Synthesis and properties of hyperbranched polyester polyacrylic acids and their metal complexes

New polydentate ligands based on the hyperbranched third generation polyesters containing terminal acrylic acid fragments were synthesized. The ionization and complexation parameters of new compounds in solution were estimated by spectrophotometry and pH-metric titration followed by experimental data processing using mathematical simulation by the CPESSP program. The procedure for the synthesis was proposed. The polynuclear cobalt(II), nickel(II), and copper(II) complexes with polyester polycarboxylates were synthesized. © 2014 Springer Science+Business Media, Inc

Hyperbranched polyester poly[3-(morpholin-4-yl)propionates] and their copper(II) complexes

© 2017, Pleiades Publishing, Ltd. Novel polydentate ligands on the basis of second- and third-generation hyperbranched polyesters containing terminal poly[3-(morpholin-4-yl)propionate] groups and their 6 : 1 and 13 : 1 polynuclear copper(II) complexes were synthesized. The degree of functionalization of the polyesters with morpholine increases in going from the second (56%) to third generation (68%). According to IR and electronic spectroscopy data, each coordination entity in the complexes is an isolated paramagnetic center of the formula CuN 2 O 2 Solv 2 (Solv = H 2 O, DMSO)

Hyperbranched polyester poly(3-diethylaminepropionate)s and their copper(II) complexes: Synthesis, characterization and biological investigation

© 2016 Elsevier B.V. All rights reserved.New polydentate ligands based on hyperbranched second and third generation polyesters containing terminal (3-diethylamino)propionate fragments and their polynuclear copper(II) complexes were synthesized and characterized by spectroscopic methods. The acid-base properties spectroscopy determined that the functionalization degree of the diethylamine-modified hyperbranched polyesters (LI, LII) increases from the second (56%) to third (81%) generation. The polynuclear complexes Cu(II)-LI and Cu(II)-LII were observed. A coordination site of the complexes contains paramagnetic fragment CuN2O2Solv2 where Solv is H2O or DMSO. The hyperbranched poly(ester amine) of the third generation have strong antifungal activity against Aspergillus fumigatus culture, and its metal complex is active against Candida albicans culture

Лекарственные препараты пыльцевых аллергенов: современные аспекты стандартизации

Scientific relevance. Pollen allergen medicines are in high demand, and their therapeutic benefits directly correlate with their standardisation. Better diagnosis and treatment of allergic diseases require state-of-the-art procedures for assessing the allergenic activity of pollen allergen products using reference standards and physicochemical testing methods.Aim. The study aimed at developing methodological approaches to the standardisation of pollen allergen products in order to shift to measuring their potency in allergenic activity units (AAU) and bring their quality in line with the requirements of the State Pharmacopoeia of the Russian Federation.Materials and methods. The study used pollen allergen reference standards by Microgen, the WHO International Standard for timothy grass (Phleum pratense) pollen extract, a gel filtration standard kit of molecular weight markers ranging from 1.35 to 670 kDa, bovine serum albumin, serum samples with specific IgE obtained from donors sensitised to the study pollen allergens, labelled anti-human IgE antibodies, and reference standards for determining residual volatile solvents by gas chromatography. The identification of in-house reference standards for the potency of pollen allergens involved Western blotting (for allergenic components). The total protein content was determined by Bradford’s assay. In addition, the authors used high-performance liquid chromatography to study protein fractions and gas–liquid chromatography to determine the content of residual organic solvents.Results. To substitute the existing method of non-specific characterisation of allergenic activity in protein nitrogen units (PNU), the authors developed and tested a new method to control allergenic activity in allergenic activity units (AAU) based on an in vitro competitive enzyme-linked immunosorbent assay (ELISA) procedure developed and validated in this study. Furthermore, the authors developed and certified 15 primary in-house reference standards with allergenic activity established in AAU/mL using skin tests in vivo. The experimental data were analysed to  standardise  the  allergenic  activity  of  the  pollen  allergens  manufactured by Microgen. The authors developed physicochemical methods for the certification of in-house reference standards and validated these methods in accordance with the State Pharmacopoeia of the Russian Federation. The study involved selecting chromatographic separation  conditions for residual organic solvents (acetone and diethyl ether) and establishing system suitability criteria for the chromatographic system. The allergenic activity of secondary in-house reference standards was certified against that of primary in-house reference standards using competitive ELISA. Thus, the authors managed to shift to the standardisation of pollen allergen products in vitro.Conclusions. The authors developed their competitive ELISA-based method to standardise pollen allergen products by comparing the inhibition of immune responses to a product and       a standard. The study demonstrated the feasibility of substituting allergenic activity quantification (in AAU) for protein nitrogen content determination (in PNU) and showed the first example of using AAU for the certification of in-house reference standards. Additionally, the authors developed and validated an analytical procedure for determining the content of residual organic solvents in pollen allergen products by gas–liquid chromatography.Актуальность. Лекарственные препараты пыльцевых аллергенов являются наиболее востребованными. Терапевтическая польза от их применения зависит от стандартизации. Для повышения эффективности диагностики и лечения аллергических заболеваний необходимы современные методы оценки специфической (аллергенной) активности лекарственных препаратов пыльцевых аллергенов с применением стандартных образцов и методов физико-химического анализа.Цель. Разработка методологических подходов к стандартизации лекарственных препаратов пыльцевых аллергенов для перехода к нормированию специфической активности в единицах аллергенной активности (ЕАА) и приведения качества препаратов в соответствие с требованиями Государственной фармакопеи Российской Федерации.Материалы и методы. Использовали стандартные  образцы  пыльцевых  аллергенов  (АО «НПО «Микроген»), стандарт ВОЗ аллергена из пыльцы тимофеевки посевной, набор стандартов для эксклюзионной хроматографии MW 1350–670000 Da, бычий сывороточный альбумин, специфические IgE-содержащие сыворотки крови от лиц, сенсибилизированных к исследуемому аллергену, меченые антитела к IgE человека, стандартные образцы летучих растворителей для газовой хроматографии. Подтверждение подлинности стандартного образца предприятия аллергенной активности аллергена (СОП ААА) проводили методом вестерн-блота (аллергенные компоненты), содержание общего белка определяли колориметрически (метод Бредфорда). Дополнительно для изучения белковых фракций применяли метод высокоэффективной жидкостной хроматографии. Количество остаточных органических растворителей в препаратах аллергенов оценивали при помощи газожидкостной хроматографии.Результаты. Вместо существующей ранее неспецифической характеристики аллергенной активности в единицах белкового азота (Protein Nitrogen Unit, PNU) был разработан  и апробирован новый метод контроля специфической активности в ЕАА на основе конкурентного иммуноферментного анализа (кИФА). Разработана и валидирована методика контроля аллергенной активности in vitro на основе кИФА. Проведены разработка и аттестация 15 первичных СОП ААА с присвоением им аллергенной активности в  EAA/мл по результатам тестирования методом кожных проб in vivo. Выполнен анализ экспериментальных данных с целью установления норм аллергенной активности для номенклатуры пыльцевых аллергенов, выпускаемых АО «НПО «Микроген». Разработаны и валидированы в соответствии с Государственной фармакопеей Российской Федерации физико-химические методы аттестации СОП ААА. Определены условия хроматографического разделения остаточных органических растворителей (ацетона, диэтилового эфира) и параметры пригодности хроматографической системы. Проведена аттестация вторичных СОП ААА методом кИФА по показателю аллергенной активности относительно первичных СОП, что позволило перейти к стандартизации препаратов аллергенов методом in vitro.Выводы. Разработана методология  стандартизации препаратов  аллергенов  методом кИФА по степени ингибирования иммунологической реакции в сравнении со стандартным образцом. Обоснована целесообразность исключения  показателя  «Содержание  белкового азота» (в единицах белкового азота, PNU) и замены его на показатель «Аллергенная активность» (в ЕАА). Полученные СОП ААА впервые на предприятии были аттестованы в ЕАА. Разработана и валидирована аналитическая методика определения количественного содержания остаточных органических растворителей в препаратах аллергенов с помощью метода газожидкостной хроматографии

EXCITON - INDUCED PROCESSES IN SOLID MOLECULAR OXYGEN - NEON SOLUTIONS

Author Institution: B. Verkin Institute for Low Temperature Physics and Engineering, Ukrainian Academy of SciencesThe paper is concerned with the processes induced by the trapping of excitons of the neon matrix by impurity centres O and Xe. Binary and triple solutions are studied by a cathodoluminescence spectroscopy method. It is found that the exciton trapping by impurity particles results in an effective dissociation of O molecules, causes an accelerated migration of atoms through the the crystal and a desorption of O, initiates a defect formation in the vicinity of impurity centers and produces a formation of excimer compounds XeO in triple solutions Ne-O -Xe. The mechanisms of these processes associated with the transport of energy of the matrix electronic excitations to an impurity subsystem and its further relaxation are considered. It is shown that all the effects are based on the general principles conditioned by the energy structure and thermophysical characteristics of the Ne matrix- (i) the fast dissipation of exciton excess energy followed by lattice local heating and deformation; (ii) the repulsive behavior of the interaction between Rydberg’s excited impurity center and surrounding atoms of the matrix

Hyperbranched polyester poly[3-(morpholin-4-yl)propionates] and their copper(II) complexes

© 2017, Pleiades Publishing, Ltd. Novel polydentate ligands on the basis of second- and third-generation hyperbranched polyesters containing terminal poly[3-(morpholin-4-yl)propionate] groups and their 6 : 1 and 13 : 1 polynuclear copper(II) complexes were synthesized. The degree of functionalization of the polyesters with morpholine increases in going from the second (56%) to third generation (68%). According to IR and electronic spectroscopy data, each coordination entity in the complexes is an isolated paramagnetic center of the formula CuN 2 O 2 Solv 2 (Solv = H 2 O, DMSO)

Hyperbranched polyester poly[3-(morpholin-4-yl)propionates] and their copper(II) complexes

© 2017, Pleiades Publishing, Ltd. Novel polydentate ligands on the basis of second- and third-generation hyperbranched polyesters containing terminal poly[3-(morpholin-4-yl)propionate] groups and their 6 : 1 and 13 : 1 polynuclear copper(II) complexes were synthesized. The degree of functionalization of the polyesters with morpholine increases in going from the second (56%) to third generation (68%). According to IR and electronic spectroscopy data, each coordination entity in the complexes is an isolated paramagnetic center of the formula CuN 2 O 2 Solv 2 (Solv = H 2 O, DMSO)

Synthesis and properties of hyperbranched polyester polyacrylic acids and their metal complexes

New polydentate ligands based on the hyperbranched third generation polyesters containing terminal acrylic acid fragments were synthesized. The ionization and complexation parameters of new compounds in solution were estimated by spectrophotometry and pH-metric titration followed by experimental data processing using mathematical simulation by the CPESSP program. The procedure for the synthesis was proposed. The polynuclear cobalt(II), nickel(II), and copper(II) complexes with polyester polycarboxylates were synthesized. © 2014 Springer Science+Business Media, Inc