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Olive mill wastewater treatment using vertical flow constructed wetlands (VFCWs) 利用垂直流人工湿地(VFCWs)处理橄榄种植园废水
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-21 DOI: 10.1186/s13065-024-01348-3
Muna Abu-Dalo, Duaa Abu-Dalo, Maha Halalsheh, Abeer Al Bawab

The study explores a synergistic two-phase system to treat olive mill wastewater (OMW), comprising a multilayer adsorbent filter (pretreatment) and a vertical flow constructed wetland (VFCW). The pretreatment phase includes layers of commercial granular activated carbon (CGAC) and volcanic tuff (VT), while the VFCW phase consists of planted tank with Phragmites australis reeds and unplanted tanks. Initially, municipal wastewater is introduced into the VFCW to establish the required microbial community. Then, pre-treated OMW is passed through the VFCW. The removal rates of various pollutants were assessed. The planted VFCW showed superior removal efficiencies, averaging 97.82% for total chemical oxygen demand (CODT), 92.78% for dissolved oxygen demand (CODd), 99.61% for total phenolic compounds (TPC), 98.94% for total nitrogen (TN), 96.96% for ammonium, and 95.83% for nitrate. In contrast, the unplanted VFCW displayed lower removal efficiencies, averaging 91.47% for CODT, 77.82% for CODd, 98.53% for TPC, 97.51% for TN, 92.04% for ammonium, and 90.82% for nitrate. These findings highlight the significant potential of VFCWs, which offer an integrated approach to OMW treatment by incorporating physical, chemical, and biological mechanisms within a single treatment system.

Graphical Abstract

该研究探索了一种处理橄榄油厂废水(OMW)的两相协同系统,包括一个多层吸附过滤器(预处理)和一个垂直流人工湿地(VFCW)。预处理阶段包括多层商用颗粒活性炭 (CGAC) 和火山凝灰岩 (VT),而垂直流湿地阶段则由种植有芦苇的水槽和未种植芦苇的水槽组成。最初,城市污水被引入 VFCW,以建立所需的微生物群落。然后,预处理过的 OMW 通过 VFCW。对各种污染物的去除率进行了评估。种植的 VFCW 显示出卓越的去除率,平均化学需氧量(CODT)去除率为 97.82%,溶解氧需求量(CODd)去除率为 92.78%,总酚类化合物(TPC)去除率为 99.61%,总氮(TN)去除率为 98.94%,铵去除率为 96.96%,硝酸盐去除率为 95.83%。相比之下,未种植的 VFCW 的去除率较低,平均 CODT 去除率为 91.47%,CODd 去除率为 77.82%,TPC 去除率为 98.53%,TN 去除率为 97.51%,铵去除率为 92.04%,硝酸盐去除率为 90.82%。这些研究结果突显了 VFCWs 的巨大潜力,它通过在单一处理系统中整合物理、化学和生物机制,为 OMW 处理提供了一种综合方法。
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引用次数: 0
Simultaneously quantifying a novel five-component anti- migraine formulation containing ergotamine, propyphenazone, caffeine, camylofin, and mecloxamine using UV spectrophotometry and chemometric models 利用紫外分光光度法和化学计量学模型同时量化含有麦角胺、异丙嗪、咖啡因、骆驼蓬素和麦考酚胺的新型五组分抗偏头痛制剂
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-20 DOI: 10.1186/s13065-024-01339-4
Ahmed Emad F. Abbas, Nahla A. Abdelshafi, Mohammed Gamal, Michael K. Halim, Basmat Amal M. Said, Ibrahim A. Naguib, Mohmeed M. A. Mansour, Samir Morshedy, Yomna A. Salem

This study presents a new method for simultaneously quantifying a complex anti-migraine formulation containing five components (ergotamine, propyphenazone, caffeine, camylofin, and mecloxamine) using UV spectrophotometry and chemometric models. The formulation presents analytical challenges due to the wide variation in component concentrations (ERG: PRO: CAF: CAM: MEC ratio of 0.075:20:8:5:4) and highly overlapping UV spectra. To create a comprehensive validation dataset, the Kennard-Stone Clustering Algorithm was used to address the limitations of arbitrary data partitioning in chemometric methods. Three different chemometric models were evaluated: Classical Least Squares (CLS), Partial Least Squares (PLS), and Multivariate Curve Resolution-Alternating Least Squares (MCR-ALS). Among these, MCR-ALS demonstrated excellent performance, achieving recovery values of 98–102% for all components, accompanied by minimal root mean square errors of calibration (0.072–0.378) and prediction (0.077–0.404). Moreover, the model exhibited high accuracy, with relative errors ranging from 1.936 to 3.121%, bias-corrected mean square errors between 0.074 and 0.389, and a good sensitivity (0.2097–1.2898 μg mL−1) for all components. The Elliptical Joint Confidence Region analysis further confirmed the predictive performance of the models, with MCR-ALS consistently showing the smallest ellipses closest to the ideal point (slope = 1, intercept = 0) for most analytes, indicating superior accuracy and precision. The approach's sustainability was rigorously assessed using six advanced metrics, validating its environmental friendliness, economic viability, and practical application. This approach effectively resolves complex pharmaceutical formulations, contributing to sustainable development objectives in quality control processes.

本研究提出了一种新方法,利用紫外分光光度法和化学计量学模型,同时对含有五种成分(麦角胺、丙菲那宗、咖啡因、骆驼蓬素和麦考酚胺)的复杂抗偏头痛制剂进行定量。该制剂的成分浓度变化很大(ERG: PRO: CAF: CAM: MEC 的比例为 0.075:20:8:5:4),且紫外光谱高度重叠,这给分析带来了挑战。为了创建一个全面的验证数据集,我们使用了 Kennard-Stone 聚类算法来解决化学计量学方法中任意数据分区的局限性。对三种不同的化学计量模型进行了评估:经典最小二乘法(CLS)、部分最小二乘法(PLS)和多变量曲线解析-替代最小二乘法(MCR-ALS)。其中,MCR-ALS 表现出色,所有成分的回收率都达到 98-102%,校准均方根误差(0.072-0.378)和预测均方根误差(0.077-0.404)都很小。此外,该模型的准确度也很高,相对误差在 1.936% 到 3.121% 之间,偏差校正均方误差在 0.074 到 0.389 之间,对所有成分的灵敏度(0.2097-1.2898 μg mL-1)都很高。椭圆联合置信区分析进一步证实了模型的预测性能,对于大多数分析物,MCR-ALS 始终显示出最接近理想点(斜率 = 1,截距 = 0)的最小椭圆,表明其准确度和精确度都很高。该方法的可持续性通过六项先进指标进行了严格评估,验证了其环境友好性、经济可行性和实际应用性。该方法可有效解决复杂的药物制剂问题,有助于实现质量控制过程中的可持续发展目标。
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引用次数: 0
New chemometrics-assisted spectrophotometric methods for simultaneous determination of co-formulated drugs montelukast, rupatadine, and desloratadine in their different dosage combinations 化学计量学辅助分光光度计新方法,用于同时测定不同剂量组合中的复方药物孟鲁司特、鲁帕他定和地氯雷他定
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-19 DOI: 10.1186/s13065-024-01345-6
Marco M. Z. Sharkawi, Nehal F. Farid, Moataz H. Hassan, Said A. Hassan

Two accurate, precise and robust multivariate chemometric methods were developed for the simultaneous determination of montelukast sodium (MON), rupatadine fumarate (RUP) and desloratadine (DES). These methods provide a cost-effective alternative to chromatographic techniques by utilizing spectrophotometry in pharmaceutical quality control. The proposed approaches, partial least squares-1 (PLS-1) and artificial neural network (ANN), were optimized using genetic algorithm (GA) to select the most influential wavelengths, enhancing model performance. A five-level, three-factor design was employed to construct a calibration set with 25 mixtures, utilizing concentration ranges of 3–19, 5–25, and 4–20 µg.mL−1 for MON, RUP, and DES, respectively. An independent validation set was employed to assess the performance of the models. GA significantly improved the PLS-1 and ANN models for RUP and DES, though minimal enhancement was observed for MON. These methods were successfully applied to the simultaneous quantification of the compounds in pharmaceutical formulations and proved useful as stability-indicating assays for RUP, given that DES is a known degradation product. The developed methods offer a valuable tool for impurity profiling and quality control in pharmaceutical analysis.

为同时测定孟鲁司特钠(MON)、富马酸鲁帕他定(RUP)和地氯雷他定(DES),开发了两种准确、精确和稳健的多元化学计量学方法。这些方法通过在药品质量控制中使用分光光度法,为色谱技术提供了一种具有成本效益的替代方法。利用遗传算法(GA)对所提出的偏最小二乘法-1(PLS-1)和人工神经网络(ANN)方法进行了优化,以选择最有影响力的波长,提高模型性能。采用五级三因子设计构建了一个包含 25 种混合物的校准集,MON、RUP 和 DES 的浓度范围分别为 3-19、5-25 和 4-20 µg.mL-1。采用独立的验证集来评估模型的性能。GA 明显改进了 RUP 和 DES 的 PLS-1 和 ANN 模型,但对 MON 的改进很小。这些方法成功地应用于药物制剂中化合物的同时定量,并证明可作为 RUP 的稳定性指示测定,因为 DES 是已知的降解产物。所开发的方法为药物分析中的杂质分析和质量控制提供了宝贵的工具。
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引用次数: 0
AQbD-enhanced green RP-UPLC-PDA methodology for quantification and forced degradation studies for omeprazole, amoxicillin, and rifabutin 用于奥美拉唑、阿莫西林和利福布汀定量和强制降解研究的 AQbD 增强绿色 RP-UPLC-PDA 方法。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-18 DOI: 10.1186/s13065-024-01337-6
S. P. Ashnah Baffinsha, Vijayageetha Ragupathi, Hemanth Kumar Chanduluru

The ternary combination like omeprazole (OMP), amoxicillin (AMX), and rifabutin (RFB) was approved by the FDA in November 2019 for combating Helicobacter pylori infections and ulcers caused by this infection. This study aims to develop and authenticate a robust and eco-friendly RP-UPLC technique aimed at the concurrent analysis of OMP, AMX, and RFB, following ICH guidelines, Analytical Quality by Design (AQbD), and green analytical chemistry (GAC) principles. The analysis used the Thermo C18 column (100 mm × 2.1 mm, 1.7 µm), ethanol, and formic acid solution (43:57) as mobile phase with a flow rate of 0.2 ml/min at 272 nm. The method was developed based on the ICH Q14 and validated according to ICH Q2(R1) followed by Forced degradation studies under various conditions. The method showed good linearity for OMP, AMX, and RFB, with coefficient of determination (r2) of 0.9995, 0.9993, and 0.9997, respectively. Precision studies indicated low %RSD values, confirming high reproducibility. Forced degradation studies confirmed the stability of the drugs for 30 min in acid, base, and redox reactions, and they were also stable for 6 h at 105 °C in dry conditions. GAPI assessment depicted a green and yellow pictogram, AGREE scored 0.85, BAGI scored 80, and RGB12 Whiteness Assessment Tool scored 97.5%. The developed RP-UPLC-PDA technique is robust and reliable for the concurrent quantification of the triple combination. It aligns with sustainability goals, enhancing the efficiency and environmental sustainability of pharmaceutical analysis, and setting a benchmark for future analytical methods.

奥美拉唑(OMP)、阿莫西林(AMX)和利福布汀(RFB)等三元复方制剂于 2019 年 11 月获得美国食品药品管理局(FDA)批准,用于防治幽门螺杆菌感染和由此引起的溃疡。本研究旨在遵循 ICH 指南、分析质量设计(AQbD)和绿色分析化学(GAC)原则,开发和验证一种稳健且环保的 RP-UPLC 技术,用于同时分析 OMP、AMX 和 RFB。分析采用 Thermo C18 色谱柱(100 mm × 2.1 mm, 1.7 µm),以乙醇和甲酸溶液(43:57)为流动相,流速为 0.2 ml/min,检测波长为 272 nm。该方法根据 ICH Q14 标准建立,并根据 ICH Q2(R1) 标准进行了验证,随后在不同条件下进行了强制降解研究。该方法对 OMP、AMX 和 RFB 的线性关系良好,测定系数(r2)分别为 0.9995、0.9993 和 0.9997。精密度研究表明,%RSD 值较低,证实了其较高的重现性。强制降解研究证实,药物在酸、碱和氧化还原反应中 30 分钟内保持稳定,在 105 °C 干燥条件下 6 小时内也保持稳定。GAPI 评估显示了绿色和黄色象形图,AGREE 得分为 0.85,BAGI 得分为 80,RGB12 白度评估工具得分为 97.5%。所开发的 RP-UPLC-PDA 技术对于三重组合的同时定量具有稳健性和可靠性。它符合可持续发展目标,提高了药物分析的效率和环境可持续性,为未来的分析方法树立了标杆。
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引用次数: 0
Chromatographic assay of recently approved co-formulation of Vonoprazan fumarate with low dose Aspirin: AGREE, Complex MoGAPI, and RGB 12-model assessments 最近批准的富马酸伏诺普拉赞与低剂量阿司匹林联合制剂的色谱分析:AGREE、Complex MoGAPI 和 RGB 12 模型评估。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-16 DOI: 10.1186/s13065-024-01344-7
Mona M. Abdel Moneim, Mohamed M. A. Hamdy

Two simple, valid and green chromatographic based techniques are developed in the present work for first time to simultaneously analyze the recently approved combination of Aspirin (ASP) with the novel gastro-protective agent Vonoprazan (VON). First method is an HPLC-DAD “diode array detection”, where separation was successful using C18 (250 × 4.6 mm) column with isocratic elution of phosphate buffer-pH 6.8 and acetonitrile in ratio of 63:37 with detection at 230 nm. Second method is an HPTLC method on HPTLC silica plates using ethyl acetate: ethanol (75%): ammonia (5:5:0.05 v/v) mobile phase followed by densitometric scanning at 230 nm. The methods were applied successfully for analysis of VON and ASP mixture in laboratory-prepared tablets and the methods were validated in regards to linearity, precision, accuracy and selectivity. The proposed methods are assessed for their greenness and whiteness as well using the “Analytical GREEnness Metric Approach”, “Complementary Modified Green Analytical Procedure Index” and the new algorithm “RGB 12 model” (Red-Green-Blue) and proved the greenness and the sustainability of the methods in the routine assay of the newly marketed formulation.

本研究首次开发了两种简单、有效和绿色的色谱技术,用于同时分析最近获批的阿司匹林(ASP)与新型胃保护剂沃诺普拉赞(VON)的复方制剂。第一种方法是 HPLC-DAD "二极管阵列检测法",使用 C18(250 × 4.6 毫米)色谱柱,以磷酸盐缓冲液-pH 6.8 和乙腈按 63:37 的比例进行等度洗脱,在 230 纳米波长下检测,成功实现了分离。第二种方法是 HPTLC 法,在 HPTLC 硅胶板上使用乙酸乙酯:乙醇(75%):氨水(5:5:0.05 v/v)流动相,然后在 230 纳米波长下进行密度扫描。这些方法成功地应用于实验室制备的片剂中VON和ASP混合物的分析,并在线性、精密度、准确度和选择性方面进行了验证。使用 "分析 GREEnness 度量方法"、"补充修正绿色分析程序指数 "和新算法 "RGB 12 模型"(红-绿-蓝)对所建议的方法进行了绿色和白度评估,证明了这些方法在新上市制剂的常规检测中的绿色性和可持续性。
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引用次数: 0
New thiophene derivatives: chemoselective synthesis, antitumor effectiveness, structural characterization, DFT calculations, Hirshfeld surface, and Fukui function analysis 新噻吩衍生物:化学选择性合成、抗肿瘤效果、结构特征、DFT 计算、Hirshfeld 表面和 Fukui 函数分析。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-14 DOI: 10.1186/s13065-024-01346-5
Abdullatif Bin Muhsinah, Mohammed M. Alharbi, Nabila A. Kheder, Saied M. Soliman, Hazem A. Ghabbour, Naglaa S. Mahmoud, Ismail A. Elhaty, Yahia N. Mabkhot

In this study, the chemoselective synthesis of two new thiophene derivatives is presented. The structure of newly synthesized thiophenes derivatives; ethyl 4-acetyl-3-phenyl-5-(phenylamino)thiophene-2-carboxylate (5) and ethyl (E)-4-(3-(dimethylamino)acryloyl)-3-phenyl-5-(phenylamino)thiophene-2-carboxylate (8) were established using different FTIR and NMR spectral analyses. Compound 8 was isolated as single crystal and its 3D structure was determined using X-ray crystallographic analysis. Possible intermolecular interactions that control the molecular packing of 8 were elucidated using Hirshfeld topology analysis. The O…H (13.7%), H…H (55.3%) and C…C (2.3%) intermolecular interactions are the most significant. Fukui functions showed that C4 in thiophene 5 and C3 in thiophene 8 are the most reactive atoms for nucleophilic attack, while N9 in thiophene 5 and C1 in thiophene 8 are the most reactive atoms for electrophilic attack. Antitumor activity of thiophene 5 was assessed and the results showed higher activity against HepG-2 (7.46 µg/mL) compared to the HCT 116 (12.60 µg/mL) cell line.

本研究介绍了两种新噻吩衍生物的化学选择性合成。通过不同的傅立叶变换红外光谱和核磁共振光谱分析,确定了新合成的噻吩衍生物:4-乙酰基-3-苯基-5-(苯基氨基)噻吩-2-甲酸乙酯(5)和(E)-4-(3-(二甲基氨基)丙烯酰基)-3-苯基-5-(苯基氨基)噻吩-2-甲酸乙酯(8)的结构。化合物 8 被分离成单晶体,并通过 X 射线晶体分析确定了其三维结构。利用 Hirshfeld 拓扑分析法阐明了控制 8 分子堆积的可能的分子间相互作用。其中,O...H(13.7%)、H...H(55.3%)和 C...C(2.3%)的分子间相互作用最为显著。福井函数表明,噻吩 5 中的 C4 和噻吩 8 中的 C3 是亲核攻击反应最活跃的原子,而噻吩 5 中的 N9 和噻吩 8 中的 C1 是亲电攻击反应最活跃的原子。对噻吩 5 的抗肿瘤活性进行了评估,结果表明其对 HepG-2 细胞株(7.46 微克/毫升)的活性高于对 HCT 116 细胞株(12.60 微克/毫升)的活性。
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引用次数: 0
Bio-inspired one-pot synthesis of luminescent silver nanoparticles and its significant utility as a fluorescence nano sensor for analysis of two adjunctive COVID-19 drugs 受生物启发的发光银纳米粒子的一锅合成及其作为荧光纳米传感器在分析 COVID-19 两种辅助药物中的重要作用。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-14 DOI: 10.1186/s13065-024-01335-8
Yasmeen E. Mostafa, Fawzi Elsebaei, Mohammed El-Sayed Metwally

This study reveals one-step green synthesis of plant inspired silver nanoparticles (Ag-NPs). The synthesis procedure relies on the bio-reduction of Ag+ to Ag0 using orange waste (orange peel) extract as cheap, readily available, sustainable, biocompatible feedstocks as a reducing and stabilizing agent. The prepared Ag-NPs passed through a full characterization procedure for better confirmation and elucidation of optical and structural properties. The fluorescence of the prepared Ag-NPs has a quantum yield of 17.15% enabling its potential use in chemical sensing of drugs. Ag-NPs are conceived to be used as a fluorescent nano sensor for sensitive, ecofriendly, rapid spectrofluorimetric determination of two recent direct oral anticoagulants, namely, rivaroxaban (RIV) and edoxaban tosylate monohydrate (EDT); COVID-19 adjunctive drugs in their raw materials and pharmaceutical tablets. The fluorescence of the prepared Ag-NPs at 333 nm ({(uplambda }_{text{ex}}=258 text{nm})) was found to be substantially quenched in existence of increasing concentrations of each drug. The quenching mechanisms were studied and explained. The validation of the method revealed linear correlation over the ranges of 0.5–10 µg/ml with an excellent regression correlation (r = 0.9999) for both drugs with minimum detection limits of 0.14 and 0.16 µg/ml for rivaroxaban and edoxaban tosylate monohydrate, correspondingly. Three different metrics were employed for verifying the greenness profile of the presented study. The findings of the greenness assessment were congruent and compatible with the green synthesis procedure, ecofriendly analysis, and the exclusion of using organic solvents and noxious materials opening an avenue for green synthesis of nanoparticles instead of chemical and physical methods.

本研究揭示了一步法绿色合成植物银纳米粒子(Ag-NPs)的方法。合成过程依赖于将 Ag+ 生物还原为 Ag0,使用橘子废料(橘子皮)提取物作为还原剂和稳定剂。制备的 Ag-NPs 经过了全面的表征程序,以更好地确认和阐明其光学和结构特性。制备的 Ag-NPs 的荧光量子产率为 17.15%,可用于药物的化学传感。Ag-NPs 被设想用作一种荧光纳米传感器,用于灵敏、环保、快速地测定两种最新的直接口服抗凝剂,即利伐沙班(RIV)和一水合甲磺酸埃多沙班(EDT);COVID-19 辅助药物的原料和药片。研究发现,在每种药物浓度增加的情况下,制备的 Ag-NPs 在 333 纳米(λ ex = 258 纳米)处的荧光会被大幅淬灭。对淬灭机制进行了研究和解释。该方法的验证结果表明,两种药物在 0.5-10 µg/ml 的范围内线性相关,回归相关性极佳(r = 0.9999),利伐沙班和一水托沙班的最低检测限分别为 0.14 µg/ml 和 0.16 µg/ml。本研究采用了三种不同的指标来验证绿色概况。绿色性评估的结果与绿色合成程序、生态友好分析以及不使用有机溶剂和有毒材料相一致,为纳米粒子的绿色合成开辟了一条替代化学和物理方法的途径。
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引用次数: 0
Utilizing MEDT analysis of [3 + 2] cycloaddition reaction: x-ray crystallography of spirooxindole linked with thiophene/furan heterocycles and triazole framework 利用 MEDT 分析 [3 + 2] 环加成反应:与噻吩/呋喃杂环和三唑框架相连的螺吲哚的 X 射线晶体学。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-14 DOI: 10.1186/s13065-024-01343-8
Abdulmajeed Abdullah Alayyaf, M. Ali, Moayad Abdullah Alwehaibi, Muhanna K. Al-Muhanna, Saied M. Soliman, Mar Ríos-Gutiérrez, Matti Haukka, Assem Barakat

Hybridization of spirooxindole with different pharmacophores such as triazole and heterocycle such as thiophene and furan moiety was achieved by the [3 + 2] cycloaddition (32CA) reaction approach. Structural investigations of the compounds 4a and 4b were performed using X-ray single crystal structure determinations and Hirshfeld analysis. Both compounds crystallized in monoclinic crystal system. The space group is P21/c for 4a and P21/n for 4b. The crystal parameters are a = 10.2619(3) Å, b = 13.6776(3) Å, c = 10.9318(3), β = 116.640(4)° for the former while a = 13.0012(1) Å, b = 14.9692(1) Å, c = 14.1178(1) Å, β = 97.101(1)° for the latter. In both compounds, the aryl group and the triazole moieties are twisted from one another. The twist angle is 84.75˚for 4a while 86.64˚ for 4b. Based on Hirshfeld calculations, the Cl…H, O…H, N…H and C…H non-covalent interactions in 4a while the O…H interactions in 4b are the most important. The molecular mechanism of the key 32CA reaction between the in situ generated azomethine ylides and the corresponding chalcones has been studied within the Molecular Electron Density Theory (MEDT). The MEDT study reveals that the low activation energies and high experimental selectivity are the result of the supernucleophilic character of the ylides and the strong electrophilicity of the chalcones, which favour the process through a high polar character. This high polar character accounts for the total endo selectivity experimentally found.

通过[3 + 2]环加成(32CA)反应方法,实现了螺吲哚与三唑和杂环(如噻吩和呋喃)等不同药源的杂化。利用 X 射线单晶结构测定和 Hirshfeld 分析法对化合物 4a 和 4b 进行了结构研究。这两种化合物均以单斜晶系结晶。4a 的空间群为 P21/c,4b 的空间群为 P21/n。前者的晶体参数为 a = 10.2619(3)埃,b = 13.6776(3)埃,c = 10.9318(3),β = 116.640(4)°;后者的晶体参数为 a = 13.0012(1)埃,b = 14.9692(1)埃,c = 14.1178(1)埃,β = 97.101(1)°。在这两种化合物中,芳基和三唑分子相互扭曲。4a 的扭转角为 84.75˚,而 4b 的扭转角为 86.64˚。根据 Hirshfeld 计算,4a 中的 Cl...H、O...H、N...H 和 C...H 非共价相互作用最为重要,而 4b 中的 O...H 相互作用最为重要。分子电子密度理论(MEDT)研究了原位生成的偶氮甲基酰化物与相应的查耳酮之间的关键 32CA 反应的分子机理。分子电子密度理论研究表明,低活化能和高实验选择性是由酰化物的超亲核性和查耳酮的强亲电性造成的,它们通过高极性特征促进了反应过程。这种高极性是实验发现的总内选择性的原因。
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引用次数: 0
New N-amino-5-cyano-6-pyridones as antimicrobial small molecules endowed with DNA gyrase a inhibitory activity: design, one-pot synthesis, biological assessment and in silico insights 具有 DNA gyrase a 抑制活性的新型 N-氨基-5-氰基-6-吡啶酮类抗菌小分子:设计、一锅合成、生物学评估和硅学研究。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-13 DOI: 10.1186/s13065-024-01342-9
Omkulthom Al Kamaly, Amel S. Younes, Marwa F. Harras, Rehab Sabour, Aisha A. Alsfouk, Mona H. Ibrahim

A set of innovative N-amino-5-cyano-6-pyridones derivatives was developed and produced using one-pot three-component procedures. The evaluated molecules were examined for their antimicrobial efficacy. Based on the acquired findings, most of the investigated compounds had promising antimicrobial properties. Out of these derivatives of 3-cyanopyridine, compounds 3d and 3e exhibited minimum inhibitory concentrations (MIC) of 3.91 µg/mL against E.coli. In vitro evaluation of DNA gyrase A displayed that molecule 3d exhibited promising potency as an inhibitor, with an IC50 value of 1.68 µg/mL compared to ciprofloxacin (IC50 = 0.45 µg/mL). Furthermore, it was observed that molecule 3e exhibited a moderate inhibitory effect, as indicated by its IC50 value of 3.77 µg/mL. A kinetics study conducted to assess the time required to kill E. coli bacteria demonstrated that gentamycin and compounds 3d and 3e exhibited bactericidal effects within a time frame of 90–120 min. Based on the ADME predictions, compounds 3d and 3e are expected to have favorable oral bioavailability and are unlikely to penetrate the blood-brain barrier. Computational mutagenicity and tumorigenicity studies were conducted on compounds 3d and 3e. The molecular docking investigation has conclusively demonstrated the binding of compounds 3d and 3e to the target DNA gyrase A enzyme, further reinforcing the existing data.

采用三组份一锅法开发并生产了一组创新的 N-氨基-5-氰基-6-吡啶酮衍生物。对所评估的分子进行了抗菌功效检测。根据获得的研究结果,大多数研究化合物都具有良好的抗菌性能。在这些 3-氰基吡啶衍生物中,化合物 3d 和 3e 对大肠杆菌的最低抑制浓度 (MIC) 为 3.91 µg/mL。DNA 回旋酶 A 的体外评估显示,分子 3d 具有良好的抑制作用,与环丙沙星(IC50 = 0.45 µg/mL)相比,IC50 值为 1.68 µg/mL。此外,还观察到分子 3e 显示出中等程度的抑制作用,其 IC50 值为 3.77 微克/毫升。为评估杀死大肠杆菌所需的时间而进行的动力学研究表明,庆大霉素、化合物 3d 和 3e 在 90-120 分钟的时间范围内表现出杀菌效果。根据 ADME 预测,化合物 3d 和 3e 预计具有良好的口服生物利用度,不太可能穿透血脑屏障。对化合物 3d 和 3e 进行了诱变性和致瘤性计算研究。分子对接研究确证了化合物 3d 和 3e 与目标 DNA 回旋酶 A 的结合,进一步巩固了现有数据。
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引用次数: 0
Separation properties and fouling resistance of polyethersulfone membrane modified by fungal chitosan 真菌壳聚糖改性聚醚砜膜的分离性能和抗堵塞性
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-11 DOI: 10.1186/s13065-024-01341-w
Hilya N. Iman, Henry Susilo, Adhi Satriyatama, Ignatius D. M. Budi, Kiki A. Kurnia, I. G. Wenten, K. Khoiruddin

This research explores the enhancement of polyethersulfone (PES) membranes through the incorporation of chitosan derived from the lignicolous fungus Ganoderma sp. Utilizing wet phase inversion and solution casting techniques, chitosan was successfully integrated into the PES matrix, as confirmed by Fourier Transform Infrared Spectroscopy (FT-IR), which indicated a high deacetylation degree of 75.7%. The incorporation of chitosan significantly increased the membrane hydrophilicity, as evidenced by a reduction in the water contact angle and a substantial improvement in pure water permeability, from 17.9 L m-2 h-1 bar-1 to 27.3 L m-2 h-1 bar-1. The membrane anti-fouling properties were also notably enhanced, with the Flux Recovery Ratio (FRR) increasing from approximately 60–80%. Moreover, the chitosan-modified PES/CS membrane, particularly at a 5% chitosan concentration, demonstrated exceptional efficacy in pollutant removal, achieving over 90% elimination of total suspended solids, cadmium (Cd), and lead (Pb), alongside a 79% reduction in color during the treatment of textile wastewater.

这项研究探讨了通过加入从木质素真菌灵芝中提取的壳聚糖来增强聚醚砜(PES)膜的性能。 利用湿相反转和溶液浇铸技术,壳聚糖成功地融入了聚醚砜基质,傅立叶变换红外光谱(FT-IR)证实了这一点,该光谱显示壳聚糖的脱乙酰度高达 75.7%。壳聚糖的加入大大提高了膜的亲水性,这表现在水接触角的减小和纯水渗透性的大幅提高,从 17.9 升/米-2-时-1 巴-1 提高到 27.3 升/米-2-时-1 巴-1。膜的防污性能也明显增强,通量回收率(FRR)从约 60% 提高到 80%。此外,壳聚糖改性的 PES/CS 膜,尤其是在壳聚糖浓度为 5%的情况下,在去除污染物方面表现出了卓越的功效,在处理纺织废水的过程中,总悬浮固体、镉(Cd)和铅(Pb)的去除率超过了 90%,色度降低了 79%。
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引用次数: 0
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