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Facile and Efficient Synthesis of Xanthene Derivatives Mediated by Lanthanum(Iii) Nitrate Hexahydrate under Solvent Free Conditions 无溶剂条件下六水硝酸镧介导的杂蒽衍生物的快速高效合成
IF 0.5 Q3 Chemistry Pub Date : 2020-12-01 DOI: 10.19261/cjm.2020.774
K. Shaikh, Uddhav N. Chaudhar
The present paper shows that lanthanum(III) nitrate hexahydrate can be used as mild and environment friendly homogeneous catalyst for an efficient one-pot multi-component synthesis of biologically active 1,8-dioxo-octahydroxanthene and 14H-dibenzo[a,j]xanthene derivatives. The solvent free condensation reaction of aromatic aldehydes and dimedone or β-naphthol was carried out at 70-80oC during 10-30 min. The obtained compounds were analysed by mass and NMR spectroscopic techniques. The advantages of this eco-friendly synthesis route are numerous, and include the use of an inexpensive catalyst, high to excellent yield, short reaction time and high catalytic activity that can make this method an interesting alternative to multi-step approaches.
研究表明,六水硝酸镧(III)可作为温和、环境友好的均相催化剂,高效地一锅多组分合成具有生物活性的1,8-二氧基八羟基蒽和14h -二苯并[a,j]杂蒽衍生物。芳香族醛与二美酮或β-萘酚在70-80℃下进行无溶剂缩合反应,反应时间为10-30 min。所得化合物通过质谱和核磁共振技术进行了分析。这种环保合成路线的优点很多,包括使用廉价的催化剂,高到优异的产率,短的反应时间和高的催化活性,使这种方法成为多步骤方法的一个有趣的替代方法。
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引用次数: 0
Novel Β-lactams and Thiazolidinone Derivatives from 1,4-dihydroquinoxaline Schiff’s Base: Synthesis, Antimicrobial Activity and Molecular Docking Studies 1,4-二氢喹啉席夫碱的新型Β-lactams和噻唑烷酮衍生物:合成、抗菌活性和分子对接研究
IF 0.5 Q3 Chemistry Pub Date : 2020-06-01 DOI: 10.19261/CJM.2019.647
H. Hrichi, Nadia Ali Ahmed Elkanzi, R. Bakr
A series of novel isolated β-lactams 3a-c and thiazolidinone derivatives 4a-c were successfully synthesized from reactions of new Schiff's bases 2a-c with chloroacetyl chloride and thioglycolic acid. The chemical structures of the new compounds were confirmed through different spectroscopic techniques including IR, 1 H and 13 C NMR, mass spectrometry and elemental analysis. The antimicrobial activity of the obtained compounds was assessed in vitro against gram-positive Staphylococcus aureus and gram-negative Escherichia coli bacteria and Aspergillus flavus and Candida albicans fungi. All compounds exhibited good to excellent antimicrobial activity against the tested strains. Furthermore, a molecular docking study was carried out for the synthesized compounds and the results indicated that compounds 3b and 4b display comparable binding affinity scores as that of glutamate. These two compounds are promising candidates as antibacterial and antifungal agents that would deserve further investigations.
以新型希夫碱2a-c与氯乙酰氯和巯基乙酸为原料,成功地合成了一系列新的β-内酰胺类化合物3a-c和噻唑烷酮衍生物4a-c。通过不同的光谱技术,包括IR、1h和13c NMR、质谱和元素分析,确定了新化合物的化学结构。所得化合物对革兰氏阳性金黄色葡萄球菌、革兰氏阴性大肠杆菌、黄曲霉和白色念珠菌的体外抑菌活性进行了评价。所有化合物均表现出良好至优异的抑菌活性。此外,对合成的化合物进行分子对接研究,结果表明化合物3b和4b的结合亲和力与谷氨酸相当。这两种化合物都是抗菌和抗真菌药物,值得进一步研究。
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引用次数: 9
Simultaneous Quantitative Estimation of Lisinopril and Hydrochlorothiazide Residues Using HPLC for Cleaning Validation 高效液相色谱法同时定量测定赖诺普利和氢氯噻嗪的残留
IF 0.5 Q3 Chemistry Pub Date : 2020-06-01 DOI: 10.19261/cjm.2020.669
I. Rubashvili, Natela Karukhnishvili, Khatuna Makharadze
The aim of this study was to develop and validate direct swab and indirect rinse sampling procedures and a high performance liquid chromatography (HPLC) method for simultaneous quantitative estimation of residues of active pharmaceutical ingredients (API) – lisinopril and hydrochlorothiazide (HCT) in cleaning control samples collected from pharmaceutical manufacturing equipment surfaces after manufacturing of lisinopril/hydrochlorothiazide 20/25 mg uncoated tablets. The swab and rinse sampling procedures were developed and validated in order to obtain a suitable and good recovery (>80%). The acceptance limits of the above-mentioned APIs on the manufacturing equipment surfaces have been established based on pharmacological and toxicological criteria. The new, rapid, specific and selective, developed HPLC method for simultaneous quantitative determination of lisinopril and HCT residues was validated with respect to robustness, system suitability test, specificity, linearity-range, precision, limits of detection and quantitation. The stability of APIs solutions and membrane filter compatibility were studied as well. The method validation was carried out according to ICH Q2 guideline and United States Pharamcopeia requirements. The limit of detection and the limit of quantitation for lisinopril were 0.039 μg/mL and 0.155 μg/mL and for HCT 0.012 μg/mL and 0.025 μg/mL, respectively.
本研究的目的是建立并验证直接拭子取样和间接冲洗取样方法,以及高效液相色谱法(HPLC)同时定量测定赖诺普利/氢氯噻嗪20/ 25mg无包衣片剂生产后从制药设备表面采集的清洁对照样品中活性药物成分(API) -赖诺普利和氢氯噻嗪(HCT)残留量。开发并验证了拭子和冲洗取样程序,以获得合适且良好的回收率(bbb80 %)。上述原料药在生产设备表面的可接受限度已根据药理学和毒理学标准确定。通过鲁棒性、系统适用性、特异性、线性范围、精密度、检出限和定量等方面验证了建立的高效液相色谱法同时定量测定赖诺普利和HCT残留的新方法。研究了原料药溶液的稳定性和膜过滤器的相容性。方法验证按照ICH Q2指南和美国药典要求进行。赖诺普利的检测限和定量限分别为0.039 μg/mL和0.155 μg/mL, HCT的检测限和定量限分别为0.012 μg/mL和0.025 μg/mL。
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引用次数: 0
Organochlorine Pesticides Residues in Soil of Soroca District, Republic of Moldova 摩尔多瓦共和国索罗卡地区土壤中有机氯农药残留
IF 0.5 Q3 Chemistry Pub Date : 2020-06-01 DOI: 10.19261/cjm.2020.672
Elena Culighin
Abstract. The level, composition, and distribution of hexachlorocyclohexane (HCH) and dichlorodiphenyltrichloroethane (DDT) residues were determined by GC-ECD technique in soil samples from the Soroca district, Republic of Moldova. The concentrations of DDTs and HCHs were up to 1100 and 640 mg/kg, respectively. The obtained results indicated that in 77% of analysed soil samples the (DDE+DDD)/DDT ratios showed aged sources of DDT pollution, suggesting that in the studied area, the DDT residues have been transformed significantly into their degradation products. The α-HCH/γ-HCH ratios were generally high (in the range of 1-28) suggesting that technical HCH is the main source of contamination. The high concentration and the degradation rates of pesticides in soil suggest that the contaminated sites are acting as continuous sources of pollution for the environment.
摘要采用气相色谱- ecd技术测定了摩尔多瓦共和国Soroca地区土壤样品中六氯环己烷(HCH)和二氯二苯三氯乙烷(DDT)残留的水平、组成和分布。DDTs和HCHs浓度分别高达1100和640 mg/kg。结果表明,在77%的土壤样品中,(DDE+DDD)/DDT的比值显示了DDT污染源的老化,这表明在研究区域,DDT残留物已明显转化为其降解产物。α-HCH/γ-HCH比值普遍较高(在1 ~ 28之间),说明技术性HCH是主要污染源。土壤中农药的高浓度和降解率表明,污染场地是环境的持续污染源。
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引用次数: 0
Chromatographic Analysis of Orchid Extracts and Quantum Chemical Calculations of Individual Components Interaction with Silica 兰花提取物的色谱分析及各组分与二氧化硅相互作用的量子化学计算
IF 0.5 Q3 Chemistry Pub Date : 2020-06-01 DOI: 10.19261/cjm.2020.694
O. Kazakova, R. Ivannikov, I. Laguta, O. Stavinskaya, V. Anishchenko, Olga Severinovska, L. Buyun
The aim of the work was to identify the main components of orchid extracts and to study their interaction with silica. Composition of sixteen orchid extracts was investigated by means of high performance liquid chromatography and laser desorption/ionization mass spectrometry; as it was shown in this study, flavonoids and phenolic acids were the main bioactive compounds available in the extracts. The interaction between various phenols and silica silanol groups was studied by quantum chemical method. Results show that the strength of interaction of phenols with silica increased in the following order: ferullic, feruloylquinic and fertaric acids< kaempferol, apingenin<< сhlorogenic and caffeic acids, rhamnetin, quercetin, luteolin, epicatechin gallate. The common feature of compounds characterized by the strongest interaction with silanol groups is the presence of a phenol ring with two neighbouring hydroxyl groups. The hydrogen bonds formed between these groups and silanol groups are much shorter (about 0.17 nm) than those formed by other hydroxyl groups of phenols (up to 0.28 nm).
目的是鉴定兰花提取物的主要成分,并研究其与二氧化硅的相互作用。采用高效液相色谱和激光解吸/电离质谱法对16种兰花提取物的成分进行了研究;本研究表明,黄酮类化合物和酚酸是提取物中主要的生物活性化合物。采用量子化学方法研究了不同酚类化合物与硅烷醇基团的相互作用。结果表明,酚类化合物与二氧化硅的相互作用强度依次为阿魏酸、阿魏酰奎宁和铁酸<山奈酚、芹菜素<绿原咖啡酸、鼠李素、槲皮素、木犀草素、表儿茶素没食子酸酯。与硅烷醇基团相互作用最强的化合物的共同特征是存在一个带有两个相邻羟基的酚环。这些基团与硅醇基团之间形成的氢键比其他酚羟基形成的氢键(最长0.28 nm)短得多(约0.17 nm)。
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引用次数: 2
Design and Synthesis of Two Bicyclo[3.3.1]nonane-steroid Derivatives 两个双环[3.3.1]壬烷甾类衍生物的设计与合成
IF 0.5 Q3 Chemistry Pub Date : 2020-06-01 DOI: 10.19261/cjm.2019.657
Lauro Figueroa, Alejandra Garcimarero, R. Garcia, Francisco Díaz, Marcela Rosas, Virginia Mateu, María I. López, Lenin Hau, Tomas Lopez, Abelardo Camacho, Yaritza Borges
Several studies for the synthesis of bicyclo[3.3.1]nonane analogues have been reported, however, there is little information on the preparation of bicyclo[3.3.1]nonane-steroid derivatives. In this way, the aim of this study was to synthesize two steroid-bicyclo[3.3.1]nonane analogues (11 or 12) from either estradiol or estrone using some reactions such as etherification, addition, nucleophilic substitution and cyclization. The chemical structure was evaluated through NMR spectroscopic analysis. The results showed higher yield for 11 compared with 12. It is noteworthy, that the reagents used in this investigation are not expensive and do not require special conditions for handling.
一些合成双环[3.3.1]壬烷类似物的研究已经有报道,但是关于双环[3.3.1]壬烷甾类衍生物的制备的资料很少。因此,本研究的目的是通过醚化、加成、亲核取代和环化等反应,以雌二醇或雌酮为原料合成两种甾体-双环[3.3.1]壬烷类似物(11或12)。通过核磁共振波谱分析对其化学结构进行了评价。结果表明,11号的产量高于12号。值得注意的是,本研究中使用的试剂并不昂贵,也不需要特殊的处理条件。
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引用次数: 0
Evaluation of the Thermal Behaviour of Agricultural Wastes for Possible Use in the Biomass Pellets Industry 对可能用于生物质颗粒工业的农业废弃物热行为的评价
IF 0.5 Q3 Chemistry Pub Date : 2020-06-01 DOI: 10.19261/cjm.2020.717
A. Marcu, G. Lisa, I. Şofran, I. Anghel, M. Serban
This paper tackles the potential uses of agricultural wastes (sawdust, sunflower seed shells, pumpkin seed shells, cherry pits, walnut shells, and green walnut shells) for the production of pellets. Combustion heat was determined for these wastes and their thermal decomposition in an air atmosphere was analysed. Five types of mini-pellets were made from different combinations of available wastes and their thermal behaviour was analysed by the microscale combustion calorimetry method. The results were compared with those obtained for pellets available on the market and it was concluded that the mini-pellets obtained from agricultural wastes can be used to maintain combustion in heating systems based on pellets boilers.
本文探讨了农业废弃物(锯末、葵花籽壳、南瓜籽壳、樱桃核、核桃壳和绿核桃壳)在颗粒生产中的潜在用途。测定了这些废物的燃烧热,并对其在空气中的热分解进行了分析。利用可利用废弃物的不同组合制备了5种不同类型的微球,并采用微尺度燃烧量热法对其热行为进行了分析。将所得结果与市场上可获得的颗粒进行了比较,得出结论:从农业废弃物中获得的微颗粒可以用于基于颗粒锅炉的加热系统中保持燃烧。
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引用次数: 2
Synthesis of Different Structural Types of Zeolites in the Halloysite-dolomite-obsidian System 高岭石-白云石-黑曜石体系中不同结构类型沸石的合成
IF 0.5 Q3 Chemistry Pub Date : 2020-06-01 DOI: 10.19261/cjm.2020.664
G. Mamedova
Gismondine, laumontite and levyne type zeolites have been synthesized based on the natural minerals of Nakhchivan and the optimal crystallization conditions have been established. The influence of temperature, alkaline solution concentration, ratio of starting components and time of processing on the synthesis process has been studied. The mineral resources of Nakhchivan − halloysite deposits of Pirigel, dolomite deposits of Negram and obsidian deposits of Zangezur served as samples. The initial components and the reaction products have been examined by X-ray diffraction, thermogravimetric and elemental analysis. The optimal conditions for the synthesis of gismondine zeolite with a 100% crystallinity are as follows: temperature of 200°C, alkaline solution of 2 N NaOH, ratio of the initial components of halloysite (H):dolomite (D):obsidian (O)= 1:1:1, processing time of 50 hours. The optimal conditions for laumontite synthesis are: temperature of 220°C, alkaline solution of NaOH of 1 N, H:D:O= 1:3:1, processing time of 75 hours. The optimal conditions for levyne are: temperature of 200°C, alkaline solution of KOH of 4 N, H:D:O= 2:1:2, processing time of 100 hours. It was found that changes in the temperature, alkalinity, ratio of starting components and time of processing of the reaction have different effects on the rate of formation of products, on their degree of crystallinity and on the phase purity of the obtained zeolite.
以纳希切万天然矿物为原料,合成了吉斯蒙丁型、湖沸石型和利维安型沸石,并确定了最佳结晶条件。研究了温度、碱液浓度、起始组分配比、加工时间等因素对合成过程的影响。以piigel的Nakhchivan高岭石矿床、Negram的白云岩矿床和Zangezur的黑曜岩矿床为样品。用x射线衍射、热重和元素分析等方法对初始组分和反应产物进行了表征。合成结晶度为100%的gismondine沸石的最佳条件为:温度200℃,碱性溶液为2n NaOH,高岭石(H):白云石(D):黑曜石(O)的初始组分比= 1:1:1,处理时间50小时。合成沸石的最佳条件为:温度220℃,NaOH碱性溶液为1 N, H:D:O= 1:3:1,处理时间75小时。发酵的最佳条件为:温度200℃,KOH碱性溶液为4n, H:D:O= 2:1:2,处理时间100小时。结果表明,反应温度、碱度、起始组分配比和反应时间的变化对产物的形成速度、结晶度和所得沸石的相纯度有不同程度的影响。
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引用次数: 1
Toward a Multidisciplinary Strategy for the Classification and Reuse of Iron and Manganese Mining Wastes 铁矿和锰矿废弃物分类与再利用的多学科策略研究
IF 0.5 Q3 Chemistry Pub Date : 2020-06-01 DOI: 10.19261/cjm.2019.650
D. Guglietta, G. Belardi, G. Cappai, B. Casentini, A. Godeas, S. Milia, D. Passeri, R. Salvatori, A. Scotti, V. Silvani, E. Tempesta, S. Ubaldini, Francesca Trapasso
Mining and mineral-processing wastes have been giving a lot of concern in recent times. This paper has evaluated an integrated multidisciplinary strategy for mining wastes characterization, their possible recycling and reuse, and critical raw materials recovery. After the in situ sampling campaigns, mining wastes have been characterized and the acquired mineralogical, chemical and spectral information have been used to create a map of mining waste deposits by means of the new multispectral satellite Sentinel-2A classification. The use of Fe-Mn rich wastes in arsenic removal and phosphorus recovery from water was discussed. Furthermore, mycorrhizal-assisted phytoextraction of metals from contaminated soils classified as Class 1 to 4 by remote sensing showed a good potential for their possible recovery from biomass, and results indicated that the system was suitable for the uptake of several elements. Results are encouraging and the application of such approach can be important to develop a circular model for sustainable exploitation of mining wastes.
近年来,采矿和矿物加工废物引起了人们的广泛关注。本文评估了采矿废物特性、可能的回收和再利用以及关键原材料回收的综合多学科战略。在实地取样活动之后,对采矿废料进行了特征分析,并利用所获得的矿物学、化学和光谱资料,利用新的多光谱卫星Sentinel-2A分类,绘制了一幅采矿废料分布图。探讨了富铁锰废物在水中除砷、回收磷中的应用。此外,利用遥感技术,菌根辅助植物从1 ~ 4类污染土壤中提取金属,显示出从生物质中回收金属的良好潜力,结果表明该系统适合多种元素的吸收。结果令人鼓舞,这种方法的应用对于发展可持续利用采矿废料的循环模式是重要的。
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引用次数: 3
Analysis of Heavy Metal Accumulation in Fishes from the Coast of Lautoka, Fiji 斐济劳托卡海岸鱼类重金属积累分析
IF 0.5 Q3 Chemistry Pub Date : 2020-06-01 DOI: 10.19261/cjm.2020.701
S. S. Ghani, Aman Deo
The concentrations of the accumulated heavy metals such as cadmium, lead, copper, mercury, zinc, and chromium have been determined in the muscles, gills and liver of the fish species of Clupea pallasii, Macolor niger and Pristipomoides filamentosus collected from the waters of the South Pacific Ocean around Lautoka in Fiji. Results of this study show the order of metal accumulation in tissues of all fishes as follows: Zn ˃Cu ˃ Cr ˃Cd ˃Pb ˃Hg. Overall, the contents of heavy metals in all the samples were below the permissible limits, except for chromium that is slightly higher than the limits of 0.15 mg/kg and 0.05 mg/kg set by Food and Agriculture Organization of the United Nations and World Health Organization regulations respectively. As anticipated, the muscles contain the lowest concentration of all metals. Significant variations in heavy metal concentrations were found between different tissues within each species of fish.
对从斐济劳托卡周围的南太平洋水域收集的黄颡鱼(Clupea pallasii)、黑鲭鱼(Macolor niger)和丝状拟鱼(pritipomoides filamentosus)的肌肉、鳃和肝脏中积累的镉、铅、铜、汞、锌和铬等重金属的浓度进行了测定。本研究结果表明,各鱼类组织中金属的富集顺序为:Zn - Cu - Cr - Cd - Pb - Hg。总体而言,除铬略高于联合国粮食及农业组织规定的0.15 mg/kg和世界卫生组织规定的0.05 mg/kg外,所有样品中的重金属含量均低于允许限量。正如预期的那样,肌肉中金属的浓度最低。在每种鱼类的不同组织之间发现了重金属浓度的显著差异。
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引用次数: 0
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Chemistry Journal of Moldova
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