. A procedure of sample preparation of oil samples for the determination of chloride ions, which are part of high- molecular organic compounds, has been developed. The procedure consists in the extraction of chloride ions from oil into the aqueous phase with a solution of sodium nitrate, followed by ionochromatographic detection. The work was performed on a high- performance LC-20 Prominence liquid chromatograph with LC Solution software (Shimadzu, Japan), equipped with a conductometric detector (CDD-10 Avp/10Asp), a 120x5 mm KanK-ASt14 mu m separating column (GEOHI RAS, Russia) and a 200x6 mm SPS-SAC 50 suppression column mu m (LLC PC << Aquilon >>, Russia). A carbonate buffer solution (2.5 mM Na2CO3 + 3.0 mM NaHCO3) was used as an eluent. The volume of the injected sample is 100 mu l. The eluent flow rate was 2.0 ml/min. The temperature of the column thermostat is 33 C-degrees. Under these conditions, satisfactory separation of fluoride, chloride, nitrate, and sulfate ions is achieved, and hydrogen sulfide does not have ionic forms and does not manifest ionochromatographically. Using the method of full factorial experiment, the main parameters determining the efficiency of extraction of chloride ions from the organic phase were optimized: extraction of 1 mM with an aqueous solution of

In this work, polyhydroxyalkanoates- based microparticles containing antibacterial drug rifampicin were obtained. The main characteristics of the microparticles were investigated: the particles yield, encapsulation efficiency and drug loading, average radius, surface morphology, polydispersity index, zeta potential and cytotoxicity towards HeLa cells. Loading of RIF into microparticles leads to the substantial decrease of its cytotoxicity.

An ICP-AES method with Concentration Ratio Calibration (calibration in relative concentrations) makes it possible to improve significantly the metrological characteristics of certified reference materials (metals, alloys, technical and geological materials). The main reasons for this improvement are the advantages of the ICP-AES in combination with the advantages of the Concentration Ratio Calibration. The errors of sample weighting and the uncertainty of final volume, as well as the error attributed to the addition internal standard aliquot are excluded from the total error of analysis. Lithium hydroxide fusion in silver crucibles has been developed for the complete transfer of the ilmenite and zirconium concentrates, as well as Mg- and Cr- based refractories into solution. Compared with fusion with lithium metaborate in platinum crucibles, the proposed method is advantageous for a significantly lower cost of crucibles, higher solubility of the melt, and possibility of boron determination as an impurity in the analyzed materials. When certifying the reference samples, it is necessary to use the main principle of Concentration Ratio Calibration, i.e., the total amount of certified mass fractions and positive errors of the components to be determined should not exceed 100 % even when the ICP-AES method is not used. While conventional calibration methods use one-dimensional space and one-dimensional traceabihty the concentration ratio calibration works in re-dimensional space and provides higher accuracy of results due to n-dimensional traceabihty It is necessary to develop a theory of re-dimensional traceabihty which will provide a more reliable certification of reference samples in practice than the one-dimensional traceabihty that exists today.

An overview of researches, mainly by foreign specialists, on current available approaches for sampling to study the traces of gunshot residue (GSR) is presented. The comparative characteristics of traditional methods of samples (use of cotton and gauze tampons, blotting paper, textile fabrics, adhesive tapes, adhesives and vacuum samplers), as well as advanced technologies, including special devices and sorbents, are given. The characteristics of samplings from hands, scalp, nostrils, clothes of examined persons as well as procedures, that allow to increase the duration of GSR detection, are described in details. The importance of GSR sustainability over time is noted. On average, the most likely detection periods of particles are less than 1 hour for samples, collected from hands, more than 1 hour for samples from clothes and 2-3 hours for face. It is possible to detect the GSR particles in hair up to 24 h., and in nasal mucus after 6 h. of shot. The methods of identification and determination for analytes of inorganic and organic nature are discussed. The most common methods for determining heavy metal particles are atomic spectrometry, namely atomic absorption with electrothermal atomization and atomic emission. The combination of scanning laser ablation and mass-spectrometry with inductively coupled plasma makes it possible to detect more than 15 analytes in a single sample. Scanning electron microscopy with X-ray detectors is effective for the examination of powder particles. The described methods of sampling complement each other increasing the possibility of evidence base for court proceedings.

A method for the analysis of iron ore raw materials (IORM) using inductively coupled plasma atomic- emission spectrometry (ICP-AES) and Concentration Ratio Calibration (CRC) has been developed. However, the general eq. for calibration by concentration ratios used in analysis of metals and alloys was modified with allowance for the IORM characteristics: all the elements, except sulfur, were represented as oxides, iron was represented as FeO and Fe2O3, and the total of 100% included ignition losses (LOI). A variant of solving the equation is proposed, which allowed us to relate the relative concentrations of the components (the ratios of the mass fraction of the determined components to the mass fraction of iron oxide) to the ratio of the line intensities of the certain element and iron line measured on a spectrometer. The equation takes into account the content of FeO and LOI, which are determined by standard methods of analysis. A method for acid decomposition of the samples in autoclaves heated in a HotBlock 200 system is proposed: a sample weight of 0.25 g was decomposed in closed vessels at a temperature of 150 – 180°C in the mixture of HCl, HF and HNO3. The following components were determined in concentrates and pellets: Fe2O3, Fetot, Al2O3, CaO, Cr2O3, K2O, MgO, MnO, Na2O, P2O5, SiO2, TiO2, Co, Cu, Mo, Ni, Pb, S, V, Zn. The correctness of the developed method is confirmed by the analysis of SS of iron ore and iron concentrates, as well as by comparison with the results obtained by standardized methods. The proposed technique provides iron determination in iron ore raw materials with an accuracy no worse than that specified in GOST 23581, all other components are determined in a wider range of contents and with a higher accuracy.

A device and a method for sample preparation have been developed, which make it possible to implement successive stages of thermal separation of volatile components from a solid (liquid) matrix, their capture from the gas phase by a solid sorbent, and liquid microextraction of sorbates for further gas chromatographic analysis. The device and the algorithm of its application for GC–MS determination of a number of volatile organic compounds from matrices with complex chemical composition have been tested

We propose an algorithm for comparative study of plastic smoking mixtures containing synthetic cannabinoids using gas chromatography in the following configuration: a Crystal 5000.2 chromatograph (Russia) with a quartz capillary column (L = 50 m,  = 0.32 mm) with a grafted phase based on polyethylene glycol modified with nitroterephthalic acid and a flame ionization detector. Plastic smoking mixtures (40 samples) seized from illegal circulation by officers of the Transport Department of the Ministry of Internal Affairs of Russia in the Siberian Federal District were used as test samples. Mathematical processing of chromatograms was performed using Chromatek Analytic 2.5 and Unscrambler 11.0 programs. It is shown that profiles of the volatile polar components of the fillers of plastic smoking mixtures containing synthetic cannabinoids are quite well manifested and reproduced, which gives them a very high identification value. To compare the profiles of impurities, 44 target compounds were selected, which provided the best reproducibility of the areas of chromatographic peaks during repeated measurements. The chromatographic peak areas of the target compounds were normalized, and the Pearson correlation coefficients and the Euclidean distances were calculated. A hierarchical clustering of the obtained data was carried out with construction of the dendrograms demonstrating the levels of the similarity of samples from different lots. It is shown that samples could be assigned to a single batch (recipe) if the Euclidean distances between the corresponding profiles do not exceed 0.14, and the Pearson distances — 0.12 rel.u. An algorithm procedure for the comparative study of plastic smoking mixtures containing synthetic cannabinoids using gas chromatography has been developed. This procedure includes profiling of the impurities, selection of the target compounds, normalization of the areas of their chromatographic peaks and subsequent mathematical processing using cluster analysis and calculation of Pearson correlation coefficients and Euclidean distances. The obtained results allow us to recommend the developed procedure for use in expert studies of smoking mixtures containing synthetic cannabinoids.

Calibration by the concentration ratio provides better metrological characteristics compared to other calibration modes when using the inductively coupled plasma atomic emission spectrometry (ICP-AES) for analysis of geological samples and technical materials on their base. The main reasons for the observed improvement are: i) elimination of the calibration error of measuring vessels and the error of weighing samples of the analyzed materials from the total error of the analysis; ii) high intensity of the lines of base element; and iii) higher accuracy of measuring the ratio of intensities compared to that of measuring the absolute intensities. Calcium oxide is better suited as a base when using calibration by the concentration ratio in analysis of carbonate rocks, technical materials, slags containing less than 20% SiO2 and more than 20% CaO. An equation is derived to calculate the content of components determined in carbonate materials when using calibration by the concentration ratio. A method of ICP-AES with calibration by the concentration ratio is developed for determination of CaO (in the range of contents 20 – 100%), SiO2 (2.0 – 35%), Al2O3 (0.1 – 30%), MgO (0.1 – 20%), Fe2O3 (0.5 – 40%), Na2O (0.1 – 15%), K2O (0.1 – 5%), P2O5 (0.001 – 2%), MnO (0.01 – 2%), TiO2 (0.01 – 2.0%) in various carbonate materials. Acid decomposition of the samples in closed vessels heated in a HotBlock 200 system is proposed. Correctness of the procedure is confirmed in analysis of standard samples of rocks. The developed procedure was used during the interlaboratory analysis of the standard sample of slag SH17 produced by ZAO ISO (Yekaterinburg, Russia).

We propose an algorithm for comparative study of plastic smoking mixtures containing synthetic cannabinoids using gas chromatography in the following configuration: a Crystal 5000.2 chromatograph (Russia) with a quartz capillary column ( L = 50 m,  = 0.32 mm) with a grafted phase based on polyethylene glycol modified with nitroterephthalic acid and a flame ionization detector. Plastic smoking mixtures (40 samples) seized from illegal circulation by officers of the Transport Department of the Ministry of Internal Affairs of Russia in the Siberian Federal District were used as test samples. Mathematical processing of chromatograms was performed using Chromatek Analytic 2.5 and Unscrambler 11.0 programs. It is shown that profiles of the volatile polar components of the fillers of plastic smoking mixtures containing synthetic cannabinoids are quite well manifested and reproduced, which gives them a very high identification value. To compare the profiles of impurities, 44 target compounds were selected, which provided the best reproducibility of the areas of chromatographic peaks during repeated measurements. The chromatographic peak areas of the target compounds were normalized, and the Pearson correlation coefficients and the Euclidean distances were calculated. A hierarchical clustering of the obtained data was carried out with construction of the dendrograms demonstrating the levels of the similarity of samples from different lots. It is shown that samples could be assigned to a single batch (recipe) if the Euclidean distances between the corresponding profiles do not exceed 0.14, and the Pearson distances — 0.12 rel.u. An algorithm procedure for the comparative study of plastic smoking mixtures containing synthetic cannabinoids using gas chromatography has been developed. This procedure includes profiling of the impurities, selection of the target compounds, normalization of the areas of their chromatographic peaks and subsequent mathematical processing using cluster analysis and calculation of Pearson correlation coefficients and Euclidean distances. The obtained results allow us to recommend the developed procedure for use in expert studies of smoking mixtures containing synthetic cannabinoids.

Градуировка в относительных концентрациях является эффективным средством значительного повышения точности метода АЭС-ИСП. В случае геологических материалов при реализации такого способа градуировки необходимо принять во внимание следующие особенности: не все компоненты проб определяются методом АЭС-ИСП; матричные элементы, которые вносят большой вклад в сумму 100 %, могут присутствовать в разных степенях окисления. В настоящей работе разработана схема применения градуировки в относительных концентрациях для геологических материалов.

Background: In the last decade, new psychoactive substances including synthetic cannabinoids (SC) have appeared and are rapidly spreading in the Siberian Federal District of Russia. The determination of the individual composition of the synthetic cannabinoids is very important, first of all, for assessing the risk of harming the health of potential consumers as well as for determining sources of their appearance. Objective: To describe the types of synthetic cannabinoids, the dynamics of their occurrence and distribution in the illegal market of drugs in the territory of the Siberian Federal District (Russia) for the period from January 2009 till December 2018. Compare the results obtained with the SC distribution trends in other countries. Method: A retrospective analysis of databases (narcotic reports, chromatograms, mass-spectrums) obtained from GC-MS studies of 2142 samples taken from illicit trafficking in the territory of the Siberian Federal District (Russia) from January 2009 to December 2018 was conducted. Results and conclusion: During the analyzed period, 61 individual SCs of various types were identified in the studied samples. Of these, the AB-PINACA-CHM, MDMB(N)-2201, CBL-2201, TMCP-2201 were found most frequently (10-24% cases). In single cases JWH-018-Br, JWH-018-CI, JWH-019, MBA-2201 and QCBL (N)-2201 were identified. The share of the other identified individual SC did not exceed 10%. The results obtained are compared with the SC distribution trends in some countries of the Asia-Pacific region, the European Union and Turkey. Creating an objective global picture of the prevalence of SC requires a unified approach to the provision of relevant representative data. (C) 2019 Elsevier B.V. All rights reserved.

This article discusses the analysis of a database, i. e. chromatogram and mass spectra that were received from subdivisions of Criminal Expertise Centre of Directorate for Law Enforcement in Transport Means of Russian Ministry of Internal Affairs for Siberian Federal District and former Main Directorate of Federal Narcotics Control Service of the Russian Federation for Krasnoyarsk Territory within 2012-2016 when studying synthetic cannabinoids samples confiscated from illegal trafficking. Typical profile impurities of synthesis reagents were identified, as well as of substances that are fillers for the most wide-spread classes of synthetic cannabinoids.

For the extraction-fluorimetric determination of nanogram amounts of codeine in human urine the use of the fluorescence of the toluene extract of the codeine ionic associate with eosin was proposed. The formed ionic associate was characterized by the intensive fluorescence with a maximum of 550 nm. It was shown that the fluorescence intensity of the codeine ion associate with eosin in toluene was 10 times higher than the intensity of its luminescence in carbon tetrachloride, and 3 times higher than its intensity in chloroform. The optimal conditions for the formation of the fluorescent ion associate of the positively charged codeine ion with a negatively charged form of eosin were determined. The maximum fluorescence intensity of the ion associate was observed during the toluene extraction from the aqueous solutions with pH of 6 - 8 and the eosin concentration in the range of 1·10 -5 -1·10 -3 mol·L -1 . The fluorescence intensity of the extract was maintained at the initial level for 24 hours. The extraction-fluorometric procedure for determining the nanogram amounts of codeine in human urine was developed. The limit of detection of codeine, calculated by 3s-criterion, was equal to 6 ng·ml -1 . The calibration curve linearity was maintained in the range of 30 – 320 ng·ml -1 . The procedure for the determination of codeine in real expert samples of urine was tested. The relative standard deviation did not exceed 0.08. The obtained results for the extraction-fluorimetric determination of codeine in human urine allowed recommending the developed procedure for its use in the solutions of certain tasks in the practice of the institutions of the corresponding profile. Keywords: Сodeine, determination, human urine, extraction, fluorescence (Russian) DOI: http://dx.doi.org/10.15826/analitika.2017.21.4.006 S.I. Metelitsa 1 , E.V. Kireeva 1 , V.V. Nemikhin 2 , S.V. Kachin 1 , V.N. Losev 1 , S.A. Sagalakov 1 1 Siberian Federal University, Svobodnyi pr., 79, Krasnoyarsk, 660041, Russian Federation 2 Krasnoyarsk Regional Bureau of Forensic Medical Examination, Mira pr., 35, Krasnoyarsk, 660049, Russian Federation