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Development and validation of the method for quantitative determination of preservatives in sodium oxybutyrate syrup 丁酸氧钠糖浆中防腐剂含量测定方法的建立与验证
Q4 Chemistry Pub Date : 2023-03-05 DOI: 10.29235/1561-8331-2023-59-1-26-34
Z. Kuvaeva, S. P. Kacherskaya, O. S. Mastitskaya, E. A. Khvalova
A simple, fast, sensitive method for the determination of preservatives (methyl parahydroxybenzoate, propyl parahydroxybenzoate) in the finished dosage form of sodium oxybutyrate syrup based on the simultaneous determination of preservatives using high performance liquid chromatography (HPLC) is proposed. The HPLC method was validated. The correlation coefficient of the linearity of the technique was 0.999 in the application range of 80–120 % of the normalized value. The calibration graph is linear in the region of 0.495–0.990 mg/ml of methyl 4-hydroxybenzoate and 0.165–0.330 mg/ml of propyl 4-hydroxybenzoate. It has been established that the analytical characteristics of the test procedure (selectivity, linearity, correctness, repeatability, reproducibility) satisfy the selected acceptance criteria.
在高效液相色谱法同时测定防腐剂的基础上,建立了一种简便、快速、灵敏的方法测定氧化丁酸钠糖浆成品剂型中防腐剂(对羟基苯甲酸甲酯、对羟基苯甲酸丙酯)的含量。并对HPLC法进行了验证。在归一化值的80 ~ 120%范围内,该方法的线性相关系数为0.999。在4-羟基苯甲酸甲酯含量0.495 ~ 0.990 mg/ml和4-羟基苯甲酸丙酯含量0.165 ~ 0.330 mg/ml范围内,校准曲线呈线性关系。试验程序的分析特性(选择性、线性、正确性、可重复性、再现性)满足选定的验收标准。
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引用次数: 0
The release of antimony into the atmospheric air on the territory of Belarus: sources, levels and long-term dynamics 向白俄罗斯境内大气中释放的锑:来源、水平和长期动态
Q4 Chemistry Pub Date : 2022-11-29 DOI: 10.29235/1561-8331-2022-58-4-423-432
S. Kakareka, T. Kukharchyk
The results of the first assessment of the antimony release into the atmospheric air on the territory of Belarus are discussed. The main anthropogenic sources of antimony emission have been identified, the emission factors have been developed, and the volumes of antimony emission for the period from 1990 to 2020 have been calculated. It is shown that total antimony emissions varied in the range from 1.6 to 5.6 tons per year with maximum values in the early 1990 s, and minimal – in 2000. Antimony emission in 2020 on the territory of the country is estimated at 2.4 t, the contribution of Belarus to global emission is 0.1 %. Decreasing trend of antimony emission over a 30-year period and a change in the contribution of the main sources to total emission have been established. A significant decrease in the contribution of stationary combustion of fuel (from 66 to 14 %) is due to a change in the fuel balance and is accompanied by increase of the contribution of brake wear (from 34 to 61 %). The data obtained can be used to model the transport and dispersion of antimony, to assess health and ecosystems risks, and to develope measures to reduce the releases of antimony into the environment.
讨论了白俄罗斯境内向大气中释放的锑的第一次评估结果。确定了主要的人类排放源,开发了排放因子,并计算了1990 - 2020年的锑排放量。结果表明,锑的总排放量在每年1.6至5.6吨之间变化,1990年代初达到最大值,2000年达到最小值。据估计,2020年该国境内的锑排放量为2.4吨,白俄罗斯对全球排放量的贡献为0.1%。已经确定了30年期间锑排放的减少趋势和主要排放源对总排放贡献的变化。燃料稳定燃烧的贡献显著减少(从66%到14%)是由于燃料平衡的变化,同时伴随着制动磨损的贡献增加(从34%到61%)。所获得的数据可用于模拟锑的运输和扩散,评估健康和生态系统风险,并制定减少向环境中排放锑的措施。
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引用次数: 0
Quantum-chemical modeling of doxorubicino-fullerenol agents of cancer therapy 阿霉素-富勒烯醇抗癌药物的量子化学模型
Q4 Chemistry Pub Date : 2022-11-29 DOI: 10.29235/1561-8331-2022-58-4-369-378
E. Dikusar, A. Pushkarchuk, T. V. Bezyazychnaya, E. A. Akishina, A. Soldatov, S. Kuten, S. Stepin, A. Nizovtsev, S. Kilin, V. Kulchitsky, V. Potkin
In order to therapeutically destroy neoplasms, chemotherapy or radiotherapy is usually applied, and in isotope medicine short-lived radionuclides are injected into the tumor (59Fe, 90Y, 95Zr, 99mTc, 106Ru, 114*In, 147Eu, 148Eu, 155Eu, 170Tm, 177mLu, 188Re, 210Po, 222Rn, 230U, 237Pu, 240Cm, 241Cm, 253Es). Binary (or neutron capture) therapy is a technology designed to selectively treat malignant tumors and using drugs tropic to tumors containing non-radioactive nuclides (10B, 113Cd, 157Gd at al.). Triadic therapy is the sequential introduction into the body of a combination of two or more separately inactive and harmless components, tropic to tumor tissues and capable of selectively accumulating in them or entering into chemical interaction with each other and destroying tumor neoplasms under certain sensitizing external influences. The aim of this work is to quantum-chemically simulate the electronic structure and to analyze the thermodynamic stability of new doxorubicino-fullerenol agents for the treatment of tumor neoplasms. The need for preliminary studies on the modeling of such objects is due to the extremely high labor intensity, cost and complexity of their practical production.
为了治疗性地破坏肿瘤,通常采用化疗或放疗,在同位素医学中,将短寿命放射性核素(59Fe, 90Y, 95Zr, 99mTc, 106Ru, 114*In, 147Eu, 148Eu, 155Eu, 170Tm, 177mLu, 188Re, 210Po, 222Rn, 230U, 237Pu, 240Cm, 241Cm, 253Es)注射到肿瘤中。二元(或中子俘获)疗法是一种选择性治疗恶性肿瘤的技术,其目的是使用对含有非放射性核素(10B, 113Cd, 157Gd等)的肿瘤有亲和力的药物。三位一体疗法是将两种或两种以上分别无活性和无害成分的组合依次引入体内,这些成分向肿瘤组织返回,能够选择性地在肿瘤组织中积累或相互化学作用,并在某些致敏的外部影响下摧毁肿瘤。本研究的目的是用量子化学方法模拟新型阿霉素-富勒烯醇治疗肿瘤药物的电子结构,并分析其热力学稳定性。由于其实际生产的劳动强度、成本和复杂性极高,因此需要对此类物体的建模进行初步研究。
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引用次数: 1
Aluminium and mica azide surface functionalization 铝和云母叠氮化物表面功能化
Q4 Chemistry Pub Date : 2022-11-29 DOI: 10.29235/1561-8331-2022-58-4-379-386
B. Ranishenka, I. Chelnokova, A. Poznyak
Aluminium and mica (muscovite) plates have been functionalized with azide groups by a protocol which includes (3-chloropropyl) trichlorosilane modification followed by chlorine atom nucleophilic substitution by azide. The azide groups have been transformed to dimethoxytrityl (DMT) ones by [3+2] azide-alkyne cycloaddition reaction. This made it possible to determine their number per surface unit photometrically, based on the absorption of the DMT cation. The functionalization method allowed to achieve high surface load of the materials by azide groups, which was 2.2 and 2.7 nm-2 for mica and aluminium, respectively. The mica plates have been additionally functionalized by 25 kDa branched polyethylenimine. The samples have shown a capability for adsorptive nanoand microobjects immobilization. The feature could be useful for atomic force microscopy, which have been demonstrated with erythrocytes and exosomes.
铝和云母(白云母)板采用叠氮化物基团进行功能化,其中包括(3-氯丙基)三氯硅烷改性,然后由叠氮化物进行氯原子亲核取代。叠氮化物基通过[3+2]叠氮化物-炔环加成反应转化为二甲氧基三硝基(DMT)。这使得根据DMT阳离子的吸收,可以用光度法确定每表面单位的数量。这种功能化方法可以通过叠氮基团实现材料的高表面负载,云母和铝的表面负载分别为2.2和2.7 nm-2。云母板被25 kDa支化聚乙烯亚胺额外功能化。所制备的样品具有吸附固定纳米和微物体的能力。这一特征可能对原子力显微镜有用,这已经在红细胞和外泌体中得到证实。
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引用次数: 0
Development and validation of the method for determination of amitraz in honey using high-performance liquid chromatography with mass spectrometric detection 高效液相色谱-质谱联用测定蜂蜜中阿米特拉兹的方法的建立与验证
Q4 Chemistry Pub Date : 2022-11-29 DOI: 10.29235/1561-8331-2022-58-4-387-397
A. G. Polonevich, S. Leschev, V. A. Bulhakava, L. L. Belyshava
Method for determination of the insecticide amitraz residual content in honey has been developed and validated. The method is selective, express and easy-to-perform. The technique is based on the extraction of amitraz from alkalized aqueous solutions of honey with n-hexane and quantitative determination by high-performance liquid chromatography with mass spectrometric detection. Validation was performed using three types of honey at three levels of amitraz application 6, 120 and 220 µg/kg. The limit of quantification was 0.9 µg/kg, the calibration curves were linear in the concentration range from 2.5 to 125.0 ng/mL (the corresponding analyte content in honey is from 5.0 to 250.0 µg/kg), relative values of the standard deviations of repeatability and within-laboratory reproducibility did not exceed 3.4 and 5.9 %, respectively, the bias values varied from –8.2 to 5.6 %, the expanded uncertainty estimates of the results ranged from 12 to 16 % (P = 0.95). Instrumental limit of quantification, overall efficiency of the process and robustness were also evaluated during the validation process.
建立了测定蜂蜜中杀虫剂阿米特唑残留量的方法,并进行了验证。该方法具有选择性强、快速、简便等特点。本技术以正己烷萃取蜂蜜碱化水溶液中的阿米特拉兹为基础,采用高效液相色谱-质谱法进行定量测定。使用三种蜂蜜在阿米特拉兹的三种水平(6、120和220µg/kg)下进行验证。量化的极限是0.9µg /公斤,校准曲线的线性浓度范围从2.5到125.0 ng / mL(相应的蜂蜜是分析物含量从5.0到250.0µg / kg),重复性和相对标准差的值within-laboratory重现性不超过5.9%和3.4,分别偏差值变化从-8.2到5.6%,结果的扩展不确定度的估计范围从12至16% (P = 0.95)。在验证过程中还评估了定量的仪器极限,过程的总体效率和稳健性。
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引用次数: 1
Optimization of the technology for obtaining guide RNA using plate automatic synthesizer 利用平板自动合成器获得向导RNA的工艺优化
Q4 Chemistry Pub Date : 2022-11-29 DOI: 10.29235/1561-8331-2022-58-4-398-406
E. Ulashchik, T. P. Akhlamionok, P. Y. Baryshchyk, O. Sharko, V. Shmanai
A synthetic protocol was developed and optimal reagents have been selected for obtaining guide RNA oligonucleotides for the CRISPR/Cas system using ASM-2000 automatic synthesizer in 500 nmol scale. Methods for the isolation, purification and analytical control of synthetic RNA oligonucleotides have been developed. The improved technology has been used for preparation of guide RNAs for the CRISPR Cas12a system.
采用ASM-2000型自动合成仪,在500 nmol的条件下制备了CRISPR/Cas系统所需的向导RNA寡核苷酸。研究了合成RNA寡核苷酸的分离、纯化和分析控制方法。改进后的技术已用于制备CRISPR Cas12a系统的引导rna。
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引用次数: 0
Composite technology for the production of paper and cardboard including synthetic fibers 用于生产纸和纸板的复合技术,包括合成纤维
Q4 Chemistry Pub Date : 2022-11-29 DOI: 10.29235/1561-8331-2022-58-4-418-422
U. Eshbaeva, A. Djalilov
In the modern world, the importance and volumes of packaging produced are constantly increasing. It is a powerful means of promoting goods on the market, but at the same time, the role of its quality increases. Currently, paper and paperboard packaging is not only a significant part of paper and paperboard market in general, but also a large part of the world’s packaging consumption. Currently, the world pays special attention to the use of secondary paper waste for the production of paper and cardboard and increase the volume of their processing. The article is devoted to the production of new types of multilayer paper and cardboard with the addition of chemical fiber and secondary waste, as well as high-quality paper and cardboard that can be used in the printing industry, in order to save valuable cotton cellulose in the country. However, the article shows in what proportions it is advisable to use secondary fibers in combination with cellulose in the production of multilayer composite paper and cardboard for the printing and paper industries.
在现代世界,包装生产的重要性和数量不断增加。它是在市场上推销商品的有力手段,但与此同时,其质量的作用也在增加。目前,纸和纸板包装不仅是一般纸和纸板市场的重要组成部分,而且也是世界包装消费的很大一部分。目前,世界各国都特别重视利用二次纸废料生产纸张和纸板,并增加其处理量。本文致力于生产添加化学纤维和二次废弃物的新型多层纸和纸板,以及可用于印刷业的高质量纸和纸板,以节省国内宝贵的棉花纤维素。然而,文章表明,在印刷和造纸工业生产多层复合纸和纸板时,以何种比例使用二次纤维与纤维素结合是可取的。
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引用次数: 0
Influence of rosin resin acids amides on the strength of interfiber bonds in paper in the z-direction 松香树脂、酸、酰胺对纸张纤维间键强度的影响
Q4 Chemistry Pub Date : 2022-11-29 DOI: 10.29235/1561-8331-2022-58-4-407-417
V. Fleisher
Resin acid amides of rosin, depending on the structure, can have both a hydrophobizing and hardening effect on paper pulps. It has been established that the developed products of rosin modification (adhesive rosin composition TMAS3N and polyamide resin ProChem DUO) containing amides of resin acids, when introduced into paper pulps made from fibrous suspensions of sulphate cellulose (unbleached and bleached) of coniferous and broad-leaved species and waste paper, different in the degree of grinding (25, 40 and 70 °ShR), contribute to the increase in the strength of interfiber bonds in paper in the z-direction. The effect of the TMAS-3N emulsion was compared with the traditionally used TM and AKD sizing emulsions. The introduction of the TMAS-3N emulsion into paper pulps (0.40 % of a. d. w.) provides the maximum increase in the strength of interfiber bonds in paper in the z-direction made from cellulose, equal to 16.7–88.6 %, and from waste paper – 19.4–75.4 %, which is 1.6–6.4 and 2.3–4.5 times more compared to TM emulsion, respectively. The achieved positive effect is due to the presence in the TMAS-3H emulsion of particles of the dispersed phase of hydroxyethylamides and aminoethyl ethers capable of forming hydrogen bonds with hydroxyl groups on the mating surfaces of cellulose fibers. Sizing paper stocks with AKD emulsion reduces the strength of interfiber bonds in paper in the z-direction over the entire range of paper content studied. Polyamide resin ProChem DUO, which is a polyaminoamide of rosin resin acids, at its content in paper stocks of 0.10 %, increases the strength of interfiber bonds in paper in the z-direction, made from cellulose and waste paper suspensions, by 50.0–92.3 and 44.4–63.5 %, respectively. The obtained results of increasing the strength of interfiber bonds in paper in the z-direction by resin acid amides of rosin are in full agreement with the mechanism of bridged bonds and the theory of hydrogen bonds.
松香的树脂酸酰胺,根据其结构不同,对纸浆既有疏水作用又有硬化作用。研究发现,将松香改性产物(胶粘剂松香成分TMAS3N和聚酰胺树脂ProChem DUO)引入不同研磨度(25、40和70°ShR)的针叶树和阔叶树硫酸盐纤维素纤维悬浮液和废纸中,可提高纸张纤维间键在z方向上的强度。比较了TMAS-3N乳液与传统的TM和AKD上浆乳液的效果。在纸浆中掺入TMAS-3N乳液(占总用量的0.40%)后,纤维素和废纸的z向纤维间键强度分别提高了16.7 - 88.6%和19.4 - 75.4%,分别是TM乳液的1.6-6.4和2.3-4.5倍。所取得的积极效果是由于在TMAS-3H乳液中存在羟基乙胺和氨基乙醚的分散相颗粒,这些颗粒能够与纤维素纤维配合表面的羟基形成氢键。在研究的整个纸张含量范围内,用AKD乳剂施胶纸张会降低纸张中纤维间键在z方向上的强度。聚酰胺树脂ProChem DUO是一种松香树脂酸的聚酰胺,在原纸中含量为0.10%时,纤维素和废纸悬浮液在z方向上的纤维间键强度分别提高50.0% - 92.3%和44.4% - 63.5%。松香树脂酸酰胺提高纸张纤维间键z方向强度的结果与桥键机理和氢键理论完全一致。
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引用次数: 1
Preparation, structure and photocatalytic activity of nanocomposites based on cerium oxide 氧化铈纳米复合材料的制备、结构及光催化性能
Q4 Chemistry Pub Date : 2022-11-28 DOI: 10.29235/1561-8331-2022-58-4-351-359
I. Matsukevich, E. D. Yundel, N. Kulinich, Y. Yahorava, L. Kulbitskaya, T. F. Kuznetsova
Mesoporous CeO2 and MgO powders and nanocomposites based on them were synthesized by the method of self-propagating high-temperature synthesis, and the mutual influence of magnesium oxide and cerium oxide on the crystal structure, microstructure, and morphology of the obtained materials was studied. It has been established that CeO2 is formed on the surface of magnesium oxide, while the developed surface of the material is preserved. It has been established, that the sizes of CeO2 crystallites in the composition of nanocomposites change insignificantly and range from 6.5 to 7.4 nm, while the values of the specific surface area and average pore diameter of the studied samples depend on the composition and vary in the ranges of 19–41 m2/g and 11.9‒19 nm, respectively. The highest efficiency of photodegradation of dyes of acid telon blue and direct bright blue is observed for samples of MgO–CeO2 (30 mol.%) and MgO–CeO2 (50 mol.%) ‒ 98.5 and 92.5 %, respectively, taking into account the effect of direct photolytic decomposition under the influence of ultraviolet radiation.
采用自蔓延高温合成的方法合成了介孔CeO2和MgO粉末及其纳米复合材料,并研究了氧化镁和氧化铈对材料晶体结构、微观结构和形貌的相互影响。结果表明,CeO2在氧化镁表面形成,而材料的显影表面被保留。结果表明,纳米复合材料中CeO2晶体的尺寸变化不大,范围在6.5 ~ 7.4 nm之间,而样品的比表面积和平均孔径随复合材料的组成而变化,分别在19 ~ 41 m2/g和11.9 ~ 19 nm之间。考虑到在紫外辐射作用下的直接光解作用,MgO-CeO2 (30 mol.%)和MgO-CeO2 (50 mol.%)样品对酸性塔隆蓝和直接亮蓝染料的光降解效率最高,分别为98.5%和92.5%。
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引用次数: 0
Effect of crystallization conditions on modafinil substance polymorphism 结晶条件对莫达非尼物质多态性的影响
Q4 Chemistry Pub Date : 2022-11-28 DOI: 10.29235/1561-8331-2022-58-4-360-368
E. G. Karankevich, Z. Kuvaeva, L. Kulbitskaya, A. Popov
The effect of the crystallization conditions of modafinil from its methanol solutions on the polymorphic state of the resulting substance was studied using the X-ray powder diffraction method. It is shown that changes in the cooling rate and the concentration of saturated solutions have an effect on obtaining samples of the modafinil substance with differences in diffractometric characteristics. Moreover, the cooling rate practically does not affect the yield of the crystalline product, which depends on the degree of saturation of crystallization solutions. It was found that the I polymorphic form of modafinil can be obtained from modafinil solutions with a concentration in the range of 0.34–0.44 M with slow cooling of solutions, mainly with a temperature gradient of 5–10 °C/hour to a temperature of 5 ± 2 °C. An increase in the cooling rate of saturated solutions and their concentration >0.44 M leads to the production of mixed polymorphic forms of modafinil crystals.
用x射线粉末衍射法研究了甲醇溶液中莫达非尼结晶条件对产物多晶态的影响。实验结果表明,冷却速率和饱和溶液浓度的变化对得到的莫达非尼样品的衍射特性有影响。此外,冷却速度实际上并不影响结晶产品的产率,这取决于结晶溶液的饱和程度。研究发现,在浓度为0.34 ~ 0.44 M的莫达非尼溶液中,缓慢冷却可获得I型莫达非尼的多晶形态,主要是温度梯度为5 ~ 10℃/h至5±2℃。饱和溶液冷却速率的增加和饱和溶液浓度>0.44 M导致莫达非尼晶体的混合多晶形式的产生。
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引用次数: 0
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Proceedings of the National Academy of Sciences of Belarus, Chemical Series
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