles, graphene oxide and ionic liquid for the extraction of bisphenol A from bottom sediments by matrix solid-phase dispersion
Abstract
A composite based on Fe3O4 nanoparticles, graphene oxide and ionic liquid (1-butyl-3-methylimidazolium-2-carboxylate) is proposed as a sorbent for the extraction of bisphenol A (BPA) from bottom sediments by matrix solid-phase dispersion (MSPD). The saturation magnetization of the synthesized sorbent was 34 emu/g. Grinding of bottom sediments and subsequent grinding with the sorbent was carried out in a ball mill. Some stages of MSPD are partially automated, in particular the procedures of magnetic separation, BPA desorption and sorbent regeneration. The degree of extraction of BPA under experimentally selected conditions (sorbent weight is 0.5 g, the time required for grinding the sorbent is 5 minutes) is 94%. The sorbent can withstand four sorption-desorption cycles without loss of sorption capacity. To clean the matrix from interfering influences, washing with n-heptane is proposed. Bisphenol A was determined by gas chromatography-mass spectrometry after derivatization with acetic anhydride. The analytical characteristics of the method were established using model samples of bottom sediments that artificially polluted BPA. The limit of determination by the developed method was 0.1 μm/kg, the linearity interval of the calibration graph was 0.3–12 μm/kg (r2 = 0.994). The bottom sediments selected near the discharge of the Voronezh wastewater treatment plants (Voronezh River and Don River) were used as real objects for analysis. The concentration of BPA in bottom sediments was 3.83–6.52 μm/kg.



Magnetic solid-phase extraction with dispersion of magnetic hypercrosslinked polystyrene with carbon dioxide for the isolation of amphenicols from honey and milk in their determination by HPLC-MS/MS
Abstract
The magnetic solid phase extraction method with the dispersion of magnetic hypercrosslinked polystyrene (MHCPS) with carbon dioxide is proposed for the isolation and concentration of amphenicols (chloramphenicol, florfenicol and thiamphenicol) from honey and milk before their determination by HPLC-MS/MS. Effervescent tablets consisting of sodium bicarbonate, citric acid and MHCPS in the case of honey, sodium bicarbonate and MHCPS in case of milk were used. The conditions for the preparation of tablets (the amount and ratio of acid, base and MHCPS in the composition of the tablet and its mass) were selected, ensuring the quantitative isolation of amphenicols. Methods for the determination of amphenicols in honey and milk with dispersion of the sorbent with carbon dioxide and subsequent determination of compounds by HPLC-MS/MS have been developed. The limits of determination were 0.3–1 and 0.02–0.05 µg/kg for honey and milk, respectively.



Selective voltammetric determination of dopamine on an electrode modified with palladium particles and a molecular imprinted polymer from nicotinamide
Abstract
A method for manufacturing a glass-carbon electrode with electrodeposited palladium particles and a molecular imprinted polymer from nicotinamide for the determination of dopamine in the presence of structurally related compounds has been developed. The use of a polymer with specific recognition centers complementary to the template molecule led to an increase in the sensitivity and selectivity of dopamine detection. Immobilization of palladium particles on the electrode surface made it possible to increase the selectivity of the voltammetric determination of dopamine in the presence of adrenaline and norepinephrine. The potential difference of the oxidation peaks of these compounds is 200 mV. The linear bilogarithmic dependence of the analytical signal on the dopamine concentration is observed in the range from 5.0 × 10–9 to 5.0 × 10–3 М. The proposed method was tested in the analysis of urine samples.



IN THE SCIENTIFIC COUNCIL FOR ANALYTICAL CHEMISTRY OF THE RAS
Council Bureau meeting


