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Chromatographic parameters as tools for predicting the biological activity of azo derivatives 用色谱参数预测偶氮衍生物的生物活性
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-05-11 DOI: 10.20450/MJCCE.2021.2045
S. Apostolov, G. Vastag
Preliminary assessment of the bioactive profile of azo derivatives was performed applying drug-likeness rules. As the presumed criteria of lipophilicity chromatographic parameters (RM0, m and C0) were calculated in mixtures water/ methanol and water/ acetonitrile by using reversed phase thin-layer chromatography (RPTLC C18/ UV254s). The relationships between chromatographic parameters and relevant software parameters of biological activity of azo derivatives were examined by linear regression and by two multivariate methods. Good linear relationships for each applied system were obtained. The multivariate methods show similarity of the chromatographic parameters (RM0, C0) with standard measure of lipophilicity and pharmacokinetic predictors. The chromatographic parameter m obtained in the same conditions exhibits better agreement with the drug-likeness and toxicity parameters. On the values of azo derivatives’ bioactivity parameters the polarity of the substituent has higher impact than its electronic effects.
应用药物相似规则对偶氮衍生物的生物活性进行了初步评估。采用反相薄层色谱法(RPTLC C18/ UV254s)计算水/甲醇和水/乙腈混合物中亲脂性色谱参数(RM0, m和C0)作为假定标准。采用线性回归和两种多元分析方法考察了偶氮衍生物的色谱参数与相关软件参数之间的关系。得到了各应用系统良好的线性关系。多变量方法显示色谱参数(RM0, C0)与亲脂性标准测量和药代动力学预测指标相似。在相同条件下得到的色谱参数m与药物相似度和毒性参数具有较好的一致性。取代基极性对偶氮衍生物生物活性参数值的影响大于其电子效应。
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引用次数: 0
ICP-OES elemental impurities study on different pharmaceutical dosage forms of Ibuprofen using microwave-assisted digestion procedure 微波消解法研究不同剂型布洛芬的ICP-OES元素杂质
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-05-11 DOI: 10.20450/MJCCE.2021.2100
Katerina Jancevska, G. Petrushevski, Mirjana Bogdanoska, T. Stafilov, S. Ugarkovic
Fast and simple closed-vessel microwave-assisted digestion procedure was developed for decomposition of three pharmaceutical dosage forms of ibuprofen such as tablets, suspension and gel, prior to elemental impurity analysis by one robust and precise ICP-OES method. Samples were digested by four-step microwave program consisting of a 10 min temperature gradient to 180°C, maintained at 180°C for 10 min, followed by 5 min ramping time to 210°C with holding time of 10 min on 210°C. Subsequently, ICP-OES method was developed and validated for simultaneous determination of selected elemental impurities. Results of recovery studies range between 77% and 105% for each element in all analyzed formulations. Correlation coefficients of the regression equations were higher than 0.999 for all analyzed elements. Validation results reveal that the proposed method is specific, accurate, and precise and could be applied for simultaneous quantitative analysis of multi element solutions in different pharmaceutical dosage forms of ibuprofen.
开发了快速简单的封闭容器微波辅助消化程序,用于分解布洛芬的三种药物剂型,如片剂、悬浮液和凝胶,然后通过一种稳健精确的ICP-OES方法进行元素杂质分析。通过四步微波程序消化样品,包括10分钟的温度梯度至180°C,在180°C下保持10分钟,然后在210°C上保持10分钟的升温时间至210°C。随后,开发并验证了ICP-OES方法,用于同时测定选定的元素杂质。所有分析配方中每种元素的回收率研究结果在77%至105%之间。所有分析元素的回归方程的相关系数均高于0.999。验证结果表明,该方法具有特异性、准确性和精密性,可用于布洛芬不同剂型中多元素溶液的同时定量分析。
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引用次数: 2
Variability of the arbutin content in wild growing populations of Arctostaphylos uva-ursi (L.) Spreng from Korab Mountain, Western Balkan 西巴尔干Korab山熊果苷在野生种群中含量的变异性
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-05-11 DOI: 10.20450/MJCCE.2021.2095
G. Stefkov, Ivana Cvetkovikj Karanfilova, Viktorija Labroska, Orhidea Krsteska, Bujar Qazimi, M. Karapandzova, Z. Gjoni, N. Bardhi, S. Kulevanova
Due to the presence of arbutin and hydroquinone in the bearberry plant (Arctostaphylos uva-ursi (L.) Spreng., Ericaceae), it is widely used as a urinary tract antiseptic and diuretic. The herbal substance consists of whole or cut dried leaves, and it should not contain less than 7.00% of anhydrous arbutin (Ph.Eur.10). The supply of this herbal substance in Balkan countries mainly comes from a wild plant harvested in the mountains. It is a common practice to collect the leaves during the flowering season of the plant (June-July). There is an abundance of wild growing natural populations of bearberry on Korab Mountain that represents a unique natural resource of this herbal substance for both countries, Albania and North Macedonia. The aim of the present study was to determine the arbutin content and to assess its variability in the bearberry leaves of seven wild populations from Korab Mountain. The leaves were collected monthly (May-October) during a period of 3 years (2014-2016). The HPLC assay (Ph.Eur.10) revealed that all populations have arbutin content over 7.00% (7.03-9.42%) and that the highest content of arbutin can be attained in September/October, during the phase after the fructification. Statistical analysis showed that there is significant difference between the content of arbutin in the different populations. The content was related to the altitude of the collection site and the collection month and year.
由于熊果属植物中存在熊果苷和对苯二酚(Arctostaphylos uva ursi(L.)Spreng。,Ericaceae),它被广泛用作尿路防腐剂和利尿剂。草药由整片或切下的干叶组成,其无水熊果苷含量不应低于7.00%(欧洲药典第10版)。这种草药在巴尔干国家的供应主要来自山区收获的野生植物。在植物的开花季节(6月至7月)收集叶子是一种常见的做法。Korab山上有大量野生生长的自然熊果种群,这对阿尔巴尼亚和北马其顿两国来说都是这种草药的独特自然资源。本研究的目的是测定Korab山七个野生种群熊果苷的含量并评估其变异性。在3年期间(2014-2016年),每月(5月至10月)收集叶片。HPLC测定(欧洲药典10)显示,所有种群的熊果苷含量都超过7.00%(7.03-9.42%),并且在果实成熟后的9月/10月可以达到熊果苷的最高含量。统计分析表明,不同种群的熊果苷含量存在显著差异。内容与采集地点的海拔高度以及采集月份和年份有关。
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引用次数: 0
Procedure for the assessment of cognitive complexity: Development and implementation in the topic "Hydrolysis of salts" 认知复杂性评估程序:“盐的水解”专题的发展和实施
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-05-11 DOI: 10.20450/MJCCE.2021.2240
Saša A. Horvat, J. Mihajlović, Tamara N. Rončević, Dušica D. Rodić
The aim of this research was the creation and validation of a procedure for determining the cognitive complexity of problem tasks in the field of salt hydrolysis. The procedure created included an assessment of the difficulty of concepts and an assessment of their interactivity. One of the research tasks was to determine whether there were misconceptions by students that might have influenced their achievement. There were 50 Bachelor of Science in Chemistry students who participated in the study. A knowledge test was used as a research instrument to assess the performance and a seven-point Likert scale to evaluate the invested mental effort. The validity of this instrument for the assessment of cognitive complexity was confirmed by a series of regression analyses, where acceptable and statistically significant correlation coefficients were obtained among the examined variables: student performance and invested mental effort as dependent variables and cognitive complexity as independent variable
本研究的目的是创建和验证一种程序,用于确定盐水解领域问题任务的认知复杂性。创建的程序包括对概念难度的评估和对其互动性的评估。研究任务之一是确定学生是否存在可能影响他们成绩的误解。有50名化学理学学士学生参与了这项研究。使用知识测试作为评估绩效的研究工具,并使用七点Likert量表来评估投入的心理努力。该工具用于评估认知复杂性的有效性通过一系列回归分析得到了证实,其中在被测变量之间获得了可接受且具有统计学意义的相关系数:学生表现和投入的脑力劳动作为因变量,认知复杂性作为自变量
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引用次数: 1
Synthesis and characterization of novel 1,2,3-triazole-bridged oxime polyurethanes obtained from an isomannide derivative 异曼尼衍生物制备新型1,2,3-三唑桥肟聚氨酯的合成与表征
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-05-09 DOI: 10.20450/MJCCE.2021.2220
F. Bayrak, A. Oral, K. Ay
Polyurethanes (PUs) are synthesized by the reaction of diisocyanates and diols and are widely used in furniture foams, thermal insulation, coatings, and adhesives. In this work, a 1,2,3-triazole-bridged dioxime (compound 6) as a diol source was synthesized from isomannide via tosylation, azidation, and cyclization-addition and used in the syntheses of new PUs. A new carbohydrate-based linear P-1 was synthesized by the reaction of 6 and 1,6-hexamethylene diisocyanate (1,6-HMDI). Besides, three new linear PUs (P-2, P-3, and P-4) were synthesized by the reaction of 6, isomannide compound (used in different molar ratios), and 1,6-HMDI. The thermal properties of the new PUs were determined by thermogravimetry (TG), their molecular structures were characterized by FTIR, 1H- and 13C-NMR, and the molecular weights of some polymers were determined by GPC/SEC. Additionally, the surface characteristics of the synthesized PUs were examined via scanning electron microscopy (SEM).
聚氨酯(PU)是由二异氰酸酯和二醇反应合成的,广泛用于家具泡沫、隔热、涂料和粘合剂。在本工作中,以异曼尼为原料,通过甲苯磺酰化、叠氮化和环化加成合成了1,2,3-三唑桥二氧肟(化合物6)作为二醇源,并用于合成新的PU。由6和1,6-六亚甲基二异氰酸酯(1,6-HMDI)反应合成了一种新型的基于碳水化合物的线性P-1。此外,通过6,异曼尼化合物(以不同摩尔比使用)和1,6-HMDI的反应,合成了三种新的线性PU(P-2、P-3和P-4)。用热重法(TG)测定了新型PU的热性能,用FTIR、1H-和13C-NMR表征了它们的分子结构,并用GPC/SEC测定了一些聚合物的分子量。此外,通过扫描电子显微镜(SEM)检查了合成的PU的表面特性。
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引用次数: 2
Critical aspects in exploring time analysis for the voltammetric estimation of kinetic parameters of surface electrode mechanisms coupled with chemical reactions 探索与化学反应耦合的表面电极机制动力学参数的伏安估计的时间分析的关键方面
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2021-05-05 DOI: 10.20450/MJCCE.2021.2270
R. Gulaboski, V. Mirčeski, M. Lovrić
The accurate determination of the rate constant related to the electron transfer step of so-called “surface redox active compounds” by voltammetric measurements is very important because it is linked to the reactivity and stability of many biological and chemical systems such as redox enzymes, vitamins, hormones, and many more. Evaluation of the kinetics of the electron transfer is often challenging, especially when chemical equilibria are coupled to the electron transfer step. In this work, we theoretically consider some critical aspects of the time-related methodologies in square-wave voltammetry (SWV), which is designed to analyze the kinetics of the electron transfer step of surface mechanisms coupled with chemical reactions. We demonstrate with a series of simulated scenarios that caution must be taken when exploring the time-related analysis for kinetic characterizations for both surface CE and EC mechanisms. The main concern stems from the fact that the SW frequency simultaneously affects both the kinetics of electron transfer and that of chemical reactions as well. Under defined conditions, the SW frequency variation in the case of surface EC and CE mechanisms may produce unexpected features of the voltammetric patterns. In many scenarios, time-independent analysis, such as those related to the square-wave amplitude and potential increment, are seen as alternative tools to evaluate the rate parameter of electrode reactions.
通过伏安测量准确测定与所谓的“表面氧化还原活性化合物”的电子转移步骤有关的速率常数是非常重要的,因为它与许多生物和化学系统的反应性和稳定性有关,如氧化还原酶、维生素、激素等。电子转移动力学的评估通常是具有挑战性的,特别是当化学平衡与电子转移步骤耦合时。在这项工作中,我们从理论上考虑了方波伏安法(SWV)中与时间相关的方法的一些关键方面,该方法旨在分析表面机制与化学反应耦合的电子转移步骤的动力学。我们通过一系列模拟场景证明,在探索表面CE和EC机制的动力学特征的时间相关分析时必须谨慎。主要的关注源于这样一个事实,即微波频率同时影响电子转移动力学和化学反应动力学。在规定的条件下,在表面EC和CE机制的情况下,SW频率变化可能产生意想不到的伏安模式特征。在许多情况下,与时间无关的分析,如与方波振幅和电位增量相关的分析,被视为评估电极反应速率参数的替代工具。
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引用次数: 3
Infrared and Raman spectra of magnesium ammonium phosphate hexahydrate (struvite) and its isomorphous analogues. X. Vibrational spectra of magnesium rubidium arsenate hexahydrate and magnesium thallium arsenate hexahydrate 六水磷酸铵镁(鸟粪石)及其同形类似物的红外和拉曼光谱。十、六水合砷酸铷镁和六水合砷酸铊镁的振动谱
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2020-12-11 DOI: 10.20450/mjcce.2020.2168
V. Stefov, V. Koleva, M. Najdoski, A. Cahil, Z. Abdija
Polycrystalline samples of struvite-type MgRbAsO 4 ·6H 2 O and MgTlAsO 4 ·6H 2 O in both protiated and deuterated forms have been prepared for the first time by a precipitation method. Detailed analysis of their infrared (IR) and Raman (R) spectra recorded at room temperature (RT) and liquid nitrogen temperature (LNT) has been carried out and assignment of the vibrational bands has been proposed. The observed spectral pictures confirm the isostructurality of the two arsenate salts in agreement with the structural data. Similarly to other struvite-type and structure-related arsenate salts, the n 1 (AsO 4 ) modes appear at higher frequencies than the n 3 (AsO 4 ) vibrations. Low intensity and temperature sensitive bands that could be assigned as due to stretching Mg–O vibrations and n 4 (AsO 4 ) modes are observed below 500 cm –1 in the LNT IR spectra of the studied compounds, at 472 cm –1 and 445 cm –1 for the rubidium analogue and at 470 cm –1 and 440 cm –1 for the thallium analogue. In the far-infrared and Raman spectra many bands are observed between 400 cm –1 and 200 cm –1 , most of which are sensitive to deuteration, suggesting that they are not pure but coupled and can be related to n(Mg–Ow) modes. On the other hand, a band around 405 cm –1 in the spectra of the protiated compounds most probably is due to n 2 (AsO 4 ) mode because of its frequency position, intensity and slight sensitivity to deuteration.
首次用沉淀法制备了鸟粪石型MgRbAsO4·6H2 O和MgTlAsO4·6 H2 O的多晶样品,它们既有质子形式,也有氘化形式。对它们在室温(RT)和液氮温度(LNT)下记录的红外(IR)和拉曼(R)光谱进行了详细分析,并提出了振动带的分配。观察到的光谱图证实了两种砷酸盐的同构性与结构数据一致。与其他鸟粪石类型和结构相关的砷酸盐类似,n1(AsO4)模式出现的频率高于N3(Aso4)振动。在所研究化合物的LNT IR光谱中,在500 cm–1以下,铷类似物在472 cm–1和445 cm–1,铊类似物在470 cm–1到440 cm–1处观察到可归因于拉伸Mg–O振动和n 4(AsO 4)模式的低强度和温度敏感带。在远红外和拉曼光谱中,在400 cm–1和200 cm–1之间观察到许多谱带,其中大多数对氘化敏感,这表明它们不是纯的,而是耦合的,并且可能与n(Mg–Ow)模式有关。另一方面,质子化合物光谱中约405 cm–1的谱带很可能是由于N2(AsO4)模式,因为它的频率位置、强度和对氘化的轻微敏感性。
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引用次数: 2
Probing students' higher order thinking skills using pictorial style questions 用图画式问题探究学生的高阶思维能力
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2020-12-06 DOI: 10.20450/mjcce.2020.2133
Habiddin Habiddin, E. Page
The ability to use Higher Order Thinking Skills (HOTS) plays a substantial role in determining students’ success in future studies. Therefore, it is important that students’ ability in this skill is continually refined by training and assessment. This paper explores the responses of first-year university students’ to a range of pictorial-style questions in chemical kinetics that require the use of HOTS. 80 food science and 57 chemistry students (137 in total) at The University of Reading (UoR) participated in the study. The results showed that many students demonstrated limited ability to answer HOTS questions. The implications for the teaching of chemical kinetics, particularly at the university level, are discussed.
运用高阶思维技能(HOTS)的能力在决定学生未来学习的成功方面发挥着重要作用。因此,通过培训和评估不断提高学生的这项技能是很重要的。本文探讨了大学一年级学生对化学动力学中一系列需要使用HOTS的绘画风格问题的反应。雷丁大学的80名食品科学和57名化学专业学生(共137名)参与了这项研究。结果显示,许多学生在回答HOTS问题时表现出有限的能力。讨论了对化学动力学教学,特别是大学化学动力学教学的启示。
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引用次数: 5
Synthesis and characterization of a new conjugated polymer containing bithiazole group and its thermal decomposition kinetics 一种新型双噻唑基团共轭聚合物的合成、表征及其热分解动力学
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2020-11-28 DOI: 10.20450/mjcce.2020.2025
A. Kurt, H. Andan, M. Koca
A new conjugated polymer containing a bithiazole group is prepared by the polycondensation of 2,2'-diamino-4,4'-bithiazole and terephthaldialdehyde in the presence of glacial acetic acid. The kinetics of thermal degradation of the new polymer are investigated by thermogravimetric analysis at different heating rates. The temperature corresponding to the maximum rate loss shifts to higher temperatures with increasing heating rate. The thermal decomposition activation energies of the conjugated polymer in a conversion range of 3–15 % are 288.4 and 281.1 kJ/mol by the Flynn–Wall–Ozawa and Kissinger methods, respectively. The Horowitz–Metzger method shows that the thermodegradation mechanism of the conjugated polymer proceeds over a three-dimensional diffusion type deceleration D 3 mechanism. The optimum heating rate is 20 oC/min.
以2,2′-二氨基-4,4′-双噻唑和对苯二醛为原料,在冰醋酸存在下缩聚制备了一种新的含双噻唑基团的共轭聚合物。通过热重分析研究了不同升温速率下新型聚合物的热降解动力学。随着升温速率的增加,最大速率损失对应的温度向更高的温度移动。采用Flynn-Wall-Ozawa和Kissinger方法,在转化率为3 ~ 15%范围内,共轭聚合物的热分解活化能分别为288.4和281.1 kJ/mol。Horowitz-Metzger方法表明,共轭聚合物的热降解机制是三维扩散型减速三维机制。最佳升温速率为20℃/min。
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引用次数: 1
Optimization and kinetic study of anthraquinone dye removal from colored wastewater using soybean seed as a source of peroxidase for environmental welfare 以大豆种子为过氧化物酶源去除有色废水中蒽醌染料的工艺优化及动力学研究
IF 1 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2020-11-26 DOI: 10.20450/mjcce.2020.2150
M. Svetozarević, N. Šekuljica, Z. Knežević-Jugović, D. Mijin
As water contamination emerges as a serious threat to the environment, ventures for cleaner and sustainable solutions are continuously being developed. The present study investigates the ability of crude peroxidase extract from soybean seeds to degrade the anthraquinone dye Acid Violet 109. The influence of the essential parameters pH, dye concentration, hydrogen peroxide dosage, and temperature were inspected. The enzyme had 81.9 % biodegradation at pH 4 in 30 min with 0.1 U peroxidase, 40 mg/l dye concentration, and 1 mM hydrogen peroxide. Considering that substrate concentration can cause reaction inhibition, a kinetic study was performed. Kinetic data fitting using bisubstrate kinetics with a substrate inhibition model revealed the high inhibitory effect of the dye, which was confirmed by the inhibition constant, 7.123·10 –5 mM. Alongside the inhibition constant values, the Ping-Pong Bi-Bi model gave the maximum rates 15.788 and 14.321 mM/min for hydrogen peroxide and dye inhibition, respectively.
随着水污染成为对环境的严重威胁,正在不断开发更清洁和可持续的解决方案。研究了大豆种子过氧化物酶粗提物对蒽醌染料酸性紫109的降解能力。考察了基本参数pH、染料浓度、过氧化氢用量和温度对染料性能的影响。用0.1U过氧化物酶、40mg/l染料浓度和1mM过氧化氢,该酶在pH 4下30分钟内具有81.9%的生物降解率。考虑到底物浓度会引起反应抑制,进行了动力学研究。使用双底物动力学和底物抑制模型拟合的动力学数据显示了染料的高抑制作用,抑制常数7.123·10–5 mM证实了这一点。除了抑制常数值外,Ping Pong Bi-Bi模型对过氧化氢和染料的抑制分别给出了15.788和14.321 mM/min的最大速率。
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引用次数: 3
期刊
Macedonian Journal of Chemistry and Chemical Engineering
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