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Structural Elucidation and NMR Spectral Assignments of New Diphenyl Ether Derivatives From Liuweizhiji Gegen-Sangshen Oral Liquid. 六味地黄口服液中新的二苯醚衍生物的结构阐释和核磁共振谱定位
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-18 DOI: 10.1002/mrc.5496
Jinghao Cui, Xin Zhou, Baorui Teng, Dan Zhang, Xiujuan Fu, Siwei Chen, Sijing Liu, Zhi Li, Hui Lei

Chemical investigation of the Liuweizhiji Gegen-Sangshen oral liquid afforded one new diphenyl ether derivative (1), together with one known compound (2). Their structures were established by 1D and 2D NMR, and HR-ESI-MS spectroscopic analysis and the absolute configuration of 1 was confirmed by ECD calculation. Compounds 1 and 2 were evaluated for the cytotoxic activities, and compounds 1 and 2 showed weak cytotoxic activities towards HepG2 human liver cancer cells, with IC50 values of 97.3 and 79.6 μM, respectively.

通过对六味地黄格根散口服液的化学研究,发现了一种新的二苯醚衍生物(1)和一种已知化合物(2)。通过一维和二维核磁共振以及 HR-ESI-MS 光谱分析确定了它们的结构,并通过 ECD 计算确认了 1 的绝对构型。对化合物 1 和 2 进行了细胞毒活性评估,结果表明,化合物 1 和 2 对 HepG2 人肝癌细胞具有微弱的细胞毒活性,IC50 值分别为 97.3 和 79.6 μM。
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引用次数: 0
Liquid-Phase NMR of Humic and Fulvic Acids. 腐殖酸和富味酸的液相核磁共振。
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-16 DOI: 10.1002/mrc.5493
Leonid B Krivdin

Present review focuses on the most recent advances in the NMR of the coal-derived humic and fulvic acids, covering exclusively the results of the liquid-phase NMR and leaving apart an overwhelming amount of publications dealing with the solid-state NMR investigations in this field (the latter are comprehensively reviewed elsewhere). Owing to the complexity of humic and fulvic acids together with other coal-derived products, their 1H and 13C NMR spectra consist of a number of overlapping signals belonging to different hydrocarbon types. Comprehensive studies of humic and fulvic acids by means of NMR revealed characteristic functional groups of their composition together with spectral regions in which they resonate. Quantitative 1H and 13C NMR spectra characterize aromatic and saturated carbons spread over many structural moieties, which provides a solid guideline into molecular structure of humic and fulvic acids together with parent coal-derived products. Nowadays, quantitative 13C NMR measurements yield information about a variety of structural parameters such as functional group distribution, aromaticity, degree of condensation of aromatic rings, and medium chain lengths together with many other more specific parameters. The structural NMR studies of the coal-derived products are developing on a background of a marked progress in experimental and computational NMR. Discussed in the present review are the most recent advances in the liquid-state NMR studies of the coal-derived humic and fulvic acids together with their processing products.

本综述侧重于煤衍生腐植酸和富勒酸核磁共振方面的最新进展,只涉及液相核磁共振结果,而不涉及该领域大量有关固态核磁共振研究的出版物(后者在其他地方进行了全面综述)。由于腐植酸和富勒酸以及其他煤炭衍生产品的复杂性,它们的 1H 和 13C NMR 光谱由许多属于不同碳氢化合物类型的重叠信号组成。通过核磁共振对腐植酸和叶酸进行全面研究,揭示了其成分中的特征官能团及其共振谱区。定量 1H 和 13C NMR 光谱显示了分布在许多结构分子中的芳香碳和饱和碳的特征,为了解腐植酸和富勒酸以及煤衍生产品的分子结构提供了可靠的指导。如今,定量 13C NMR 测量可获得各种结构参数的信息,如官能团分布、芳香度、芳香环的缩合程度、中链长度以及许多其他更具体的参数。煤炭衍生产品的结构核磁共振研究是在实验和计算核磁共振取得显著进展的背景下发展起来的。本综述讨论了煤衍生腐植酸和富勒酸及其加工产品的液态 NMR 研究的最新进展。
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引用次数: 0
Two New Alkaloids of the Endophytic Fungus Rhizopus oryzae From Atractylodes macrocephala Koidz. 白术内生真菌 Rhizopus oryzae 的两种新生物碱 Koidz.
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-15 DOI: 10.1002/mrc.5495
Yue Meicen, Lei Hui, Teng Baorui, Fu Xiujuan, Chen Siwei, Wang Zan, Zhang Dan, Luo Yu

Two new alkaloids, named migenomycin I (1) and II (2), along with nine known compounds (3-11), were isolated from the fungus Rhizopus oryzae from Atractylodes macrocephala Koidz. The structures of compounds 1 and 2 were determined by spectroscopic methods (MS, NMR, and CD). All compounds were isolated from Rhizopus oryzae for the first time. In addition, the antitumor activities of compounds 1 and 2 and the hypoglycemic activities of most compounds were evaluated.

研究人员从白术真菌中分离出两种新生物碱,分别命名为migenomycin I(1)和II(2),以及九种已知化合物(3-11)。化合物 1 和 2 的结构是通过光谱方法(质谱、核磁共振和 CD)确定的。所有化合物都是首次从根瘤菌中分离出来。此外,还评估了化合物 1 和 2 的抗肿瘤活性以及大多数化合物的降血糖活性。
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引用次数: 0
HRMAS NMR for Studying Solvent-Induced Mobility of Polymer Chains and Metallocene Migration Into Low-Density Polyethylene (LDPE). HRMAS NMR 用于研究溶剂诱导的聚合物链流动性以及茂金属向低密度聚乙烯 (LDPE) 的迁移。
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-06 DOI: 10.1002/mrc.5484
John C Hoefler, Maxwell R Kimball, Janet Blümel

HRMAS (high-resolution magic angle spinning) nuclear magnetic resonance (NMR) spectroscopy of low-density polyethylene (LDPE) affords 1H and 13C NMR spectra with superior resolution. For acquiring HRMAS NMR spectra, the polymer is first swollen with representative organic solvents. Then, the samples are measured with a conventional solid-state NMR spectrometer in the wideline mode or at the low spinning speed of 2 kHz. Anisotropic interactions like CSA (chemical shift anisotropy) and dipolar interactions are reduced due to the additional mobility of the polymer chains in the presence of the solvent within the polymer network. The combined effect of this mobility and MAS leads to signals with substantially reduced halfwidths as compared to classic MAS of the dry polymer. With HRMAS, all signals of the polymer become visible, and the spectra can be used for a quick and easy assessment of the polymer swelling behavior in diverse solvents. Being able to characterize polymers on the molecular level, and identifying the solvents that penetrate the polymer network best, enables the study of post-synthesis modifications of the polymers. It is demonstrated by paramagnetic HRMAS that the metallocene nickelocene (Cp2Ni) penetrates the LDPE network along with the solvent and is homogeneously dispersed in the polymer. SEM images prove that the structure of the polymer is not altered by the presence of a solvent and Cp2Ni. The impact of the paramagnetic Cp2Ni on the 1H signal halfwidth and T1 time of LDPE is studied. HRMAS allows a quick assessment of metal complexes regarding their ability to penetrate the LDPE network and therefore supports future studies of catalytic polymer degradation.

低密度聚乙烯(LDPE)的 HRMAS(高分辨率魔角旋转)核磁共振(NMR)光谱可提供分辨率极高的 1H 和 13C NMR 光谱。要获取 HRMAS NMR 光谱,首先要用有代表性的有机溶剂溶胀聚合物。然后,使用传统固态 NMR 光谱仪以宽线模式或 2 kHz 的低旋转速度测量样品。由于聚合物网络中存在溶剂,聚合物链具有额外的流动性,因此 CSA(化学位移各向异性)和偶极性等各向异性相互作用会减弱。与干聚合物的传统 MAS 相比,这种流动性和 MAS 的共同作用导致信号的半宽度大大减小。有了 HRMAS,聚合物的所有信号都变得清晰可见,光谱可用于快速、轻松地评估聚合物在不同溶剂中的溶胀行为。能够在分子水平上描述聚合物的特性,并确定最能穿透聚合物网络的溶剂,有助于研究聚合物的合成后改性。顺磁 HRMAS 证明,茂金属二茂镍 (Cp2Ni) 与溶剂一起渗透到 LDPE 网络中,并均匀地分散在聚合物中。扫描电子显微镜图像证明,聚合物的结构不会因溶剂和 Cp2Ni 的存在而改变。研究了顺磁 Cp2Ni 对 LDPE 的 1H 信号半宽和 T1 时间的影响。HRMAS 可以快速评估金属复合物穿透 LDPE 网络的能力,因此有助于今后对催化聚合物降解的研究。
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引用次数: 0
Structural Elucidation and Complete NMR Spectral Assignments of Monascus Monacolin Analogs. Monascus Monacolin 类似物的结构阐释和完整 NMR 光谱分配。
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-05 DOI: 10.1002/mrc.5489
Jiachen Liu, Qingjiang Xu, Xin Wang, Ronghua Pan, Lizhong Zheng, Yonghong Zhang, Xiaoya Shang, Nan Wang

One new monacolin analog, monacolin V (1), together with two new monacolin-like natural products, 6-hydroxyl monacolin P (2) and 3-keto monacolin S (3), were isolated from the ethyl acetate portion of red yeast rice ethanol extract. Their structures were identified by HRESIMS and NMR experiments, and the complete assignments of 1H and 13C NMR data for three compounds were obtained by the aid of HSQC, HMBC, 1H-1H COSY, and NOESY data. This is the first time that the NMR data of compounds 2 and 3 have been fully assigned.

从红曲米乙醇提取物的乙酸乙酯部分中分离出了一种新的独活素类似物--独活素 V(1),以及两种新的独活素类天然产物--6-羟基独活素 P(2)和 3-酮独活素 S(3)。借助 HSQC、HMBC、1H-1H COSY 和 NOESY 数据,对三种化合物的 1H 和 13C NMR 数据进行了完整的分配。这是首次对化合物 2 和 3 的核磁共振数据进行完整的赋值。
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引用次数: 0
Reversibly Compressible Cross-Linked Polystyrene Gels, Compatible With Toluene-d8 and Pyridine-d5, for Measurement of Residual Dipolar Couplings and Residual Chemical Shift Anisotropies. 与甲苯-d8 和吡啶-d5 兼容的可逆压缩交联聚苯乙烯凝胶,用于测量残余双极耦合和残余化学位移各向异性。
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-04 DOI: 10.1002/mrc.5494
Franciane G Dos Santos, Daiane S Carvalho, Fernando Hallwass, Armando Navarro-Vázquez

A chemically cross-linked version of polystyrene is presented here that allows the preparation of reversibly mechanically compressible gels as NMR weakly aligning media. The gels can be successfully swollen in aromatic solvents such as toluene-d8 and pyridine-d5, as well as in CDCl3, and provided accurate measurements of 1DCH RDCs and 13C-RCSAs.

本文介绍了一种化学交联型聚苯乙烯,它可以制备可逆机械压缩凝胶,作为 NMR 弱对准介质。这种凝胶可以在甲苯-d8 和吡啶-d5 等芳香溶剂以及 CDCl3 中成功溶胀,并提供了 1DCH RDC 和 13C-RCSA 的精确测量。
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引用次数: 0
A New qNMR Compliant Savitzky-Golay Apodization Function for Resolution Enhancement. 用于提高分辨率的新型 qNMR 兼容型 Savitzky-Golay 光晕函数
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-03 DOI: 10.1002/mrc.5492
Carlos Cobas, José Antonio García-Pulido, Paula Mora, Giovanni Selva, Stan Sykora

In this work, we introduce a novel NMR apodization function designed to enhance spectral resolution while maintaining compatibility with qNMR standards. This function is based on a modified Savitzky-Golay filter, adapted for time-domain application. It effectively suppresses the negative components typically associated with derivative spectra, while also ensuring the preservation of quantitative integrity in NMR analyses.

在这项工作中,我们介绍了一种新型 NMR 光栅化函数,旨在提高光谱分辨率,同时保持与 qNMR 标准的兼容性。该功能基于改进的 Savitzky-Golay 滤波器,适用于时域应用。它能有效抑制通常与导数光谱相关的负成分,同时还能确保在 NMR 分析中保持定量完整性。
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引用次数: 0
NMR Relaxometry to Monitor In Situ the Loading of Amberlite IR120 and Dowex Marathon MSC Resins With Ni2+ and Cu2+ During a Column Experiment. 核磁共振弛豫测定法用于监测 Amberlite IR120 和 Dowex Marathon MSC 树脂在色谱柱实验中对 Ni2+ 和 Cu2+ 的原位加载。
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-30 DOI: 10.1002/mrc.5490
Marie Bernardi, Rodrigo de Oliveira Silva, Quoc Lam Vuong, Dimitrios Sakellariou, Yves Gossuin

The removal of heavy metal ions from wastewater often necessitates the use of ion exchange resins. Current methods for assessing ion exchange efficiency are indirect and destructive. Some heavy metal ions, such as Cu2+ and Ni2+, are paramagnetic and influence the NMR relaxation times of water protons. NMR relaxometry can therefore be utilized to track the removal of these ions by ion exchange resins. In this study, we use relaxometry to monitor in situ the loading with Ni2+ and Cu2+ of Amberlite IR120 and Dowex Marathon MSC resins, with the resin column inserted into a low-field NMR device. The multiexponential transverse relaxation curves were fitted using a biexponential model. Before and during the loading of the resin, the water with the slowest relaxation corresponds to treated water (free of Ni2+ or Cu2+) flowing between the resin beads. After saturation, the slowest fraction corresponds to the untreated solution (containing Ni2+ or Cu2+) flowing between the resin beads saturated with paramagnetic ions. The evolution with time of the transverse relaxation rate and the amplitude of the slowly relaxing water fraction shows a clear transition, occurring later at the bottom of the resin bed compared with the middle and top. This is interpreted as an indication of the saturation of the studied zone with paramagnetic ions, confirmed by the quantification of Ni2+ or Cu2+ in the effluent using AES spectroscopy. This proof-of-concept study demonstrates that NMR relaxometry can be used in situ to monitor the loading of a resin bed with paramagnetic ions.

去除废水中的重金属离子通常需要使用离子交换树脂。目前评估离子交换效率的方法既间接又具有破坏性。某些重金属离子(如 Cu2+ 和 Ni2+)具有顺磁性,会影响水质子的核磁共振弛豫时间。因此,核磁共振弛豫测定法可用于跟踪离子交换树脂去除这些离子的情况。在本研究中,我们将树脂柱插入低场 NMR 设备中,使用弛豫测定法原位监测 Amberlite IR120 和 Dowex Marathon MSC 树脂的 Ni2+ 和 Cu2+ 负载情况。使用双指数模型拟合了多指数横向弛豫曲线。在加载树脂之前和期间,弛豫速度最慢的水是在树脂珠之间流动的经过处理的水(不含 Ni2+ 或 Cu2+)。在饱和之后,最慢的部分对应于在树脂珠之间流动的未处理溶液(含有 Ni2+ 或 Cu2+),该溶液已被顺磁离子饱和。随着时间的推移,横向弛豫速率和缓慢弛豫水部分的振幅发生了明显的变化,树脂床底部发生的时间晚于中部和顶部。这可以解释为所研究区域内顺磁性离子达到饱和的迹象,并通过使用 AES 光谱定量检测流出物中的 Ni2+ 或 Cu2+ 得到证实。这项概念验证研究表明,核磁共振弛豫测量法可用于现场监测顺磁离子对树脂床的负载情况。
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引用次数: 0
To Gibbs or Not to Gibbs Effect of Entropic Contribution in the NMR Calculations of Flexible and Polar Molecules-Updating the DP4+App. 柔性和极性分子核磁共振计算中熵贡献的吉布斯效应(To Gibbs or Not to Gibbs Effect of Entropic Contribution in the NMR Calculations of Flexible and Polar Molecules)-更新 DP4+App.
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-30 DOI: 10.1002/mrc.5491
Milagros Amichetti, Bruno A Franco, María Marta Zanardi, Ariel M Sarotti

The application of quantum-based NMR methods for the structural elucidation of natural and unnatural products has grown significantly. However, accurately calculating the conformational landscape of flexible molecules with intricate intramolecular hydrogen bonding (IHB) networks continues to be a major challenge. In this work, we thoroughly studied the effect of entropic contributions (trough Gibbs free energies calculations) in the DP4+ performance. Our results show that to solve biased systems with strong IHB interactions requires computing the Boltzmann contributions using Gibbs free energies computed with at least triple-ξ basis set and SMD solvation model. In response to this finding, we have updated our DP4+App, a user-friendly Python applet that automates the entire process of calculating DP4+ probabilities. In the new version, the program allows for calculating of conformational contributions at any selected theory level, using either SCF or Gibbs free energies.

基于量子的核磁共振方法在天然和非天然产物的结构阐释方面的应用已大幅增长。然而,精确计算具有复杂分子内氢键(IHB)网络的柔性分子的构象格局仍然是一项重大挑战。在这项工作中,我们深入研究了熵贡献(通过吉布斯自由能计算)对 DP4+ 性能的影响。结果表明,要求解具有强 IHB 相互作用的偏态系统,需要使用至少三ξ基集和 SMD 溶解模型计算的吉布斯自由能来计算玻尔兹曼贡献。针对这一发现,我们更新了 DP4+App 程序,这是一个用户友好的 Python 小程序,可以自动完成 DP4+ 概率的整个计算过程。在新版本中,该程序允许使用 SCF 或吉布斯自由能计算任何选定理论水平的构象贡献。
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引用次数: 0
Understanding the Interactions of Nanoparticles and Dissolved Organic Matter at the Molecular Level by 1H 2D Multi-Exponential Transverse Relaxation NMR Spectroscopy. 通过 1H 2D 多指数横向弛豫 NMR 光谱了解纳米粒子与溶解有机物在分子水平上的相互作用。
IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-16 DOI: 10.1002/mrc.5487
Malak Dia, Jonathan Farjon, Clotilde Raveleau, André Simpson, Pierre-Emmanuel Peyneau, Béatrice Béchet, Denis Courtier-Murias

The interaction between humic acid (HA) and engineered nanoparticles (NPs) is critical in environmental sciences, especially for understanding the behavior of NPs in natural waters. This study employs 1H 2D Multi-Exponential Transverse Relaxation (METR) NMR spectroscopy to examine the molecular-level interactions between Pahokee Peat humic acid (HA) and carboxyl-functionalized iron oxide nanoparticles (NPCOs). First, 1H 2D METR NMR spectroscopy allowed not only the identification of HA in terms of its chemical composition but also the separation of molecules with the same chemical shift values but different rates of molecular tumbling. Then, using solutions with varying NPCO concentrations (0, 10, 40, and 100 μM), we observed significant changes in the T2 relaxation times of HA components, indicating interactions between HA and NPCO. Analysis showed the biggest effect on two chemical shift regions, corresponding to lipids and carbohydrates, revealing that smaller molecules within these regions exhibit the most significant changes in T2 values upon the addition of NPCO. This suggests that these molecules are the initial sites of interaction, with the entire HA system being affected at higher NPCO concentrations. These findings highlight the utility of METR NMR spectroscopy in studying complex environmental mixtures and provide insights into the behavior of HA and NPs, essential for understanding the fate of NPs in the environment.

腐植酸(HA)与工程纳米粒子(NPs)之间的相互作用在环境科学中至关重要,特别是对于了解天然水体中 NPs 的行为。本研究采用 1H 2D 多指数横向弛豫(METR)核磁共振波谱来研究帕霍基泥炭腐植酸(HA)与羧基功能化氧化铁纳米粒子(NPCOs)之间的分子级相互作用。首先,通过 1H 2D METR NMR 光谱不仅可以识别 HA 的化学成分,还可以分离出化学位移值相同但分子翻滚速率不同的分子。然后,使用不同浓度的 NPCO 溶液(0、10、40 和 100 μM),我们观察到 HA 成分的 T2 弛豫时间发生了显著变化,这表明 HA 与 NPCO 之间存在相互作用。分析表明,与脂质和碳水化合物相对应的两个化学位移区域受到的影响最大,这表明在添加 NPCO 后,这些区域中的小分子在 T2 值上表现出最显著的变化。这表明这些分子是相互作用的初始位点,当 NPCO 浓度较高时,整个 HA 系统都会受到影响。这些发现凸显了 METR NMR 光谱在研究复杂环境混合物方面的实用性,并提供了有关 HA 和 NPs 行为的见解,这对了解 NPs 在环境中的归宿至关重要。
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引用次数: 0
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Magnetic Resonance in Chemistry
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