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Surfactant-modified carbon nano-onion-β-cyclodextrin nanocomposite as an efficient sorbent in dispersive solid phase extraction of metoprolol and atenolol from plasma samples prior to HPLC–PDA analysis 表面活性剂修饰的纳米碳离子-β-环糊精纳米复合材料作为一种高效吸附剂,用于在 HPLC-PDA 分析前从血浆样品中分散固相萃取美托洛尔和阿替洛尔
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-29 DOI: 10.1007/s13738-024-03107-6
Zahra Aslanabadi, Mohammad Reza Afshar Mogaddam, Faranak Ghaderi, Elnaz Marzi Khosrowshahi, Aysa Abasalizadeh, Mir Ali Farajzadeh, Mahboob Nemati

In the present study, a modified carbon nano-onion and β–cyclodextrin composite was utilized in micro-solid phase extraction of atenolol and metoprolol from human plasma samples. The synthesized sorbent structure and morphology were evaluated. In this method, a proper amount of the sorbent was contacted with the diluted plasma sample under vortexing (to promote the sorbent contact area with the solution). The separated particles by centrifugation were contacted with a proper eluent to desorb the target analytes. After that, the eluent was separated by centrifugation and used during analysis of the analytes by high-performance liquid chromatograph. Several effective extraction parameters such as the sorbent amount, type and elution solvent volume, and extraction time were evaluated and optimized. The validated factors showed that detection and quantification were 0.09 and 0.01 and 0.29 and 0.03 ng mL–1, for metoprolol and atenolol, respectively. The method precision, considered as relative standard deviation, was ≤ 2.5 and ≤ 3.6% for intra- (n = 5) and inter-day (n = 4) precisions, respectively. The extraction recovery values were obtained 84 and 63% for metoprolol and atenolol, respectively. Lastly, the developed method was utilized successfully on the plasma samples of patients treated with metoprolol and atenolol.

本研究利用改性纳米碳离子和β-环糊精复合材料对人血浆样品中的阿替洛尔和美托洛尔进行微固相萃取。对合成的吸附剂结构和形态进行了评估。在该方法中,适量的吸附剂在涡旋状态下与稀释的血浆样品接触(以增加吸附剂与溶液的接触面积)。离心分离出的颗粒与适当的洗脱液接触,以解吸目标分析物。然后,通过离心分离洗脱液,并在使用高效液相色谱仪分析分析物时使用。评估并优化了几个有效的萃取参数,如吸附剂用量、类型和洗脱溶剂量以及萃取时间。结果表明,美托洛尔和阿替洛尔的检出限和定量限分别为 0.09 和 0.01 ng mL-1 及 0.29 和 0.03 ng mL-1。方法的精密度为相对标准偏差,日内精密度(n = 5)和日间精密度(n = 4)分别为≤2.5%和≤3.6%。美托洛尔和阿替洛尔的提取回收率分别为 84% 和 63%。最后,该方法成功地应用于美托洛尔和阿替洛尔治疗患者的血浆样品中。
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引用次数: 0
Novel Eu(III) and Tb(III) complexes bearing carboxamide ligand: antiproliferative activity, photoluminescence properties, and thermogravimetric studies 含羧酰胺配体的新型 Eu(III)和 Tb(III)配合物:抗增殖活性、光致发光特性和热重研究
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-28 DOI: 10.1007/s13738-024-03112-9
Ahmet Oral Sarıoğlu, Hatice Gamze Sogukomerogullari, Ayşegül Köse, Senem Akkoc, Mehmet Sönmez, Mehmet Hakan Morcalı

In this study, β-diketone derivative new carboxamide Eu(III) and Tb(III) lanthanide complexes were synthesized and characterized by FT-IR, elemental analysis, UV–Vis, and molar conductivity techniques. There is no electrolytic conductivity in the compounds. Moreover, the photoluminescence properties and thermal behavior of the synthesized lanthanide complexes were investigated. Photoluminescence data revealed that the Tb(III) complex showed metal-based f-f transitions. The β-diketone derivative carboxamide ligand exhibited as antenna that transmitted the excited energy to the emission energy levels of the Tb(III) ion. These metal complexes were screened in two different common cancer cell lines and a human normal embryonic kidney cell line for 48 h. The results showed that these complexes have more antiproliferative activities in the colon cancer cell line compared to the lung cancer cell line.

本研究合成了β-二酮衍生物的新型羧酰胺 Eu(III)和 Tb(III)镧系配合物,并通过傅立叶变换红外光谱、元素分析、紫外可见光和摩尔电导率技术对其进行了表征。这些化合物没有电解导电性。此外,还研究了合成的镧系配合物的光致发光特性和热行为。光致发光数据显示,铽(III)配合物显示出基于金属的 f-f 转变。β-二酮衍生物羧酰胺配体作为天线将激发能量传递到 Tb(III)离子的发射能级。结果表明,与肺癌细胞系相比,这些配合物对结肠癌细胞系具有更强的抗增殖活性。
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引用次数: 0
Electrocatalytic reduction of nitrate using Mg(OH)2 copper modified electrode 使用改性铜镁(OH)2 电极电催化还原硝酸盐
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-28 DOI: 10.1007/s13738-024-03115-6
Nadia Ait Ahmed, Katia Hebbache, Samia Kerakra, Nabila Aliouane, Marielle Eyraud

In order to improve the activity of copper (Cu) towards electrolytic reduction of nitrate, thin films of magnesium hydroxide (Mg(OH)2) were deposited on Cu substrate. For the first time, these films were synthesized by electrochemical deposition in a potassium sulfate bath containing Mg2+ at 70 °C. The effect of various experimental parameters, such as deposition time and potential, on the electrocatalytic activity for the nitrate reduction was investigated. Surface analysis techniques (SEM, EDX and XRD) were used to get information on the morphology, the composition and the structure of the deposits. The activity of the modified electrode was studied by cyclic voltammetry, and amperometric method. The modified Mg(OH)2/Cu sensor exhibited a good electrocatalytic behavior towards the reduction of nitrates with high reproducible reduction peak currents. In addition, the sensor exhibits a linear answer for concentration in nitrate between 0.125 to 7 mM, combined with high sensitivity (24.6 µA mM−1 cm−2) and limit of detection (225.35 µM) values. When common interfering molecules were added to the solution, Mg(OH)2/Cu electrodes have kept their good selectivity. They demonstrated acceptable detection levels for nitrates in tap water.

为了提高铜(Cu)电解还原硝酸盐的活性,在铜基底上沉积了氢氧化镁(Mg(OH)2)薄膜。这些薄膜首次是在 70 °C、含 Mg2+ 的硫酸钾浴中通过电化学沉积法合成的。研究了沉积时间和电位等各种实验参数对硝酸盐还原电催化活性的影响。利用表面分析技术(SEM、EDX 和 XRD)了解了沉积物的形态、组成和结构。通过循环伏安法和安培法研究了修饰电极的活性。改性后的 Mg(OH)2/Cu 传感器对硝酸盐的还原具有良好的电催化性能,还原峰电流具有很高的再现性。此外,该传感器对 0.125 至 7 mM 的硝酸盐浓度呈线性响应,灵敏度(24.6 µA mM-1 cm-2)和检出限(225.35 µM)均很高。当溶液中加入常见的干扰分子时,Mg(OH)2/Cu 电极仍能保持良好的选择性。它们对自来水中硝酸盐的检测水平是可以接受的。
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引用次数: 0
Catalyst-free one-pot three-component synthesis and in silico bioactivity of new 4-pyrazolyl pyrano[3,4-c] pyrrole derivatives 新型 4-吡唑基吡喃并[3,4-c] 吡咯衍生物的无催化剂一锅三组份合成及其硅学生物活性
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-25 DOI: 10.1007/s13738-024-03125-4
Brahim Cherfaoui, Houria Lakhdari, Norah Bennamane, Hocine Merazig, Ahmed Djafri, Abdelghani Bouchama, Bellara Nedjar-Kolli

An unexpected route for the synthesis of pyrano [3,4-c] pyrrole derivatives has been reported via catalyst-free, three-component reaction of 1,3-dicarbonyl pyrazole, aromatic primary amines and fumaryl chloride. This novel cascade reaction sequence led to create two new rings and four new σ bonds containing two C–N, one C–C, and one C–O bond. The newly synthesized compounds were elucidated on the basis of their spectroscopic data (1H, 13C, 2D NMR, HRMS, IR) and additionally confirmed by single-crystal X-ray diffraction analysis. The molecular docking simulation was performed utilizing the AutoDock 4.2 program to predict the binding affinity of one derivative of the synthesized compounds to the target mitogen-activated protein kinase P38 (MAPK P38) and mitogen-activated protein kinase 14 (MAPK 14).

Graphical abstract

据报道,通过 1,3-二羰基吡唑、芳香族伯胺和富马酰氯的无催化剂三组分反应,合成吡喃 [3,4-c] 吡咯衍生物的途径出人意料。这种新型级联反应顺序产生了两个新环和四个新的σ键,其中包含两个 C-N、一个 C-C 和一个 C-O 键。新合成的化合物根据其光谱数据(1H、13C、2D NMR、HRMS、IR)进行了阐明,并通过单晶 X 射线衍射分析进行了确认。利用 AutoDock 4.2 程序进行了分子对接模拟,以预测合成化合物的一种衍生物与靶标丝裂原活化蛋白激酶 P38(MAPK P38)和丝裂原活化蛋白激酶 14(MAPK 14)的结合亲和力。
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引用次数: 0
Direct oxidative esterification of benzaldehydes and benzylalcohols using task-specific imidazolium based perchlorate ionic liquid 使用任务特异性咪唑基高氯酸盐离子液体直接氧化酯化苯甲醛和苯甲醇
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-25 DOI: 10.1007/s13738-024-03121-8
Hassan Valizadeh, Mina Ahmadi

Imidazolium perchlorate task-specific ionic liquids (TSILs) were used for in-situ oxidation esterification of benzaldehydes and benzylalcohols in reaction with alcohols. CO2H functional group containing TSIL show dual role as catalyst and reaction media toward oxidative esterifications. Excellent yields of esters could be obtained for a series of benzaldehydes and benzylalcohols via the reaction with alcohols. This reaction can be regarded as a new method for the efficient oxidation esterification of benzaldehydes and benzylalcohols under mild catalyst and solvent-free conditions.

Graphical abstract

咪唑高氯酸盐特异性离子液体(TSIL)被用于苯甲醛和苯甲醇与醇类反应的原位氧化酯化。含有 CO2H 官能团的 TSIL 在氧化酯化过程中显示出催化剂和反应介质的双重作用。通过与醇反应,一系列苯甲醛和苯甲醇可以获得极高的酯产率。该反应可视为在温和催化剂和无溶剂条件下高效氧化酯化苯甲醛和苄醇的一种新方法。
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引用次数: 0
An electrochemical sensor based on NH2-MWCNTS-CMC and ZIF-67 peroxidase-like nanocomposite for sensitive luteolin detection 一种基于 NH2-MWCNTS-CMC 和 ZIF-67 过氧化物酶样纳米复合材料的电化学传感器,用于灵敏检测木犀草素
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-23 DOI: 10.1007/s13738-024-03122-7
Lin-Lin Ma, Ke-Xin Xu, Bao-Lin Xiao, Sanad Abdalbage Mohammed Abdalsadeg, Yu-Jie Chen, Yu-Ying Li, Jun Hong, Ali Akbar Moosavi-Movahedi

Luteolin (Lut) is a flavonoid compound with antioxidant, anti-inflammatory and other biological properties. Lut has been used in many fields such as biomedicine and food safety. Therefore, the quantitative measurement of Lut is of great significance. In this study, an electrochemical sensor based on aminated multi-walled carbon (NH2-MWCNTs), sodium carboxymethylcellulose (CMC), ZIF-67 and chitosan (Chi) is developed for the measurement of Lut. NH2-MWCNTs are better dispersed by CMC, and NH2-MWCNTs are cross-linked with ZIF-67, which further improves the response and sensitivity of the electrode to the Lut due to the peroxide-like properties of ZIF-67. The detection limit and linear range of the electrochemical sensor for Lut are 2.1 nM and 0.1–7 μM, respectively. Dandelion is a traditional Chinese medicine plant containing Lut component. The prepared electrochemical sensor is also used to analysis Lut content in various parts of dandelion. The results show that the flowers part of dandelion exhibits the highest concentration of Lut; while, the leaves contain a moderate amount, and the roots are nearly devoid of Lut. These results are consistent with those obtained by ultra-high performance liquid chromatography. The electrochemical sensor has good stability and anti-interference ability, and has good potential application value in drug concentration detection and screening.

Graphical Abstract

木犀草素(Lut)是一种类黄酮化合物,具有抗氧化、抗炎和其他生物特性。木犀草素已被用于生物医学和食品安全等多个领域。因此,对芦丁进行定量测量具有重要意义。本研究开发了一种基于胺化多壁碳(NH2-MWCNTs)、羧甲基纤维素钠(CMC)、ZIF-67 和壳聚糖(Chi)的电化学传感器,用于测量路得。CMC 能更好地分散 NH2-MWCNTs,NH2-MWCNTs 与 ZIF-67 交联后,由于 ZIF-67 具有类似过氧化物的特性,进一步提高了电极对路特的响应和灵敏度。该电化学传感器对路得的检测限和线性范围分别为 2.1 nM 和 0.1-7 μM。蒲公英是一种含有路得成分的传统中药植物。制备的电化学传感器还用于分析蒲公英各部分的路得含量。结果表明,蒲公英花的络氨酸含量最高,叶的络氨酸含量适中,根的络氨酸含量几乎为零。这些结果与超高效液相色谱法得出的结果一致。该电化学传感器具有良好的稳定性和抗干扰能力,在药物浓度检测和筛选方面具有良好的潜在应用价值。 图文摘要
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引用次数: 0
Core shell ZnO-MnO2 nanocomposites for dye degradation and DFT simulation 用于染料降解的核壳 ZnO-MnO2 纳米复合材料及 DFT 模拟
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-23 DOI: 10.1007/s13738-024-03118-3
F. Joudi, W. Selmi, J. Ben Naceur, R. Chtourou

To enhance the photogeneration and separation of charge carriers, ZnO/MnO2 nanocomposites were efficiently synthesized using a simple hydrothermal process and tested as photocatalyst for dye degradation. The samples of ZnO, MnO2, and ZnO/MnO2 nanocomposites were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–vis diffuse reflection spectroscopy, and photoluminescence spectra (PL). The photocatalytic activity of the ZnO/MnO2 prepared using 10 mg was significantly higher than that of ZnO or MnO2, as demonstrated by optical and photoluminescence measurements. In fact, the degradation efficiency of methyl orange (MO) with ZnO/MnO2 (10 mg) reaching to 98% after 2 h of sunlight irradiation. The enhanced degradation of MO compared with pure ZnO and MnO2 can be attributed to the high surface area, efficient sunlight absorption, and excellent charge carrier separation of the ZnO/MnO2 photocatalyst. Density functional theory (DFT) simulations of ZnO and MnO2 further revealed the electronic origins of the structural properties, showing that the photocatalytic activity is due to the electron transitions between the valence and conduction bands of materials.

为了提高电荷载流子的光生成和分离,采用简单的水热法高效合成了 ZnO/MnO2 纳米复合材料,并将其作为光催化剂进行了染料降解测试。通过 X 射线衍射 (XRD)、扫描电子显微镜 (SEM)、紫外-可见漫反射光谱和光致发光光谱 (PL) 对 ZnO、MnO2 和 ZnO/MnO2 纳米复合材料样品进行了研究。光学和光致发光测量结果表明,使用 10 mg 制备的 ZnO/MnO2 的光催化活性明显高于 ZnO 或 MnO2。事实上,在阳光照射 2 小时后,ZnO/MnO2(10 毫克)对甲基橙(MO)的降解效率可达 98%。与纯 ZnO 和 MnO2 相比,甲基橙的降解能力更强,这主要归功于 ZnO/MnO2 光催化剂的高比表面积、高效的阳光吸收能力和出色的电荷载流子分离能力。对 ZnO 和 MnO2 的密度泛函理论(DFT)模拟进一步揭示了结构特性的电子起源,表明光催化活性是由材料价带和导带之间的电子跃迁引起的。
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引用次数: 0
Experimental and computational insights into polymorphism in an antimicrobial sulfadrug: discovery of a novel monoclinic form of sulfamerazine 通过实验和计算深入了解抗菌磺胺药的多态性:发现磺胺嘧啶的新型单斜形态
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-22 DOI: 10.1007/s13738-024-03110-x
Amani Direm, Cemal Parlak, Brahim El Bali, Mohammed S. M. Abdelbaky, Santiago García-Granda

Sulfamerazine (4-Amino-N-(4-methylpyrimidin-2-yl) benzenesulfonamide) is a polymorphic molecule crystallizing in three forms: Form I: Pn21a polymorph (with three entries in the Cambridge Structural Database CSD), Form II: Pbca polymorph (with two entries in the CSD) and Form III: P21/c polymorph with only one entry in the CSD). We have experimentally prepared a novel monoclinic P21/c polymorph (Form IV) of the sulfadrug and also obtained crystals of Form II (Pbca polymorph) by following a different synthesis procedure. Both crystals were structurally characterized by single-crystal X-ray diffraction XRD and geometrically optimized by density functional theory DFT. The five crystal structures (1), (3)–(6) of the four mentioned polymorphs were analyzed and discussed in terms of crystal packing, Hirshfeld surface analysis HSA of the intermolecular interactions, voids’ distribution in the crystal packing, their related energies and the resulting underlying topologies. The energy and activity relations of the compounds were also investigated by DFT.

磺胺甲基嘧啶(4-氨基-N-(4-甲基嘧啶-2-基)苯磺酰胺)是一种多晶型分子,有三种结晶形式:形态 I:Pn21a 多晶型(在剑桥结构数据库 CSD 中有三个条目);形态 II:Pbca 多晶型(在剑桥结构数据库 CSD 中有两个条目);形态 III:P21/c 多晶型(在剑桥结构数据库 CSD 中只有一个条目)。我们通过实验制备出了磺胺药物的一种新型单斜 P21/c 多晶体(形态 IV),并通过不同的合成程序获得了形态 II(Pbca 多晶体)的晶体。这两种晶体都通过单晶 X 射线衍射 XRD 进行了结构表征,并通过密度泛函理论 DFT 进行了几何优化。对上述四种多晶体的 (1)、(3) - (6) 五种晶体结构进行了分析和讨论,讨论的内容包括晶体堆积、分子间相互作用的 Hirshfeld 表面分析 HSA、晶体堆积中的空隙分布、其相关能量以及由此产生的基本拓扑结构。此外,还通过 DFT 研究了这些化合物的能量和活性关系。
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引用次数: 0
Synthesis of novel propargylated derivatives of noscapine using A3-coupling reaction and their anticancer properties 利用 A3 偶联反应合成莨菪碱的新型丙炔基衍生物及其抗癌特性
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-21 DOI: 10.1007/s13738-024-03116-5
Fatemeh Famarini, Peyman Salehi, Bahareh Heidari, Morteza Bararjanian, Atefeh Hajiagha Bozorgi, Afsaneh Tavasoli, Zahra Davarzani

A series of 21 novel compounds based on noscapine were synthesized and investigated as potential anticancer therapeutics. These new compounds were prepared from the N-demethylation of noscapine followed by the three-component A3-coupling of N-nornoscapine as a secondary amine, an aldehyde and a terminal alkyne catalyzed by copper iodide (CuI). Two classes of derivatives were synthesized by applying phenylacetylene and propargyl alcohol as the alkyne moiety. Chemical structures of the products were confirmed by 1HNMR, 13CNMR, and HR-MS. In vitro cytotoxicity of the synthesized derivatives was studied on MCF-7 breast cancer cell line treated with different doses of compounds for 48 h. Compounds 6l, 6n and 6h (IC50 = 18.94, 19.29 and 32.11 µM, respectively) displayed the highest potency compared to that of noscapine (IC50 = 36.38 µM).

我们合成了一系列 21 种基于莨菪碱的新型化合物,并将其作为潜在的抗癌疗法进行了研究。这些新化合物是通过碘化铜(CuI)催化 N-去甲莨菪碱作为仲胺、醛和末端炔的 N-去甲莨菪碱三组分 A3-偶联反应制备的。以苯基乙炔和丙炔醇作为炔基,合成了两类衍生物。通过 1HNMR、13CNMR 和 HR-MS 确认了产物的化学结构。化合物 6l、6n 和 6h(IC50 分别为 18.94、19.29 和 32.11 µM)与诺卡平(IC50 = 36.38 µM)相比显示出最高的效力。
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引用次数: 0
Covalent attachment of Mn-porphyrin onto functionalized activated carbon for green oxidation of olefins 将锰卟啉共价附着到功能化活性炭上,实现烯烃的绿色氧化
IF 2.2 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-10-21 DOI: 10.1007/s13738-024-03114-7
Saeed Rayati, Makan Etefagh

Complexes of first row transition metals are a promising class of inexpensive catalysts for oxidation reactions. In this work, we studied the influence of covalent immobilization of Mn-porphyrin onto the surface of activated carbon in the green oxidation of various olefins. meso-tetrakis(4-carboxyphenyl)porphyrinatomanganese(III) acetate (MnTCPP) immobilized onto hydroxylated activated carbon (AC-OH). The anchored catalyst was characterized using FTIR, UV–VIS, atomic absorption and EDX spectroscopies. TGA analysis and BET-BJH method were employed to determine thermal behavior and surface properties of complex respectively. Then, catalytic performance of MnTCPP@AC-OH was investigated in the green oxidation of olefins with molecular oxygen and hydrogen peroxide. A comparison between two green oxidants (molecular oxygen and hydrogen peroxide) shows that although more product is obtained with hydrogen peroxide, more recyclability is obtained with molecular oxygen. The separation and recovery of the nanocatalyst was simple, effective and economical in this green oxidation method and the supported catalyst can be reused at least five times without significant loss of activity.

第一排过渡金属的络合物是一类很有前途的廉价氧化反应催化剂。在这项工作中,我们研究了将锰卟啉共价固定到活性炭表面对各种烯烃绿色氧化的影响,并将中-四(4-羧基苯基)卟啉-锰(III)醋酸盐(MnTCPP)固定到羟基活性炭(AC-OH)上。使用傅立叶变换红外光谱(FTIR)、紫外可见光谱(UV-VIS)、原子吸收光谱(Atomic absorption)和乙二胺四乙酸氙(EDX)光谱对固定催化剂进行了表征。TGA分析和BET-BJH法分别测定了复合物的热行为和表面性质。然后,研究了 MnTCPP@AC-OH 在烯烃与分子氧和过氧化氢的绿色氧化过程中的催化性能。两种绿色氧化剂(分子氧和过氧化氢)之间的比较表明,虽然过氧化氢能得到更多的产物,但分子氧能得到更多的可回收性。在这种绿色氧化方法中,纳米催化剂的分离和回收简单、有效、经济,而且支撑催化剂可重复使用至少五次而不会明显丧失活性。
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引用次数: 0
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Journal of the Iranian Chemical Society
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