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Magnetic Nanoparticles Based on DABCO as Catalysts in the Knoevenagel Reaction and Synthesis of Isatin-β-thiosemicarbazones 基于DABCO的磁性纳米颗粒在Knoevenagel反应及Isatin-β-硫代氨基脲合成中的催化作用
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230030
N. Falcão, Gilvan P. Pires, Paloma Abrantes, Poliana Abrantes, João Batista M. Resende Filho, Claudio Lima Junior, E. Teotonio, J. Vale
This work describes the route to prepare a novel core-shell catalyst based on 1,4-diazabicyclo[2,2,2]octane (DABCO) supported magnetic nanoparticles (MNPs). The morphology and composition of the obtained catalysts were characterized by Fourier-transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), X-ray powder diffraction (XRD), transmission electron microscopy (TEM), quantum design vibrating sample magnetometer (VSM) and scanning electron microscopy (SEM). These nanomaterials presented high performance as a basic catalyst for Knoevenagel condensation between malononitrile and aldehydes, leading to products with excellent yields (84-99%) and short reaction times (5-60 min). Furthermore, it was also efficient in the condensation of isatins with 4-phenylthiosemicarbazide, resulting in isatin-β-thiosemicarbazones with high yields (81-94%) and short times (60-180 min). It is worth mentioning that the catalyst was recovered and reused in these two kinds of reactions after six cycles without significant yield loss.
本文描述了一种基于1,4-重氮杂环[2,2,2]辛烷(DABCO)负载磁性纳米颗粒(MNPs)的新型核壳催化剂的制备路线。采用傅里叶红外光谱(FTIR)、热重分析(TGA)、x射线粉末衍射(XRD)、透射电子显微镜(TEM)、量子设计振动样品磁强计(VSM)和扫描电子显微镜(SEM)对催化剂的形貌和组成进行了表征。这些纳米材料作为丙二腈和醛之间的Knoevenagel缩合反应的基本催化剂,具有优异的收率(84-99%)和较短的反应时间(5-60 min)。此外,它还能有效地将isatin与4-苯基硫代氨基脲进行缩合,得到收率高(81-94%)、时间短(60-180 min)的isatin-β-硫代氨基脲类化合物。值得一提的是,在这两种反应中,催化剂经过6个循环后都得到了回收再利用,且产率损失不大。
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引用次数: 0
Dereplication of Sclerotiorin-Like Azaphilones Produced by Penicillium meliponae Using LC-MS/MS Analysis and Molecular Networking LC-MS/MS分析及分子网络技术对梅利蓬青霉类核蛋白氮杂啉类化合物的脱皮作用
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230027
E. Peres, Mayane P. Souza, T. Sousa, C. da Silva, A. Barros, F. D. da Silva, E. Costa, L. D. de Medeiros, M. Forim, A. D. de Souza, Weider H. P. Paz, G. D. da Silva, A. D. de Souza, H. Koolen
Penicillium meliponae, a recently described and rare species, was isolated as an endophytic fungus from the Amazonian plant Duguetia sthelechantha, and has been proven to be a pigment producer. Considering the high productivity of this species and the lack of data on its chemical composition, the present study aimed to characterize the chemical profile of P. meliponae and evaluate the influence of agitation and the use of different culture media. For this purpose, liquid chromatography coupled with mass spectrometry (LC-MS/MS) and molecular networking were used, allowing the identification of 17 azaphilone molecules with sclerotiorin-like skeletons, becoming the first chemical report of this species. In addition, the different production patterns in the tested culture media were indicative that this species is sensitive to changes in the composition of the carbon source and to the presence of agitation. Furthermore, this work contributes to the fragmentation mechanisms of the different possible structural arrangements for azaphilones of the sclerotiorin type and serves as a repository of information on the gas-phase behavior of this type of metabolite in mass spectrometry experiments and will assist future studies aimed at the discovery of azaphilones.
青霉菌(Penicillium meliponae)是最近发现的一种罕见的内生真菌,它是从亚马逊地区的植物Duguetia stheelechantha中分离出来的,并已被证明是一种色素生产真菌。考虑到该物种的高产和缺乏化学成分的数据,本研究旨在表征P. meliponae的化学特征,并评估搅拌和不同培养基使用的影响。为此,利用液相色谱-质谱联用(LC-MS/MS)和分子网络技术,鉴定了17个具有类似于菌核蛋白骨架的氮唑啉分子,成为该物种的首次化学报道。此外,培养基中不同的生产模式表明,该物种对碳源组成的变化和搅拌的存在很敏感。此外,这项工作有助于研究固结蛋白类型的氮化氮酮的不同可能结构排列的断裂机制,并在质谱实验中为这类代谢物的气相行为提供信息库,并将有助于未来旨在发现氮化氮酮的研究。
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引用次数: 0
Validation of an Analytical Method by Headspace Gas Chromatography with Flame Ionization and Evaluation of Matrix Effect of Volatile Compounds in Cat Food 顶空气相色谱火焰电离分析方法的验证及猫粮中挥发性化合物基质效应的评价
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230026
Bruno Carvalho, Patrícia dos Santos, Geovane da Silva, C. Senes, J. Visentainer, O. Santos
This study describes the validation of a headspace gas chromatography with flame ionization (HS-GC-FID) method for the determination of propanal, pentanal, hexanal, octanal, and trans-2-nonenal originated by lipid oxidation from cat food samples, as well as the evaluation of the matrix effect in the results. This method was applied to the analysis of commercial cat food and proved to be suitable for the determination of these volatile compounds in different samples. Mean recoveries between 88 and 109% were obtained and repeatability expressed as relative standard deviation was always lower than 6.95%. The intra- and inter-assay precisions ranged from 0.44 to 20.88% and from 0.45 to 20.52%, respectively. In addition, the matrix effect of cat food samples was determined by comparing the slopes of the standard addition method, and the external calibration curve and its influences were verified. These results highlight the high potential of this method, which allows the determination of lipid oxidation products in cat food samples directly, without requiring prior sample preparation techniques.
本研究描述了顶空气相色谱-火焰离子化(HS-GC-FID)法测定猫粮样品中脂质氧化产生的丙醛、戊醛、己醛、辛醛和反式2-壬烯醛的有效性,并对结果中的基质效应进行了评价。将该方法应用于商品猫粮的分析,证明该方法适用于不同样品中挥发性成分的测定。平均加样回收率为88 ~ 109%,重复性为相对标准偏差小于6.95%。检测内、间精密度分别为0.44 ~ 20.88%和0.45 ~ 20.52%。此外,通过对比标准添加法的斜率来确定猫粮样品的基质效应,并验证外部校准曲线及其影响。这些结果突出了该方法的巨大潜力,该方法可以直接测定猫粮样品中的脂质氧化产物,而不需要事先的样品制备技术。
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引用次数: 0
Recent Synthetic Developments of Asymmetric Multicomponent Transformations: Strecker, Mannich, Passerini and Ugi Reactions 非对称多组分转化的合成新进展:Strecker, Mannich, Passerini和Ugi反应
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230082
Marcelo H R Carvalho, G. Amarante, P. D. de Castro
Multicomponent reactions (MCRs) are important transformations, which allow the attainment of structurally complex derivatives in a single step, starting from three or more compounds with relatively simple structures. These reactions are generally associated with the principles of green chemistry, allowing the incorporation of most (or all) atoms of the starting materials in the products (atom economy) and reducing purification steps (and, consequently, the need for solvents and waste production). For a long time, asymmetric methodologies (in special enantioselective protocols) for most multicomponent transformations remained a gap in the literature, limiting the use of these reactions to produce derivatives only as racemates or in low diastereoselectivities. Over the last two decades, a better comprehension of the mechanisms associated with these transformations allowed the development of efficient enantio- and diastereoselective procedures, attracting the interest of both academia and industry. In this review, selected examples of four important multicomponent reactions (Strecker, Mannich, Passerini and Ugi) will be discussed, presenting a general overview of the development of this field and pointing out possible advantages and limitations of the above mentioned methodologies. In some cases, discussions around mechanisms, proposed transition states and activation modes will be detailed disclosed.
多组分反应(mcr)是一种重要的转化反应,它允许从三个或更多结构相对简单的化合物开始,一步得到结构复杂的衍生物。这些反应通常与绿色化学原理有关,允许在产品中加入大部分(或全部)起始材料的原子(原子经济)并减少净化步骤(因此,需要溶剂和废物产生)。长期以来,大多数多组分转化的不对称方法(在特殊的对映选择性协议中)在文献中仍然是一个空白,限制了这些反应的使用,只能以外消旋体或低非对映选择性的形式产生衍生物。在过去的二十年中,对这些转化相关机制的更好理解使得有效的对映和非对映选择性过程得以发展,吸引了学术界和工业界的兴趣。在这篇综述中,选择了四个重要的多组分反应(Strecker, Mannich, Passerini和Ugi)的例子进行讨论,提出了该领域发展的总体概述,并指出上述方法可能的优势和局限性。在某些情况下,将详细披露围绕机制、提议的过渡态和激活模式的讨论。
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引用次数: 0
Application of Disposable Pipette Extraction for Determination of Yb by High‑Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry Using Lanthanum as a Chemical Modifier 以镧为化学改性剂的一次性移液管萃取法在高分辨连续源石墨炉原子吸收光谱法测定镱中的应用
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230021
Diogo M. Betiolo, Heloisa R. Cadorim, E. Carasek, Tatiane Maranhão
The use of extraction technique with disposable tips (DPX) was applied for the first time for the extraction and preconcentration of Yb in samples of liquid waste from the petrochemical industry and environmental water using bioabsorbent cork. The use of cork as an extracting phase in the determination of Yb by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) was evaluated. The pyrolysis and atomization temperatures were optimized at 1400 and 2400 ºC, respectively. H2SO4, HNO3 and HCl acids were compared in the steps of cleaning the extraction phase and desorption of the analyte by DPX. The best extraction in the selected conditions was obtained with pH 8.0 and 5% v/v HCl. The recoveries were close to 100% for residual water and drinking water, 33 to 77% for produced water and 64 to 93% for river water. Tests with interfering ions in different concentrations were performed. The relative limit of quantification (LOQ) and limit of detection (LOD) were estimated at 0.03 and 0.01 µg L-1, respectively. The total time for the preparation of the samples by DPX was close to 1 min per sample. Extraction and pre-concentration were observed using DPX with a preenrichment factor of approximately 4 times.
首次将一次性尖端提取技术(DPX)应用于生物吸附软木对石油化工废液和环境用水样品中Yb的提取和富集。研究了高分辨率连续源石墨炉原子吸收光谱法(HR-CS GF AAS)中以软木为萃取相测定Yb的方法。优化的热解温度为1400℃,雾化温度为2400℃。比较了H2SO4、HNO3和HCl酸对分析物萃取相的清洗和DPX解吸的影响。在所选条件下,pH为8.0,HCl为5%,提取效果最佳。剩余水和饮用水的回收率接近100%,采出水的回收率为33 ~ 77%,河水的回收率为64 ~ 93%。用不同浓度的干扰离子进行了试验。相对定量限(LOQ)和检出限(LOD)分别为0.03和0.01µg L-1。DPX制备样品的总时间接近1 min /个样品。用预富集因子约为4倍的DPX进行提取和预富集。
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引用次数: 0
Warmingins A, B and C, Three New Furofuran Lignans from Aristolochia warmingii Mast. (Aristolochiaceae) 马兜铃属植物中3种新的呋喃木脂素A、B、C。(马兜铃科)
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230019
C. Cunha, Paulo Vinícius de Antonio, Maria do Carmo Gomes Lustosa, Á. Cruz, J. Holzbach, D. Pereira, Isabele R. Nascimento
The genus Aristolochia stands out as the most representative of the Aristolochiaceae plant family, with approximately 550 species distributed around the world, many of which have little or no studies reported in the literature. Investigation of the acetone extract from leaves of Aristolochia warmingii Mast. resulted in the isolation and identification of twenty-three compounds, mostly lignans and neolignans, including the new furofuran lignans warmingin A (1), warmingin B (2) and warmingin C (3). The structures of the compounds were established by comprehensive spectroscopic and spectrometric analyses. A large amount of (−)-epieudesmin (4) was isolated from the extract, which suggests that A. warmingii could be a potential source of this compound. The hexane, acetone, ethanol, and ethanol Soxhlet extracts, in addition to fourteen of the isolated compounds, were evaluated for their ability to inhibit the formation of advanced glycation end products (AGEs), but they did not show significant activities.
马兜铃属是马兜铃科植物中最具代表性的一种,大约有550种分布在世界各地,其中许多在文献中很少或没有研究报道。温马兜铃叶丙酮提取物的研究。结果分离鉴定了23个化合物,主要为木脂素类和新木脂素类,包括新呋喃木脂素类化合物warmingin A(1)、warmingin B(2)和warmingin C(3)。通过综合光谱和光谱分析确定了化合物的结构。从该提取物中分离出大量的(−)-epieudesmin(4),这表明A. warmingii可能是该化合物的潜在来源。正己烷、丙酮、乙醇和乙醇索氏提取物,以及14个分离的化合物,被评估为它们抑制晚期糖基化终产物(AGEs)形成的能力,但它们没有显示出显著的活性。
{"title":"Warmingins A, B and C, Three New Furofuran Lignans from Aristolochia warmingii Mast. (Aristolochiaceae)","authors":"C. Cunha, Paulo Vinícius de Antonio, Maria do Carmo Gomes Lustosa, Á. Cruz, J. Holzbach, D. Pereira, Isabele R. Nascimento","doi":"10.21577/0103-5053.20230019","DOIUrl":"https://doi.org/10.21577/0103-5053.20230019","url":null,"abstract":"The genus Aristolochia stands out as the most representative of the Aristolochiaceae plant family, with approximately 550 species distributed around the world, many of which have little or no studies reported in the literature. Investigation of the acetone extract from leaves of Aristolochia warmingii Mast. resulted in the isolation and identification of twenty-three compounds, mostly lignans and neolignans, including the new furofuran lignans warmingin A (1), warmingin B (2) and warmingin C (3). The structures of the compounds were established by comprehensive spectroscopic and spectrometric analyses. A large amount of (−)-epieudesmin (4) was isolated from the extract, which suggests that A. warmingii could be a potential source of this compound. The hexane, acetone, ethanol, and ethanol Soxhlet extracts, in addition to fourteen of the isolated compounds, were evaluated for their ability to inhibit the formation of advanced glycation end products (AGEs), but they did not show significant activities.","PeriodicalId":17257,"journal":{"name":"Journal of the Brazilian Chemical Society","volume":"1 1","pages":""},"PeriodicalIF":1.4,"publicationDate":"2023-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"68330120","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Corrosion Electrochemical Behavior of 2024 Aluminum Alloy in Potassium Acetate Deicing Fluid 2024铝合金在醋酸钾除冰液中的腐蚀电化学行为
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230024
Lin Xiuzhou, Zhuo Wei, Yang Feng, Yang Han, P. Qiang, Mei Yongjun, Wang Yuhao, Dou Baojie
The low-temperature electrochemical corrosion behavior of aircraft 2024 aluminum alloy was investigated in different concentrations of potassium-acetate-type fluid, and the results showed that the corrosion medium initially impacted some corrosiveness on the 2024 aluminum alloy. However, the corrosion rate of the alloy decreased with prolonged immersion in the corrosion medium, and this was attributed to the protective effect of the corrosion products layer, which impeded the attack by the aggressive solution. Time-domain analysis of electrochemical noise measurements at -5 °C revealed the occurrence of uniform corrosion on the alloy at the initial stages of immersion, general corrosion at the middle stages of immersion, and a pitting-dominated corrosion type from the middle to late stages of immersion.
研究了飞机2024铝合金在不同浓度的醋酸钾型流体中的低温电化学腐蚀行为,结果表明,腐蚀介质首先对2024铝合金的腐蚀性产生一定的影响。然而,合金的腐蚀速率随着腐蚀介质浸泡时间的延长而降低,这是由于腐蚀产物层的保护作用,它阻碍了腐蚀溶液的侵蚀。-5℃时电化学噪声测量的时域分析表明,合金在浸液初期出现均匀腐蚀,浸液中期出现一般腐蚀,浸液中后期以点蚀为主。
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引用次数: 1
Larvicidal Activity of Calcium Alginate Microcapsules Containing Clove Essential Oil Obtained by Microfluidics 丁香精油海藻酸钙微胶囊的杀幼虫活性研究
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230029
D. Conde, L. Mendes, Guilherme Ramos, Rafael G. Silva, Á. Teixeira, R. Teixeira, Gustavo Martins, C. Cerceau, R. Lopes
Essential oils (EO) have diverse applications, such as antibacterial and antifungal activity. However, they are susceptible to oxidation in the presence of air, light, and moisture. In addition, they are thermally unstable. In this sense, it is necessary to develop techniques to increase the lifespan of EO. In this work, EO was obtained from cloves and characterized by different techniques. The major compounds found were eugenol (83%), eugenol acetate (9%), and β-caryophyllene (8%). The EO was encapsulated by extrusion using a microfluidic device. The sodium alginate was used as wall material, and the CaCl2 solution was used as a crosslinking agent. The microcapsule presented sizes of 164.7 ± 0.3 µm, with an encapsulation yield of 64 ± 14%. Functional characteristic groups of EO were observed in the microcapsule by infrared and Raman spectroscopies. The microcapsule increased the thermal decomposition of the EO from 162 to 230 °C. Release kinetics of the capsule was performed, with an equilibrium time of 72 h and release of 54% of the EO. Finally, the pure EO and encapsulated EO-microcapsules were applied in the Aedes aegypti larvae control, showing mean lethal concentration necessary to eliminate 50% (LC50) values of 74.4 and 96.9 µg mL-1 and lethal concentration necessary to eliminate 90% (LC90) of 106.2 and 133.3 µg mL-1 for pure EO and encapsulated EO, respectively. Therefore, it was concluded that these microcapsules have the potential for application in the Aedes aegypti larvae control.
精油(EO)具有多种用途,如抗菌和抗真菌活性。然而,它们在空气、光和湿气的存在下容易氧化。此外,它们是热不稳定的。从这个意义上说,有必要开发延长EO寿命的技术。本研究从丁香中提取EO,并采用不同的工艺进行表征。主要化合物为丁香酚(83%)、丁香酚醋酸酯(9%)和β-石竹烯(8%)。采用微流控装置对EO进行挤压封装。以海藻酸钠为壁材,CaCl2溶液为交联剂。微胶囊尺寸为164.7±0.3µm,包封率为64±14%。用红外光谱和拉曼光谱观察了微胶囊中EO的功能特征基团。微胶囊使EO的热分解从162℃提高到230℃。进行了胶囊的释放动力学,平衡时间为72 h,释放了54%的EO。最后,将纯EO和包封EO微胶囊用于埃及伊蚊幼虫对照,结果表明,纯EO和包封EO微胶囊消除50% (LC50)所需的平均致死浓度分别为74.4和96.9µg mL-1,消除90% (LC90)所需的平均致死浓度分别为106.2和133.3µg mL-1。因此,该微胶囊在控制埃及伊蚊幼虫方面具有一定的应用潜力。
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引用次数: 0
COVID-19 Infection Changes the Functions and Morphology of Erythrocytes: A Multidisciplinary Study COVID-19感染改变红细胞功能和形态:一项多学科研究
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230031
Marcos V. S. Sales, E. Tanabe, T. Maciel, M. Tavares, Juliana Leal, L. Pinto, Keyla S. N. Pires, Jorge Coelho, E. Silva, Samuel Souza, E. Fonseca, Thiago Fragoso, Thiago Aquino, A. Borbely, U. Rocha, Josué Santos, A. C. Leite
Hematological problems are associated with Coronavirus disease 2019 (COVID-19). Respiratory impairment is the higher point studied, although without experimental studies related to the oxygen transport performed by erythrocytes. Therefore, we decided to investigate if erythrocytes from COVID-19 patients have their functionality changed. The case-control study included hospitalized patients with a positive real-time polymerase chain reaction (RT-PCR) result admitted to University Hospital. Volunteers (negative RT-PCR results) were recruited as a control group. Thus, we assessed different erythrocytes parameters, oxidative stress markers, and biophysical studies using whole blood and isolated hemoglobin. We found a decrease of 51% in oxygen uptake and reduced antioxidant enzyme activity in COVID-19 patients compared to controls. Raman spectrometry showed structural changes in the hemoglobin and lipids of the erythrocytes from COVID-19 patients; thus, these results were consolidated with an increase in Young’s modulus in erythrocytes followed by morphology changes. Besides, isolated hemoglobin from COVID-19 patients has a distinct interaction profile using a ligand model compared to the control. COVID-19 leads to structural, functional, and morphological damage to human erythrocytes. Our data showed structural and molecular changes and induction of oxidative stress in erythrocytes by COVID-19, a new perspective on the contribution of erythrocytes to a respiratory commitment in COVID-19.
血液学问题与2019冠状病毒病(COVID-19)有关。呼吸损伤是研究的较高点,尽管没有与红细胞进行氧运输相关的实验研究。因此,我们决定调查COVID-19患者的红细胞是否有功能改变。病例对照研究纳入了实时聚合酶链反应(RT-PCR)阳性的住院大学医院患者。招募志愿者(RT-PCR阴性)作为对照组。因此,我们评估了不同的红细胞参数,氧化应激标志物,并使用全血和分离血红蛋白进行生物物理研究。我们发现,与对照组相比,COVID-19患者的摄氧量和抗氧化酶活性下降了51%。拉曼光谱分析显示COVID-19患者红细胞血红蛋白和脂质结构变化;因此,这些结果与红细胞杨氏模量的增加以及形态学的改变相一致。此外,与对照相比,与配体模型相比,从COVID-19患者分离的血红蛋白具有独特的相互作用谱。COVID-19会对人红细胞造成结构、功能和形态损伤。我们的数据显示了COVID-19在红细胞中的结构和分子变化以及诱导氧化应激,这为红细胞在COVID-19呼吸承诺中的贡献提供了新的视角。
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引用次数: 0
A Hybrid Molecularly Imprinted Polymer for Selective Adsorption of Urinary S-Phenylmercapturic Acid 一种用于选择性吸附尿S-苯巯基尿酸的杂化分子印迹聚合物
IF 1.4 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-07-24 DOI: 10.21577/0103-5053.20230032
Rafaela Gomes, Marina Tonucci, M. Prete, C. Tarley, B. Baeta, R. Afonso
A hybrid molecular imprinted polymer (HMIP) obtained by the organic monomer 4-vinylpyridine (4-VP) and the inorganic precursor tetraethyl orthosilicate (TEOS) was synthesized for the selective extraction of urinary S-phenylmercapturic acid (u-SPMA), a biomarker of benzene exposure. The chemical and structural characterization of the synthetic adsorbent was performed by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and textural analysis employing N2 adsorption-desorption isotherms. Selective and adsorptive performance of the imprinted polymers were evaluated by kinetic, isothermal, thermodynamic, and selectivity studies. The kinetic data were well adjusted to pseudo-second order and intraparticle diffusion models, leading to selectivity coefficient (K) value of 0.03 g mg-1 min-1 for HMIP. In addition, the adsorption isotherms were better described by the Sip model achieving a maximum adsorption capacity of 284.81 μg g-1 (at 288.15 K).
以有机单体4-乙烯基吡啶(4-VP)和无机前体正硅酸四乙酯(TEOS)为原料合成了一种杂化分子印迹聚合物(HMIP),用于选择性提取尿中苯暴露的生物标志物s -苯基巯基酸(u-SPMA)。通过傅里叶红外光谱(FTIR)、热重分析(TGA)和N2吸附-脱附等温线的结构分析对合成吸附剂进行了化学和结构表征。印迹聚合物的选择性和吸附性能通过动力学、等温、热力学和选择性研究进行了评价。动力学数据调整为准二级和颗粒内扩散模型,使得HMIP的选择系数(K)值为0.03 g mg-1 min-1。在288.15 K条件下,其吸附量最大可达284.81 μg -1。
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引用次数: 0
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Journal of the Brazilian Chemical Society
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