Optimization of Microwave-Assisted Extraction (MAE) for the Isolation of Antioxidants from Basil (Ocimum basilicum L.) by Response Surface Methodology (RSM)

Abstract

The recovery of antioxidants from basil (Ocimum basilicum L.) was modeled with the aid of response surface methodology (RSM) using microwave-assisted extraction (MAE). Face-centered central design (FCCD) was employed to optimize the MAE operational parameters including the extraction time (1 to 7?min), extraction temperature (30 to 120?°C), solid-to-solvent ratio (0.1 to 0.4), and solvent concentration (20 to 80% ethanol, v/v), and to obtain the best possible combinations of these parameters for a high antioxidant yield from basil. The total antioxidant capacity (TAC) was expressed in trolox (TR) equivalents per gram of dried sample (DS). Three of the operational parameters (temperature, extraction time and solvent concentration) were shown to have significant effect on the extraction efficiency of antioxidants in basil extracts (p?<?0.05). The solvent concentration was shown to be the most significant factor on antioxidant yield obtained by MAE. There was a close relationship between experimental and predicted values using the proposed method. This optimized MAE method shows an application potential for the efficient extraction of antioxidants from basil in the food and pharmaceutical industries.     

基于二茂铁的两个查尔酮衍生物的合成及超快三阶非线性光学响应

二茂铁是合成新颖有机功能材料的基本单元之一。 本文设计并合成了两个基于二茂铁的同分异构查尔酮衍生物:1-二茂铁基-3-(噻吩-2-基)丙烯酮(a)和1-二茂铁基-3-(噻吩-3-基)丙烯酮(b)。 采用超快激光Z-扫描技术(脉宽180 fs,波长532 nm)测定了化合物a和b的三阶非线性光学性质。 结果表明,化合物a吸收系数β=-2.1×10^-12 m/W,折射率n₂=1.9×10^-19 m²/W,分子超极化率γ=5.37×10^-32 esu;化合物b:β=-1.2×10^-13 m/W,n₂=2.0×10^-19 m²/W,γ=4.48×10^-32 esu。 说明在飞秒激光激发下,电荷转移能够在化合物a和b分子内部快速进行,二者均具有优异的超快三阶非线性光学响应。 在B3LYP/6-311+G(d,p)理论水平下,计算了化合物a和b分子轨道能量、极化率和各基团在前线分子轨道中的占有率。 理论计算结果显示,二茂铁基团在化合物a和b前线分子轨道中占有率分别为97%和98%,对两化合物的非线性光学性能起主导作用。     

高分散纳米薄水铝石和纳米氧化铝的制备及其对甲基橙的吸附性能

以硝酸铝为铝源,尿素为沉淀剂,采用无模板水热法合成纳米薄水铝石(γ-AlO(OH))。在不同温度下煅烧后,得到氧化铝产物(γ-Al2O_3和θ-Al2O_3)。利用X射线衍射(XRD)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FTIR)、氮气吸附-脱附法和紫外-可见分光光度计(UV-Vis)对产物进行了表征分析。并且研究了产物对甲基橙(MO)的吸附性能,系统地考察了吸附时间、溶液的pH值、甲基橙浓度及循环使用对产物吸附性能的影响。此外,还对吸附过程进行了相关吸附理论研究。结果表明:与其他方法所制备的产物相比,通过该方法获得的产物的分散性更高,形态更均匀和完整。产物为高度分散的纳米捆扎状结构。γ-AlO(OH)对甲基橙的最大吸附量达1 492.5 mg·g~(-1)。另外,产物的吸附机制包含化学作用吸附机制和静电作用吸附机制等。3种产物对甲基橙的吸附均符合Langmuir单分子层吸附模型,吸附过程均符合二级动力学特征。     

Cu-Fe-PILC催化C3H6选择性还原NO的性能

采用羟基铁离子柱撑Na-Mont制备出1.0Fe-PILC,通过超声浸渍法合成不同铜负载量的nCu-Fe-PILC,并测试了其在富氧条件下催化C_3H_6选择性催化还原NO的性能。通过N_2吸附脱附、XRD、UV-Vis、H_2-TPR、Py-FTIR等技术手段表征催化剂的微观结构和物化性质,进一步解释其催化反应机理。结果表明,Cu的引入提高了1.0Fe-PILC的中低温活性和抗水硫能力。其中9Cu-Fe-PILC在300℃时NO转化率可达69.8%以上,400℃后NO转化率保持在99%以上且水硫影响较小。XRD、N_2吸附脱附结果表明,催化剂的SCR活性与所负载的活性组分和催化剂的吸附能力有关。UV-Vis结果表明,9Cu-Fe-PILC具有较强的中低温活性,与其含有较多的游离态Cu~(2+)有关。H_2-TPR结果表明,与1.0Fe-PILC相比,经Cu修饰的nCu-Fe-PILC获得了中低温还原能力。Py-FTIR结果表明,nCu-Fe-PILC表面同时含有Lewis酸和Br?nsted酸,Lewis酸是影响催化剂SCR活性的主要因素。     

Use of Cucurbit[6]uril as Ionophore in Ion Selective Electrodes for Etilefrine Determination in Pharmaceuticals

Cucurbiturils are macrocyclic molecules and have been used with promising results in the development of electrochemical sensors and biosensors due to their main properties such as shape, selectivity, binding interactions and solubility. However, its application for the development of ion selective electrodes has been scarce. In this work, cucurbit[6]uril was used as molecular‐recognition compound for etilefrine sensing membrane with potentiometric transduction. The etilefrine selective electrode was evaluated and proposed as an alternative methodology for pharmaceutical quality control. Different membranes composition were evaluated, considering the use of different solvent mediators and the presence of anionic additives. The best membrane comprises 9.24 mmol.Kg^?1 of cucurbit[6]uril, 68.90 % (w/w) of dibutylsebacate and 30.18 % (w/w) of carboxylated polyvinyl chloride. The electrode exhibited selective cationic response toward the etilefrine in a concentration interval of more than four decades, with an slope of 57.4±0.5 mV dec^?1, a practical detection limit of (8±1)×10^?7 mol L^?1 and a low limit of linear range of (1.25±0.28)×10^?6 mol L^?1. The selectivity of the electrode towards different interfering was high. A comparative evaluation of the accuracy and precision of both procedures was done using the t‐student test (t4,12=1.135) and the Fischer test (F12,4=2.42) and compared with the tabulated ones (t4,12=1.135, F11,3=5.91) for the level of confidence of 95 %.     

Electrospun EGNPs reinforced precursor carbon nanofibril composites by using RSM

Response surface methodology (RSM),based on five‐level, four variable Box‐Benkhen technique was investigated for modeling the average fiber diameter of electrospun polyacrylonitrile (PAN) nanofibers. The four important electrospinning parameters were studied including applied voltage (kV), Berry's number, deposition distance from nozzle to collector (cm), and spinning angle (? in degree). The measured fiber diameters were in a good agreement with the predicted results by using RSM technique. High‐regression coefficient between the variables and the response (R² = 87.74%) indicates excellent evaluation of experimental data by second‐order polynomial regression model. The optimum PAN average fiber diameters of 208 and 37‐nm standard deviation were collected at 19 kV, Berry's number = 10, 25^° spinning angle, and 16‐cm deposition distance. The PAN/N,N‐dimethylformamide (DMF) polymer solution with the optimum weight concentration (10 wt.%) was selected to study the effect of dispersing exfoliated graphite nanoplatelets (EGNPs) in PAN/DMF solution on the electrospun EGNP/PAN fibril composite diameter. Five different EGNPs weight concentrations (2, 4, 6, 8, and 10 wt.%) were dispersed in the optimized PAN/DMF polymer solution. Morphology of EGNPs/PAN fibril composites and its distribution were investigated by scanning electron microscopy (SEM) to show the minimum fiber diameter for the above‐mentioned 5 wt. % of EGNPs. A minimum fibril composite diameter of 182 nm was obtained at 10 wt.% of EGNPs. Morphological characteristics of electrospun fibers and their distribution were tested by Raman spectroscopy, SEM, differential light scattering, and high‐resolution transmission electron microscopy.     

Ion‐imprinted poly(methyl methacrylate‐vinyl pyrrolidone)/poly(vinylidene fluoride) blending membranes for selective removal of ruthenium(III) from acidic water solutions

While conventional approaches have been studied for removal of ruthenium(III) ions (Ru(III)), this work focuses on the applicability of ion‐imprinted poly(methyl methacrylate‐vinyl pyrrolidone)/poly(vinylidene fluoride) blending membranes (Ru(III)–ion‐imprinted membrane[IIM]) for selective removal of Ru(III) from acidic water solutions. In order to measure the effectiveness of these imprinted membranes, after fabrication, binding experiments were done with aqueous Ru(III) solutions. The results showed that Ru(III)‐IIMs were fabricated successfully at various blending ratios, and their chemical components, microstructures, hydrophilicity, and water fluxes were measured. In pH range 0.5 to 5.0, binding capacity (Q_e) of Ru(III) onto Ru(III)‐IIM increases remarkably with pH and then reaches to a maximum value (53.52 mg/g) at pH 1.5. After that, Q_e gradually decreases. Compared with a nonimprinted membrane, Ru(III)‐IIM demonstrates higher selectivity for Ru(III) at pH 1.5 in the presence of Ni(II) and Cu(II) ions, and its selectivity coefficients for Ru(III)/Ni(II) and Ru(III)/Cu(II) are 3.70 and 3.32, respectively. Also, Ru(III)‐IIM shows a good chemical stability and reusability. C─N and C═O bonds within poly(vinyl pyrrolidone) segments of poly(methyl methacrylate‐vinyl pyrrolidone) (P(MMA‐VP)) participate the uptake of Ru(III). Ru(III)‐IIM exhibited excellent hydrophilicity and Ru(III) selective adsorption ability and reusability and has potential to be used for Ru(III) removal from acidic water solutions.     

Spectroscopic ellipsometric characterization of TiAlN/TiAlON/Si3N4 tandem absorber for solar selective applications

Sputter deposited TiAlN/TiAlON/Si₃N₄ tandem absorber has been characterized by spectroscopic ellipsometry in the wavelength range of 450-1200 nm. Each layer of the tandem absorber viz., TiAlN, TiAlON and Si₃N₄ has been deposited separately on copper substrate (Cu) and ellipsometric measurements have been carried out on each of these layers. The measured ellipsometric spectra were fitted with theoretically simulated spectra and the sample structure and wavelength dispersion of optical constants of each layers have been determined. The ellipsometric measurements have also been carried out on the three-layer tandem absorber deposited on Cu substrate. By analyzing the ellipsometric data, depth profiling of the tandem absorber has been carried out using the derived optical constants of the individual layers.     

Study of closed orbit response to magnet vibrations at the SSRF storage ring

This paper presents the analytical and simulation responses of the closed orbit distortion in the SSRF storage ring to random and plane wave like magnet vibrations respectively. It is shown that the use of girder is very beneficial in the view of suppressing this response function. Effect of the independently supported gradient bending magnets to the closed orbit response is given. An analytic formula is written to give a rough estimate of the closed orbit distortion due to ground motion, taking into account the closed orbit response function and girder transfer function. As an example, the result of SSRF case is given.     

Coupling resonance of floating slab and supporting concrete box structure

This paper mainly investigates the effect of coupling resonance of floating slab and supporting short concrete box. The similarities and differences in vibration behaviors between long (30 m) and short (1.5 m) lengths of concrete box structures with the same cross-section were analyzed with finite element model (FEM). The results suggest that the major local modes for vibration and structure-borne sound radiation for long and short box structures are the same. A short concrete hollow box was constructed to verify the theoretical vibration results, and six combinations of floating slabs were installed on the box to identify the vibration and structure-borne sound control by experimental method. The resonance modes due to either concrete box or floating slab should degrade the vibration isolation performance of the floating system. There may be strong coupling between roll mode (rigid body rotation mode in the y-z plane) of the floating slab and local distortion mode of the short box structure and this can change the vibration resonance frequencies and amplify the vibration.