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Analysis of Forced Degradation Products in Rilpivirine using RP-HPLC and Peak Purity Evaluation 利用 RP-HPLC 和峰值纯度评估分析利匹韦林中的强制降解产物
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005/ojc/390613
Abburi Ramarao, Guttikonda Venkata Rao, S. Chinnamaneni, Komati Navya Sri, Mandava Bhagya Tej, Gollammudi Padma Rao, V. Abbaraju, Mandava Venkata Basaveswarao RaoBasaveswarao Rao
The primary objective of this research was to delve into the forced degradation products of Rilpivirine hydrochloride (RLP HCl), a crucial non-nucleoside reverse transcriptase inhibitor employed inmanagement of epidemic disease named HIV-1. The investigation utilised the probable of RP-HPLC in tandem with peak purity assessment .In order to simulate conceivable degradation pathways, the study encompassed a gamut of stress conditions like acidic, alkaline, oxidative , thermal and photolytic environments. Authors used Agilent zorbaxEclipse XDB C18 column (150x2.1mm, 1.8µm), RLP and impurities were separated. Buffer as pH of 3.0 and acetonitrile in gradient mode (68:32v/v), flow rate of 0.55ml/min. Volume injected is 3µL and detection wavelength is 220 nm. Temperature is maintained at 55oC by 70:30v/v mixture of water and acetonitrile.System suitability was erect to be within the limits. The average percentage recoveries for impurities were 98% to 101%.The outcomes of this meticulous study unveiled the susceptibilities of RLP to a spectrum of stress factors, in the generation of impurity profile RLP-Amide A, RLP-Amide Band Z-RLP with peak purities. The forced degradation tests demonstrate that the peak of RP-HPLC is spectroscopically pure in all stressed conditions. All degradation products are separated from the main peak and do not interfere with main substance. This exploration not only augments the comprehension of RLP’s stability profile but also underscores the pivotal role of analytical techniques in upholding the safety and efficacy benchmarks of pharmaceutical formulations.
本研究的主要目的是深入研究盐酸利匹韦林(RLP HCl)的强制降解产物,它是一种重要的非核苷类逆转录酶抑制剂,用于治疗名为 HIV-1 的流行病。为了模拟可能的降解途径,研究涵盖了各种压力条件,如酸性、碱性、氧化、热和光解环境。作者使用安捷伦 zorbaxEclipse XDB C18 色谱柱(150x2.1 毫米,1.8 微米)分离 RLP 和杂质。缓冲液 pH 值为 3.0,乙腈为梯度模式(68:32v/v),流速为 0.55 毫升/分钟。进样量为 3µL,检测波长为 220 nm。温度保持在 55 摄氏度,水和乙腈的混合比例为 70:30v/v。这项细致研究的结果揭示了 RLP 对各种应力因素的敏感性,产生了 RLP-Amide A、RLP-Amide Band Z-RLP 等杂质谱图,并具有峰值纯度。强制降解测试表明,在所有应力条件下,RP-HPLC 的峰值在光谱上都是纯的。所有降解产物都与主峰分离,不会干扰主物质。这项研究不仅加深了人们对 RLP 稳定性的理解,还强调了分析技术在维护药物制剂安全性和有效性基准方面的关键作用。
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引用次数: 0
Structural and Functional Dynamics of Secondary Metabolite from Actinokineospora cibodasensis against Pseudomonas aeruginosa Biofilm cibodasensis 放线菌次生代谢物抗铜绿假单胞菌生物膜的结构和功能动力学研究
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005/ojc/390619
Sreelakshmi K.S, U. R
Biofilm formation has incredible detrimental effects and has brought huge issue to our daily life. Pseudomonas aeruginosa is recognized as an opportunistic pathogen and its one of the antibiotic resistance mechanisms includes biofilm formation. To survive against harsh environmental conditions the microorganisms form an extracellular polymeric substance matrix. Natural products, particularly, marine natural products have been established useful in providing new chemical entities to mark biofilm inhibition and dole out as a rich source of privileged frames for studying chemical as well as biological applications. In the present study, antibiofilm potential of bioextract from Actinokineospora cibodasensis (MW513387) is tested against Pseudomonas aeruginosa (ATCC 27853) biofilm. The analysis of the quorum sensing modulation was done using exopolysaccharide (EPS) quantification and Cytotoxicity assays were performed to check toxicity. Scanning electron microscopy (SEM) was also conducted to visualize the mitigation of biofilm using the biocontrol agent. All the assays conducted evidently indicated that the potential bioactive compound from Actinokineospora cibodasensis has greater inhibition effect against pathogenic biofilm. In the near-term years it is expected that these pharmaceutical compounds from natural source be translated into antibiofilm drugs.
生物膜的形成具有令人难以置信的有害影响,给我们的日常生活带来了巨大的问题。铜绿假单胞菌(Pseudomonas aeruginosa)被认为是一种机会性病原体,其抗生素耐药性机制之一就是生物膜的形成。为了在恶劣的环境条件下生存,微生物会形成胞外聚合物物质基质。天然产品,尤其是海洋天然产品已被证实可提供新的化学实体来抑制生物膜,并为研究化学和生物应用提供了丰富的特权框架。本研究测试了 Actinokineospora cibodasensis(MW513387)生物提取物对铜绿假单胞菌(ATCC 27853)生物膜的抗生物膜潜力。使用外多糖(EPS)定量分析法定量感应调节作用,并进行细胞毒性试验检查毒性。此外,还使用扫描电子显微镜(SEM)观察生物控制剂对生物膜的缓解作用。所有检测结果都清楚地表明,Actinokineospora cibodasensis 的潜在生物活性化合物对病原体生物膜具有更强的抑制作用。在不久的将来,这些来自天然的药物化合物有望转化为抗生物膜药物。
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引用次数: 0
Preparation and Characterization of Organosiloxanes with A Liquid Crystalline Trans-4-Pentylcyclohexanoate Moiety 具有液晶反式-4-戊基环己酸酯分子的有机硅氧烷的制备与表征
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005/ojc/390601
Li-Chuan Wu, Chih-Hung Lin
In the course of this research, we successfully created three series of liquid crystalline compounds featuring the trans-cyclohexane structure. One series of compounds featured a double bond at the terminal position of the molecules, whereas the remaining two series incorporated disiloxane and trisiloxane groups. Each series comprised five spacers of different lengths, specifically 3, 4, 5, 6, and 11 methylene units. We identified the structures of the synthesized compounds using Nuclear Magnetic Resonance spectroscopy and characterized their liquid crystalline behavior through thermal analysis and polarized optical microscopy. The results revealed that both the length of the spacer and the presence of siloxane groups significantly influenced the liquid crystal phase transitions, transition temperatures, and temperature ranges. These findings provide valuable insights for designing and developing new liquid crystal materials with tailored properties for various applications.
在这项研究过程中,我们成功地制造出了三个系列的液晶化合物,它们都具有反式环己烷结构。其中一个系列的化合物在分子末端位置含有双键,而其余两个系列则含有二硅氧烷和三硅氧烷基团。每个系列都包含五个不同长度的间隔物,具体为 3、4、5、6 和 11 个亚甲基单元。我们利用核磁共振光谱确定了合成化合物的结构,并通过热分析和偏振光学显微镜鉴定了它们的液晶行为。结果表明,间隔物的长度和硅氧烷基团的存在对液晶相变、转变温度和温度范围都有显著影响。这些发现为设计和开发具有量身定制特性的新型液晶材料提供了宝贵的启示。
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引用次数: 0
Discovery of New Isoniazid Derivatives As Anti-tubercular Agents: In silico Studies, Synthesis, and In vitro Activity Evaluation 发现新的异烟肼衍生物作为抗结核药物:硅学研究、合成和体外活性评估
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005/ojc/390610
Abida Ash Mohd, Mohd Imran, Noura Yousif Alnaser, Shams Saud Altimyat, Nawaf M. Al-Otaibi, A. Bawadekji
This research aimed to discover novel isoniazid (INH) derivatives as anti-tubercular (anti-TB) agents. The chemical structures of isoniazid-based pyridazinone (IBP) derivatives were designed, and their toxicity and pharmacokinetic properties were predicted using the ProTox II and Swiss-ADME databases. The molecular docking of non-toxic IBPs was also performed concerning INH, pyrazinamide (PYZ), ethionamide (ETH), macozinone (MCZ), and BTZ043 utilizing DprE1 enzyme’s proteins (PDB IDs: 4F4Q, 4NCR and 6HEZ). Based on the in silico study results, IBP19, IBP21, IBP22, and IBP29 were selected for their synthesis, and the spectral analysis confirmed their chemical structures. In vitro, anti-TB activity against Mtb H37Rv strain and MTT assay (against HepG2 and Vero cell lines) of IBP19, IBP21, IBP22, and IBP29 were also carried out. A total of eleven non-toxic IBPs were identified with promising pharmacokinetic parameters. The docking score (DS in kcal/mol against 6HEZ protein) of IBP19 (-9.52), IBP21 (-8.78), IBP22 (-9.07), and IBP29 (-9.99) was better than MCZ (-8.76) and BTZ043 (-8.56) revealing their DprE1 enzyme inhibitory action. The in vitro anti-TB activity evaluation (MIC values) confirmed that IBP19 (1.562 µg/ml), IBP21 (1.562 µg/ml), IBP22 (1.562 µg/ml), and IBP29 (1.562 µg/ml) had almost double potency than INH (3.125 µg/ml), and PYZ (3.125 µg/ml). IBP19, IBP21, IBP22, and IBP29 also displayed a CC50 value of > 300 µg/ml against HCL and VCL cell lines. This effect was better than INH (> 200 µg/ml), ETH (> 150 µg/ml), and PYZ (> 200 µg/ml). Accordingly, IBP19, IBP21, IBP22, and IBP29 provide a new template for developing safe and effective novel DprE1 inhibitors.
这项研究旨在发现新型异烟肼(INH)衍生物作为抗结核(TB)药物。研究人员设计了基于异烟肼的哒嗪酮(IBP)衍生物的化学结构,并利用 ProTox II 和 Swiss-ADME 数据库预测了它们的毒性和药代动力学特性。此外,还利用 DprE1 酶蛋白(PDB IDs:4F4Q、4NCR 和 6HEZ)对 INH、吡嗪酰胺(PYZ)、乙硫酰胺(ETH)、大嗪酮(MCZ)和 BTZ043 等无毒 IBP 进行了分子对接。根据硅学研究结果,IBP19、IBP21、IBP22 和 IBP29 被选中用于合成,光谱分析证实了它们的化学结构。此外,还对 IBP19、IBP21、IBP22 和 IBP29 进行了抗 Mtb H37Rv 菌株的体外抗结核活性试验和 MTT 试验(针对 HepG2 和 Vero 细胞株)。共鉴定出 11 种无毒的 IBP,其药代动力学参数很有希望。与 MCZ(-8.76)和 BTZ043(-8.56)相比,IBP19(-9.52)、IBP21(-8.78)、IBP22(-9.07)和 IBP29(-9.99)的对接得分(对 6HEZ 蛋白的 DS,单位为 kcal/mol)更高,显示了它们对 DprE1 酶的抑制作用。体外抗结核活性评估(MIC 值)证实,IBP19(1.562 微克/毫升)、IBP21(1.562 微克/毫升)、IBP22(1.562 微克/毫升)和 IBP29(1.562 微克/毫升)比 INH(3.125 微克/毫升)和 PYZ(3.125 微克/毫升)几乎具有双倍的效力。IBP19、IBP21、IBP22 和 IBP29 对 HCL 和 VCL 细胞株的 CC50 值也大于 300 µg/ml。这一效果优于 INH(> 200 µg/ml)、ETH(> 150 µg/ml)和PYZ(> 200 µg/ml)。因此,IBP19、IBP21、IBP22 和 IBP29 为开发安全有效的新型 DprE1 抑制剂提供了新的模板。
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引用次数: 0
Effect of Sn-incorporation on the Structural and Optical Properties of ZnO Thin Films Prepared by Sol-Gel Method 掺入锡对溶胶-凝胶法制备的氧化锌薄膜的结构和光学特性的影响
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005/ojc/390614
Hansraj Sharma, Sunil Kumar, Jagavendra Yadav, Jagdish Prasad, Mangej Singh
In this research, thin films of ZnO doped with Sn were prepared through the sol-gel method. The effects of Sn dopant on optical, morphological and structural studies were investigated. All of the films in this work showed favored orientation along the (002) plane, according to XRD analysis. It was observed by SEM analysis that the study Sn morphological and structural studies were investigated. From AFM pictures it is clear that as the doping concentration rises, the size of the grains on the surface of thin films decreases.The existence of Zn, O and Sn was verified by the EDAX analysis. The Ultraviolet-visible spectroscope was utilized to examine the optical characteristics. That band gap increased with the dopant material percent increased.
本研究采用溶胶-凝胶法制备了掺杂锡的氧化锌薄膜。研究了掺杂锡对光学、形态和结构研究的影响。根据 XRD 分析,本研究中的所有薄膜都沿着 (002) 平面显示出良好的取向。通过扫描电镜分析,可以观察到对锡形态和结构的研究。从原子力显微镜图片可以看出,随着掺杂浓度的增加,薄膜表面的晶粒尺寸减小。紫外-可见光谱仪用于检测光学特性。带隙随着掺杂材料百分比的增加而增大。
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引用次数: 0
Adaptive Paramagnetism and Photoluminescence in Nitrogen Co-doped Mn: CdS Composite Quantum Dots 氮共掺杂 Mn.CdS 复合量子点中的自适应顺磁性和光致发光CdS 复合量子点
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005//ojc/390603
Surya Sekhar Reddy M, Kishore Kumar Y B
Manganese-doped cadmium sulfide quantum dots (QDs), co-doped with nitrogen, were synthesized using the chemical co-precipitation method (CPM). Surfactant 2-mercaptoethanol (ME) was used to efficiently regulate the size of these QDs. X-ray diffraction (XRD) analyses verified that the particles fell within the nano-dimension, measuring between 1-2 nm. A Rietveld analysis with X’pert high score software (XPHS) proved that these synthesized QDs contained many phases. The energy dispersive X-ray spectroscopy (EDX) technique confirmed the successful incorporation of both manganese and nitrogen dopants into the CdS. Ultraviolet-visible analysis (UV-Vis) demonstrated a noticeable shift towards the blue end in the energy gap, indicating the presence of a quantum-confinement effect. The photoluminescence (PL) investigations revealed a significant emission peak at λ = 634 nm, linked to the transition from 4T1 to 6A1, attributed to the incorporation of Mn2+ within the CdS core. Electron paramagnetic spectroscopy (EPR) demonstrated paramagnetic characteristics. EPR assessments of the g factor (1.995) and hyperfine splitting constant (A) values (7 mT) verified the existence of nitrogen and manganese ions in the tetrahedral positions of the CdS core. The notable alterations noticed in the magnetic and optical characteristics of the fabricated quantum dots imply promising uses in optoelectronic and magneto-luminescent applications.
利用化学共沉淀法(CPM)合成了锰掺杂硫化镉量子点(QDs)和氮掺杂硫化镉量子点(QDs)。表面活性剂 2-巯基乙醇(ME)可有效调节这些量子点的尺寸。X 射线衍射(XRD)分析证实,这些颗粒的尺寸在 1-2 纳米之间,属于纳米级。利用 X'pert 高分软件(XPHS)进行的里特维尔德分析证明,这些合成的 QDs 包含许多相。能量色散 X 射线光谱(EDX)技术证实,锰和氮掺杂剂都成功地加入到了 CdS 中。紫外可见光分析(UV-Vis)显示,能隙明显向蓝端移动,表明量子会聚效应的存在。光致发光(PL)研究显示,在 λ = 634 纳米处有一个显著的发射峰,与 4T1 到 6A1 的转变有关,这归因于 Mn2+ 在 CdS 内核中的掺入。电子顺磁谱(EPR)显示了顺磁特性。对 g 因子(1.995)和超频分裂常数(A)值(7 mT)进行的电子顺磁共振评估证实了氮和锰离子存在于 CdS 内核的四面体位置。所制备量子点的磁学和光学特性发生了显著变化,这意味着其在光电和磁致发光应用领域大有可为。
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引用次数: 0
Synthesis, Characterization, Density Functional Theory Studies and Antioxidant Activity of Novel Hydrazone Ligands and their Metal Complexes 新型腙配体及其金属复合物的合成、表征、密度泛函理论研究和抗氧化活性
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005/ojc/390624
V. Suleman, Abdul Ghany Mohammed Al-Daher
Novel hydrazone ligands (HL) derived from 2,5-hexandione and benzoyl hydrazine (HDBH), 2-furoyl hydrazine (HDFH), or 2-picolinoyl hydrazine (HDPH) were used to synthesize mononuclear Mn(II), Co(II), Ni(II), Cu(II), and Zn(II) complexes of the general formula [M(L)2].xH2O (x= 0-3). The hydrazone ligands and the isolated complexes were characterized by, spectral, thermal analysis, molar conductance, and magnetic moment measurements. Beside, density functional theory (DFT) computations have been to study structures and energetic of the ligand and its complexes. The IR spectral information suggests that the ligands exhibit monobasic tridentate behavior through their ONO donor atoms. The metal complexes were determined to possess monomeric octahedral geometry. The DPPH antioxidant capability of both the ligand and their metal complexes was evaluated.
研究人员利用源自 2,5-hexandione 和苯甲酰肼 (HDBH)、2-呋喃基肼 (HDFH) 或 2-吡啶酰肼 (HDPH) 的新型腙配体 (HL) 合成了通式为 [M(L)2].xH2O(x= 0-3)的单核 Mn(II)、Co(II)、Ni(II)、Cu(II) 和 Zn(II) 配合物。通过光谱、热分析、摩尔电导和磁矩测量,对腙配体和分离出的配合物进行了表征。此外,还通过密度泛函理论(DFT)计算研究了配体及其配合物的结构和能量。红外光谱信息表明,配体通过其 ONO 给体原子表现出单基三叉行为。金属配合物被确定为具有单体八面体几何形状。对配体及其金属配合物的 DPPH 抗氧化能力进行了评估。
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引用次数: 0
Evaluation of Lead Removal by Activated Citrus Sinensis Biochar Impregnated with Calcium Alginate Beads 海藻酸钙珠浸渍的活性柑橘生物炭除铅效果评估
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005/ojc/390615
Vandana Kachhwaha, Pooja Kumari, Naresh Giri, P. Mishra
This study introduces an innovative method of using activated carbon derived from orange peels incorporated into calcium alginate beads to remove lead from synthetic water efficiently. This novel approach demonstrates remarkable effectiveness in addressing lead pollution in water. Established techniques such as SEM and FTIR were employed to characterize the adsorbents created in the laboratories. Batch studies confirmed the lead adsorbed were conducted to evaluate the efficiency of lead removal, with the highest removal efficiencies achieved at pH 6.5 (90.3%), an adsorbent dose of 2 mg (90.3%), a contact time of 50 minutes (92.3%), and an initial lead solution concentration of 20 ppm (93.2%). The study employed various adsorption models, including Langmuir, Freundlich, and Tempkin models. The Langmuir model exhibited an excellent fit to the adsorption isotherm at 60 °C, as indicated by a high linear regression correlation coefficient. For the bioadsorption process, pseudo-second-order kinetics fits well (R2 = 0.9992). The analytical results verify that activated carbon from discarded orange peels and calcium alginate beads effectively removes Pb, offering an encouraging solution for water purification challenges.
本研究介绍了一种创新方法,即使用从橘子皮中提取的活性炭与海藻酸钙珠结合,高效去除合成水中的铅。这种新方法在解决水中铅污染问题方面效果显著。实验室采用了扫描电镜和傅立叶变换红外光谱等成熟技术来表征吸附剂。在 pH 值为 6.5(90.3%)、吸附剂剂量为 2 毫克(90.3%)、接触时间为 50 分钟(92.3%)、初始铅溶液浓度为 20 ppm(93.2%)时,去除率最高。研究采用了多种吸附模型,包括 Langmuir 模型、Freundlich 模型和 Tempkin 模型。Langmuir 模型对 60 °C 时的吸附等温线有很好的拟合效果,线性回归相关系数很高。对于生物吸附过程,伪二阶动力学拟合得很好(R2 = 0.9992)。分析结果证实,从废弃橘子皮和海藻酸钙珠中提取的活性炭可有效去除铅,为解决水净化难题提供了令人鼓舞的解决方案。
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引用次数: 0
Efficient Adsorption of Trivalent Rare Earth Elements Using Nano Copper Ferrite: Kinetics, Isotherms and Thermodynamics 使用纳米铜铁氧体高效吸附三价稀土元素:动力学、等温线和热力学
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005/ojc/390628
Sudha Thotakura
Rare earth elements (REEs) have versatile applications in various industries and are thrown as industrial waste waters, which leads to serious environmental issues.This paper describes the adsorption efficiency of nano copper ferrite on REEs namely lanthanum and cerium in their trivalent states at room temperature and at the optimum conditions of pH, contact time, adsorbent, adsorbate dosage,temperature etc. The batch adsorption studies were conducted for the adsorption studies using ICPAES (Inductive coupled plasma atomic emission spectro photometer). In addition the data is studied for Langmuir and Freundlich models and observed that data well fitted to Langmuir monolayer adsorption. From the graph and intercept values of theoretical and experimental values, the pseudo second order kinetics are followed. Thermodynamic parameters reveal that reaction is spontaneous and endothermic. From the over all observations like fast kinetics, chemical stability, high adsorption capacity it is concluded that nano CuFe 2 O 4 has maximum efficiency for the adsorption of REEs
本文介绍了纳米铜铁氧体在室温以及 pH 值、接触时间、吸附剂、吸附剂用量和温度等最佳条件下对三价态稀土元素(镧和铈)的吸附效率。使用 ICPAES(电感耦合等离子体原子发射光谱光度计)进行了批量吸附研究。此外,还研究了 Langmuir 和 Freundlich 模型的数据,发现数据与 Langmuir 单层吸附非常吻合。从理论值和实验值的曲线图和截距值来看,采用的是假二阶动力学。热力学参数表明,反应是自发的、内热的。从快速动力学、化学稳定性和高吸附容量等所有观察结果可以得出结论,纳米 CuFe 2 O 4 对稀土元素的吸附效率最高。
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引用次数: 0
Rheology of Cottonseed (Gossypium hirsutum) Oil used as Biodegradable Lubricant 用作生物可降解润滑剂的棉籽油的流变性能
IF 0.5 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-12-27 DOI: 10.13005/ojc/390633
Ioana Stanciu
Vegetable oils are often associated with well-known varieties like sunflower, olive, and corn. However, there are lesser-known options worth exploring to appreciate their distinct qualities. One such overlooked oil is cottonseed oil, derived from the Malvaceae cotton family plant. In a recent study, we delved into the rheological behavior of cottonseed oil. Similar to many vegetable oils, it exhibits a non-Newtonian behavior, making it a viable alternative to mineral oils. The rheological analysis was conducted using the Brookfield RVDV II I Ultra Rheometer, with shear rates incrementally increasing.
植物油通常与葵花籽油、橄榄油和玉米油等知名品种有关。然而,还有一些鲜为人知的选择值得我们去探索,以领略它们的独特品质。棉籽油就是这样一种被忽视的油,它提取自锦葵科棉花属植物。在最近的一项研究中,我们深入研究了棉籽油的流变行为。与许多植物油类似,棉籽油也表现出非牛顿特性,使其成为矿物油的可行替代品。流变分析使用 Brookfield RVDV II I 超流变仪进行,剪切速率逐渐增加。
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引用次数: 0
期刊
Oriental Journal Of Chemistry
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