234 research outputs found

    Comparative investigation of the structure, phase composition, and mechanical properties of Ni-based high-temperature alloys manufactured by different methods

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    A comprehensive comparative study of the structure, phase composition, and mechanical properties of heat-resistant nickel-based Ni-Cr-(X) alloys produced by the methods of traditional metallurgy and self-propagating high-temperature synthesis (SHS metallurgy) is carrie

    РАЗДЕЛЕНИЕ ЭНАНТИОМЕРОВ ТИРОЗИНА, ТРИПТОФАНА И β-БЛОКАТОРОВ МЕТОДОМ КАПИЛЛЯРНОГО ЭЛЕКТРОФОРЕЗА С УЧАСТИЕМ АМИНОКИСЛОТНОЙ ИОННОЙ ЖИДКОСТИ 1-бутил-3-метилимидазолий L-пролинат [C4MIm][L-Pro] В КАЧЕСТВЕ ХИРАЛЬНОГО СЕЛЕКТОРА

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    The current study is devoted to the synthesis of amino acid ionic 1-butyl-3-methylimidazolium L-prolinate [C4MIm][L-Pro] liquid and the investigation of its possibilities as a chiral selector for the separation of amino acids (tryptophan and tyrosine) and β-blockers (carvedilol and propranolol) enantiomers. The following factors affecting the resolution of amino acids stereoisomers under ligand exchange capillary electrophoresis were established: background electrolyte pH, concentration of chelate complex, molar ratio of metal and ligand and its nature. The enantioselectivity values of 1.25 for tryptophan enantiomers and 1.17 for tyrosine enantiomers were observed when the background electrolyte consisted of 50 mM borate buffer (pH = 12.2), 20 mM [C4MIm][L-Pro], and 10 mM CuSO4. The synergetic effect of the synthesized ionic liquid and (2-hydroxypropyl)-β-cyclodextrine when added to the background electrolyte content (20 мМ NaH2PO4, pH = 2.5) was discovered during the separation of carvedilol and propranolol enantiomers. The achieved resolution for carvedilol (Rs = 1.1) and propranolol (Rs = 1.6) enantiomers allowed determining the enantiomers ratio of active ingredients in drug formulations.Keywords: ligand exchange capillary electrophoresis, amino acid ionic liquids, chiral selector, amino acids, β-blockers, synergetic effect, enantioseparation(Russian)DOI: http://dx.doi.org/10.15826/analitika.2018.22.1.004 Kolobova E.A.1, Kartsova L.A.2, Alopina E.V.2, Smirnova N.A.2 1The Nikiforov Russian Center of Emergency and Radiation Medicine,54 Optikov st., St. Petersburg, 199034, Russian Federation2Saint-Petersburg State University, Institute of Chemistry, 26 Universitetskii prospect,  St. Petersburg, Petergof, 198504, Russian Federation Работа посвящена синтезу аминокислотной ионной жидкости (ИЖ) 1-бутил-3-метилимидазолий L-пролинат [C4MIm][L-Pro] и изучению ее возможностей в качестве хирального селектора при разделении энантиомеров аминокислот (триптофан и тирозин) и β-блокаторов (пропранолол и карведилол). Исследованы факторы, влияющие на разрешение стереоизомеров аминокислот в режиме лигандообменного капиллярного электрофореза (ЛОКЭ). Показано, что на разрешение энантиомеров влияют рН фонового электролита, концентрация хелатного комплекса, мольное соотношение «металл : лиганд», природа хирального селектора и металла-комплексообразователя. Значения энантиоселективности разделения, составившие 1.25 для энантиомеров триптофана и 1.17 для энантиомеров тирозина, были достигнуты с использованием фонового электролита, содержащего 50 мМ боратный буфер (рН = 12.2), 20 мМ [C4MIm][L-Pro], 10 мМ CuSO4. При разделении энантиомеров карведилола и пропранолола обнаружен синергетический эффект при совместном введении в фоновый электролит (20 мМ NaH2PO4, pH = 2.5) двух хиральных селекторов –  синтезированной аминокислотной ИЖ [C4MIm][L-Pro] и (2-гидроксипропил)-β-циклодекстрина. Достигнутые значения факторов разрешения для энантиомеров пропранолола (Rs = 1.1) и карведилола (Rs = 1.6)позволили определить соотношения энантиомеров действующих веществ в лекарственных препаратах.Ключевые слова: лигандообменный капиллярный электрофорез, аминокислотные ионные жидкости, хиральный селектор, аминокислоты, β-адреноблокаторы, синергетический эффект, разделение энантиомеровDOI: http://dx.doi.org/10.15826/analitika.2018.22.1.00

    Kinetic regularities, catalyst deactivation and reactivation

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    Funding text 1 The research is funded from Ministry of Education and Science of the Russian Federation Program No. 075–03–2021–287/6 (Russia). Funding text 2 XPS measurements were carried out at the Central laboratories of Tomsk Polytechnic University (Analytical Center). HRTEM was carried out at the Innovation centre for Nanomaterials and Nanotechnologies of Tomsk Polytechnic University. The ICP-OES analysis was carried out using the core facilities of “Physics and Chemical methods of analysis” of Tomsk Polytechnic University. Fundação para a Ciência e a Tecnologia for Scientific Employment Stimulus Institutional Call (CEECINST/00102/2018), UIDB/50006/2020 and UIDP/50006/2020 (LAQV), UIDB/00100/2020 and UIDP/00100/2020 (Centro de Química Estrutural).Betulin, being a pentacyclic triterpene alcohol and an extractive from birch bark, along with its oxo-derivatives, has a broad range of physiological properties of interest for synthesis of pharmaceuticals. Instead of oxidizing betulin with strong and toxic oxidizing agents the present study shows a possibility of using liquid-phase oxidation of betulin with air over supported Ag NPs catalysts as an alternative method for synthesis of its oxo-derivatives. Based on catalytic studies, high resolution transmission electron microscopy, X-ray photoelectron spectroscopy and ultraviolet-visible diffuse reflectance spectroscopy, the evolution of the surface of nanosilver catalysts during the catalysis was demonstrated, as well as under the impact of reactant gas composition. The kinetic regularities and causes of deactivation of supported Ag NPs catalysts were revealed. An approach to the regeneration of silver catalysts was proposed. Kinetic analysis with numerical data fitting was performed resulting in an adequate description of the concentration dependencies.publishersversionpublishe

    ELECTRONIC STRUCTURE OF FeSi

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    The full set of high-energy spectroscopy measurements including X-ray photoelectron valence band spectra and soft X-ray emission valence band spectra of both components of FeSi (Fe K_beta_5, Fe L_alpha, Si K_beta_1,3 and Si L_2,3) are performed and compared with the results of ab-initio band structure calculations using the linearized muffin-tin orbital method and linearized augmented plane wave method.Comment: 11 pages + 3 PostScript figures, RevTex3.0, to be published in J.Phys.:Cond.Matte

    Stocks and fraction composition of phosphorus in the Ili Alatau foothill soils and their change under long-term use

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    In soils of Ili Alatau (dark kastanozems, light kastanozems, mountain chernozems) both in continuous cropping system of sugar beet and in crop rotation with prolonged use of fertilizers the soil agrochemical indices, phosphorus reserves and group composition (total, organic and mineral) vary significantly. The total phosphorus content in the soils was 1720–2330 mg/kg and decreased in the series: virgin mountain chernozems > arable dark kastanozems > arable mountain chernozems > light kashtanozems > virgin dark kastanozems. It was observed, that in arable dark kastanozems, as compared to virgin soils, the content of available forms of phosphorus (loose-bound phosphates Ca-PI and miscellaneous calcium phosphates Ca-PII) increased, and the content of plant unavailable forms of phosphorus (poorly soluble Ca phosphates Ca-PIII, phosphates of aluminum Al-P and iron Fe-P) decreased. In arable mountain chernozems, in comparison with virgin mountain chernozems, the content of all fractions of phosphorus decreased. Arable light kastanozems contain the least amount of available phosphates and the highest of phosphates of aluminum and iron. When cultivating beets on light kastanozems, the content of all fractions of phosphorus, except iron phosphates, increased with increasing dose of fertilizers. The effectiveness of the application of the organic-mineral fertilizers was comparable to the introduction of NK + P1.5 and NK + P2, the yield of sugar beet in the crop rotation in these variants is the highest and amounts to 614 and 577 centner/ha; in the control value (obtained without fertilizers) – 197 centner/ha, and in the variant with application of only NK fertilizers – 277 centner/ha. In continuous cropping system these values were 576 and 561 centner/ha; 311 and 327 centner/ha respectively. Close values of crop yield were obtained in two variants: with the organo-mineral system and NK + P1.5, due to the additional use by the plants of sugar beet phosphorus of newly formed organic compounds

    The study of the sorghum genetic diversity using the mul¬tiplex microsatellite analysis

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    This study is focused on evaluation of the genetic structure and diversity of the national sorghum collection. Analyzing the genetic diversity of crop species is of great importance for genetic resources management and food security of any country. Huge genetic diversity of sorghum provides a great opportunity to improve the agronomic characteristics of this crop. The efficiency of microsatellite  analysis has been demonstrated in many studies on the genetic diversity of different races and geographical groups of sorghum plants. Development of multiplex PCR analysis systems based on a set of polymorphic microsatellite loci will facilitate genetic tests on a large number of plant samples, thus making the research on sorghum diversity more efficient and comprehensive. A system of multiplex PCR analysis based on 12 polymorphic microsatellite loci was developed to perform single-stage high-throughput screening of cultivated and wild forms preserved in the sorghum germplasm collection. As a result of the microsatellite analysis of 200 sorghum plants, 229 alleles were detected. The studied loci showed high polymorphism. More than 17 alleles were identified in most loci, their polymorphic index content (PIC) ranging from 0.694 to 0.954. The value of the effective multiplex ratio (EMR) in the developed system was estimated at 0.833. The microsatellite analysis of sorghum accessions resulted in obtaining quantized gene expressions profiles, with a DNA profile for each accession, and revealed significant polymorphism among the plants of different sorghum varieties (races). The developed multiplex PCR system was shown to be efficient for evaluation of the genetic diversity and genetic relationships of sorghum plants from different races. The analysis of the obtained data using three bioinformatic techniques, NJ cluster analysis, PCoA, and the Bayesian model-based clustering, helped to classify the analyzed sorghum accessions into cluster groups according to their morphological and agronomic traits

    Комбинированная двухуровневая спинально-эпидуральная анестезия с фиксацией эпидурального катетера в подкожном канале с использованием модифицированной спинномозговой иглы

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    Aim of study To develop a new safe and reliable method of fixing an epidural catheter (EC), to study and compare the results of this method of fixing EC in the subcutaneous canal using a modified spinal needle (MSN) and an adhesive tape with a standard method of fixing an EC using only an adhesive tape when performing the combined double-segment spinal-epidural anesthesia (CDSEA) in the surgical treatment of fractures of the bones of the lower limb.Material and methods A comparative study of two methods of EC fixation was carried out in patients undergoing CDSEA during the surgical treatment of fractures of the bones of the lower limb. The patients were divided into two groups. The Group 1 (comparison, n=65), where EC was fixed at the site of epidural access with adhesive tape and the Group 2 (study, n=65), where EC was fixed in the subcutaneous canal using MSN and adhesive tape at the site of EC exit on the skin.Results In the study group, where EC was fixed in the subcutaneous canal using MSN and adhesive tape at the site of EC exit to the skin, there were 32.3% fewer cases with clinically significant dislocation (more than 15 to 30 mm) than in the comparison group, where EC was fixed at the site of epidural access only with adhesive tape.Conclusions A used spinal needle in a modified version can be used to perform EC in the subcutaneous canal. The dimensions of the MSN allow tunneling of the EC less traumatic and at a great distance from the site of the epidural access, which provides more reliable fixation of the EC, the number of cases with clinically significant + dislocation decreases, this allows for a longer and better postoperative epidural analgesia. This method does not solve all the problems of EC fixation; it is required to develop new methods of EC fixation, including fixation in the subcutaneous canal.ЦЕЛЬ Разработать новый безопасный и надежный способ фиксации эпидурального катетера (ЭК), изучить и сравнить результаты данного способа фиксации ЭК в подкожном канале с использованием модифицированной спинномозговой иглы (МСИ) и лейкопластырной наклейки со стандартным способом фиксации ЭК с использованием только лейкопластырной наклейки при проведении комбинированной двухуровневой спинально-эпидуральной анестезии (КДСЭА) при оперативном лечении переломов костей нижней конечности.МАТЕРИАЛ И МЕТОДЫ Было проведено сравнительное исследование двух способов фиксации ЭК у пациентов при проведении КДСЭА при оперативном лечении переломов костей нижней конечности. Пациенты были разделены на две группы: 1-я группа — сравнения, n=65, где ЭК фиксировали в месте эпидурального доступа лейкопластырной наклейкой; 2-я группа — исследования, n=65, где ЭК фиксировали в подкожном канале с использованием МСИ и лейкопластырной наклейки в месте выхода ЭК на кожу.РЕЗУЛЬТАТ В группе исследования, где ЭК фиксировали в подкожном канале с использованием МСИ и лейкопластырной наклейки в месте выхода ЭК на кожу, случаев с клинически значимой дислокации (от 15 до 30 мм) было на 32,3% меньше, чем в группе сравнения, где ЭК фиксировали в месте эпидурального доступа только лейкопластырной наклейкой.ВЫВОДЫ Использованную спинномозговую иглу в модифицированном варианте можно применить для проведения эпидурального катетера в подкожном канале. Размеры модифицированной спинномозговая иглы позволяют провести туннелирование эпидурального катетера менее травматично и на большое расстояние от места эпидурального доступа, что обеспечивает более надежную фиксацию эпидурального катетера, уменьшается количество случаев с клинически значимой наружной дислокацией, а это позволяет проводить более длительную и качественную послеоперационную эпидуральную анастезию. Данный способ не решает всех проблем фиксации эпидурального катетера, поэтому требуется разрабатывать новые способы его фиксации, в том числе и в подкожном канале

    Multiplexed set of 10 microsatellite markers for identification of potato varieties

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    Genetic identification of potato varieties is a demanded instrument for development of new cultivars registration system, protection of plant breeders’ rights, and variety homogeneity control. The most perspective approach for distinction and identification of varieties continues to remain the use of short tandem repeats. STR amplification with the subsequent high resolution electrophoresis allows such a unique characteristic of a variety to be obtained as the DNA profile. A large scale of samples requires the creation of a robust and time-saving technique based on fragment sizing. We selected 10 polymorphic STR loci of potato: STI0032, STG0016, STI0001, STI0004, STM1104, STM5127, STI0030, STI0033, STI0014, STM5114 and designed a multiplex panel for potato DNA profiling. Fluorescent labelling of primers and size distinction of amplicones allowed us to use one tube for PCR and capillary electrophoresis. We also modified the CTAB-protocol for DNA extraction from tubers and other parts of potato plants, the PCR mix recipe and the amplification protocol for good results. Using Genetic Analyzer allows the length of alleles to be defined with an accuracy of one nucleotide and digitized genetic profiles to be developed. We created a unique DNA profile for each of 40 varieties and 23 breeding lines from Russia and other countries and evaluated the homogeneity of 8 varieties. The proposed technique оf potato DNA profiling allows a large number of samples to be rapidly analyzed in the 96-well plate format

    Separation of amino acids and β-blockers enantiomers by capillary electrophoresis with 1-butyl-3-methylimidazolium L-prolinate [C4MIm][L-Pro] as a chiral selector

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    The current study is devoted to the synthesis of amino acid ionic 1-butyl-3-methylimidazolium L-prolinate [C4MIm][L-Pro] liquid and the investigation of its possibilities as a chiral selector for the separation of amino acids (tryptophan and tyrosine) and β-blockers (carvedilol and propranolol) enantiomers. The following factors affecting the resolution of amino acids stereoisomers under ligand exchange capillary electrophoresis were established: background electrolyte pH, concentration of chelate complex, molar ratio of metal and ligand and its nature. The enantioselectivity values of 1.25 for tryptophan enantiomers and 1.17 for tyrosine enantiomers were observed when the background electrolyte consisted of 50 mM borate buffer (pH = 12.2), 20 mM [C4MIm][L-Pro], and 10 mM CuSO4. The synergetic effect of the synthesized ionic liquid and (2-hydroxypropyl)-?-cyclodextrine when added to the background electrolyte content (20 мМ NaH2PO4, pH = 2.5) was discovered during the separation of carvedilol and propranolol enantiomers. The achieved resolution for carvedilol ( Rs = 1.1) and propranolol ( Rs = 1.6) enantiomers allowed determining the enantiomers ratio of active ingredients in drug formulations.Работа посвящена синтезу аминокислотной ионной жидкости (ИЖ) 1-бутил-3-метилимидазолий L-пролинат [C4MIm][L-Pro] и изучению ее возможностей в качестве хирального селектора при разделении энантиомеров аминокислот (триптофан и тирозин) и β-блокаторов (пропранолол и карведилол). Исследованы факторы, влияющие на разрешение стереоизомеров аминокислот в режиме лигандообменного капиллярного электрофореза (ЛОКЭ). Показано, что на разрешение энантиомеров влияют рН фонового электролита, концентрация хелатного комплекса, мольное соотношение «металл : лиганд», природа хирального селектора и металла-комплексообразователя. Значения энантиоселективности разделения, составившие 1.25 для энантиомеров триптофана и 1.17 для энантиомеров тирозина, были достигнуты с использованием фонового электролита, содержащего 50 мМ боратный буфер (рН = 12.2), 20 мМ [C4MIm][L-Pro], 10 мМ CuSO4. При разделении энантиомеров карведилола и пропранолола обнаружен синергетический эффект при совместном введении в фоновый электролит (20 мМ NaH2PO4, pH = 2.5) двух хиральных селекторов - синтезированной аминокислотной ИЖ [C4MIm][L-Pro] и (2-гидроксипропил)-?-циклодекстрина. Достигнутые значения факторов разрешения для энантиомеров пропранолола ( Rs = 1.1) и карведилола ( Rs = 1.6) позволили определить соотношения энантиомеров действующих веществ в лекарственных препаратах.Работа выполнена при финансовой поддержке гранта РФФИ № 16-03-00791-a.The current study was supported by RFFI grant № 16-03-00791-a

    Синтез, свойства и биологическое действие (±)-транс- 2-диалкиламиноциклогексанолов и их сложных эфиров

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    A series of trans-2-(substituted amino)-cyclohehyl esters have been synthesized and examined for pharmacological activity. Significant responses have been noted with these compounds as ant arrhythmic substances.Синтезирована серия транс-2-диалкиламиноциклогексанолов и их сложных эфиров с целью выяснения их биологической активности. Показано, что полученные соединения обладают антиаритмической активностью и низкой токсичностью
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