Selective Solvent Research Articles

Comprehensive Single-Platform Lipidomic/Metabolomic Analysis Using Supercritical Fluid Chromatography-Mass Spectrometry.

Supercritical fluid chromatography (SFC) is a rapidly expanding technique in the analysis of nonpolar to moderately polar substances and, more recently, also in the analysis of compounds with higher polarity. Herein, we demonstrate a proof of concept for the application of a commercial SFC instrument with electrospray ionization-mass spectrometry (MS) detection as a platform for the comprehensive analysis of metabolites with the full range of polarities, from nonpolar lipids up to highly polar metabolites. The developed single-platform SFC-MS lipidomic/metabolomic method is based on two consecutive injections of lipid and polar metabolite extracts from biphase methyl tert-butyl ether extraction using a diol column and two different gradient programs of methanol-water-ammonium formate modifier. Detailed development of the method focused mainly on the pressure limits of the system, the long-term repeatability of results, and the chromatographic performance, including optimization of the flow rate program, modifier composition and gradient, and injection solvent selection. The developed method enabled fast and comprehensive analysis of lipids and polar metabolites from plasma within a 24 min cycle with two injections using a simple analytical platform based on a single instrument, column, and mobile phase. Finally, the results from SFC-MS analysis of polar metabolites were compared with widely established liquid chromatography MS analysis in metabolomics. The comparison showed different separation selectivity of metabolites using both methods and overall lower sensitivity of the SFC-MS due to the higher flow rate and worse chromatographic performance.

Assessment of alcoholic extraction of Jatropha curcas L. oil for potential reactive extraction towards fatty esters

This work dealt with the extraction of Jatropha oil using methanol and ethanol as solvents to evaluate a potential integration of extraction-transesterification to produce fatty esters. For comparison purposes, additional extractions were carried out with n-hexane as industrial benchmark solvent. The effects of type of solvent, particle size (0.44–3.57 mm), and seed-to-solvent ratio (1:4, 1:6, and 1:8 w/v) were evaluated with respect to oil yield, efficiency, saponification index (SI, mgKOH/g) and acid value (AV, mgKOH/g). As expected, highest oil yield (50.4% wt.) was obtained using n-hexane, but with a low selectivity to saponifiable materials (SI ∼ 166). When using alcohols, oil yield (8–31% wt.) and efficiency (17–70%) were lower and the quality of the oil was poor (SI 32–176; AV 4–5). Results indicated that, differently from previously claimed, integrated alcoholic extraction with alkaline transesterification would not be suitable for fatty esters production. By using experimental data and the Hildebrandt solubility parameters, it was possible to fit a continuous model suitable for further optimization and solvent selection in Jatropha oil extraction. The model was validated by predicting expected SI and oil yield using an untested solvent (i.e. petroleum ether), and difference between model predictions and experimental observations were less than 3%.

Solvent Selection Guided by Self-Consistent Field Theory for Improved Dispersion of Metal–Organic Frameworks in Polymers

Solvent Selection Guided by Self-Consistent Field Theory for Improved Dispersion of Metal–Organic Frameworks in Polymers

Recovery of filter paperase from mouldy rice husk in solid state fermentation by Aspergillus protuberus

Recovery of enzymes such as FPase (filter paperase) or exoglucanase from fermented substrate is a sustainable approach in enzyme production; however, there is a scarcity of optimization studies in this field. The present study was aimed to standardize number of parameters (selection of solvent, solvent volume, soaking time, leaching conditions and number of washes) to extract maximum amount of FPase from fermented rice husk by Aspergillus protuberus. Novel Aspergillus protuberus was first report from our lab on cellulases production in solid state fermentation (SSF). Among the tested solvents, citrate phosphate buffer (0.02 M, pH 5.0) proved best solvent for maximum recovery of FPase. Consequent experimental parameters were further optimized with citrate phosphate buffer. Two washes with citrate phosphate buffer each by shaking (60 min) in a ratio of 1 g of rice husk: 5 ml of citrate phosphate buffer together attained higher recovery efficiency (88 %) of FPase from the fermented rice husk.

Synthesis and theoretical studies of the conformational behaviour of N-vinylcaprolactam/N-vinylimidazole copolymers in selective solvent

Using complementary experimental and theoretical approaches, we demonstrate a way to obtain stimuli-responsive copolymers that form reversible globular nanostructures.

Self-assembly of rod-coil-rod block copolymers in a coil-selective solvent: coarse-grained simulation results.

The solution self-assembly of amphiphilic polymers provides a versatile approach to design novel nanostructured materials. Multiblock polymers, particularly those composed of liquid crystalline and coil blocks, are of significant interest due to the potential display of nematic ordering in liquid crystalline domains, offering intriguing optical and mechanical properties. In this study, dissipative particle dynamics is used to investigate the solution self-assembly of rod-coil-rod copolymers in a coil-selective solvent. Extensive molecular simulations were conducted to elucidate the impact of polymer composition, concentration and flexibility on the self-assembly behavior. A quantitative analysis was performed to investigate how polymer conformations varied with changes in composition, concentration, and rigidity. Simulation results show that, at small rod compositions, rod-coil-rod polymers self-assemble into micelles at low concentrations, transitioning to network formation as concentration increases. An increase in rod composition leads to the formation of larger aggregates, resulting in cylindrical micelles and membranes. The results reported here also offer insights into the role of flexibility in shaping the self-assembly behavior of rod-coil-rod triblocks in selective solvents, thus, contributing to a comprehensive understanding of the factors governing the formation of diverse structures in the solution self-assembly of triblock copolymers.

Synthesis and self-assembly of the amphiphilic homopolymers poly(4-hydroxystyrene) and poly(4-(4-bromophenyloxy)styrene)

Amphiphilic homopolymer synthesis and formation of micelles and vesicles in selective solvents.

Self-assembly of amphiphilic asymmetric comb-like copolymers with responsive rigid side chains.

Amphiphilic asymmetric comb-like copolymers (AACCs) exhibit distinct self-assembly behaviours due to their unique architecture. However, the synthetic difficulties of well-defined AACCs have prohibited a systematic understanding of the architecture-morphology relationship. In this work, we conducted dissipative particle dynamics simulations to investigate the self-assembly behaviours of AACCs with responsive rigid side chains in selective solvents. The effects of side chain length, number of branches, and spacers on the morphology of aggregates were investigated by mapping out morphology diagrams. Besides, the numbers and surface areas of aggregates clearly depicted the morphological transitions during the self-assembly process. Moreover, the rod-to-coil conformation transitions were simulated to explore the stimuli-responsive behaviour of the AACCs with responsive rigid side chains by adjusting the bond angle parameter of the rigid chains. The results indicated that without the support of the rigid chains, the assembly structure collapsed, leading to the tube-to-channelized micelles and one-compartment-to-multicompartment vesicle morphology transformations. The simulation results are consistent with earlier experimental results, which can provide theoretical guidance for assembly toward desired nanostructures.

Effect of pH on the incorporation of acrylic acid units in the core of polymer nanoparticles prepared by PISA and on their morphology

The molar fraction and ionization of acrylic acid (αAA) in the monomer feed affect the chemical composition, the composition profile and the particle morphology in PISA.

Optimization of power, duration, and water in solanesol extraction from virginia nicotiana tabacum l. leaves assisted by microwave-ultrasound using response surface methodology

Solanesol is an aliphatic terpene alcohol composed of nine isoprene units with many bioactive benefits and is commonly found in Solanaceae, including tobacco. Solanesol is difficult to synthesize artificially; Therefore, acquisition still relies on extraction. Extraction methods such as microwave-assisted extraction (MAE) and ultrasound-assisted extraction (UAE) have reduced extraction time and solvent consumption. Some variables that influence extraction performance in MAE are solvent selection, extraction time, microwave power, and sample-to-solvent ratio (S/F). This research aims to find the optimum parameters for the extraction of solanesol from Virginia variety tobacco leaves using the response surface methodology approach. This study considered the extraction time (30, 60, and 90 seconds), sample-to-water ratio (S/F) (1:1, 1:3, and 1:6), and microwave power (200, 400, and 600 W) were optimized. Solanesol from the extraction was quantified using high-performance liquid chromatography (HPLC), and the yield response was then processed using Design Expert to obtain optimum variables of MAE. This study shows that the optimum condition for the MAE process was 10 mL of water, with a power of 324.581 W for 30 seconds and a predicted solanesol yield of 2.926%.

Optical tracking of the heterogeneous solvent diffusion dynamics and swelling kinetics of single polymer microspheres.

The diffusion dynamics of small molecules into polymer entities is crucial for driving their morphology and function, which can be applied to research fields such as optical identification, medical implantation and intelligent sensing platforms. Herein, we demonstrate a nondestructive bright-field imaging strategy to monitor and control the morphology of polymer microspheres by varying the interfacial interaction and diffusion in a penetrant bath. The nanoscale interface movement of single polymer microspheres was tracked and converted into the diameter variation during the swelling event with sub-pixel accuracy, which is consistent with the calculation using Li-Tanaka's kinetic equations. More interestingly, the solvent diffusion dynamics along different directions of one particle are heterogeneous, indicating the non-uniform internal structure of a soft confined assembly. The swelling characteristics of single polymer microspheres can be quantified by this simple imaging strategy, and the transient intermediate swelling states are captured. To model the lifetime and stabilization times of microplastic entities, solvent selectivity and thermodynamic regulation were introduced to obtain the activation energy down to the single micro-entity level. This optical methodology shows capability for decoding the complex diffusion mechanism in polymer entities and provides guidance for the design of drug delivery systems, sensor platforms, and optical responsive materials.

Optimizing synthesis and applications of sodium valproate: Towards efficiency, affordability, and sustainability

This study reviews the synthesis, optimization, and potential applications of sodium valproate, a key pharmaceutical agent in the treatment of neurological disorders such as epilepsy, bipolar disorder, and depression. The primary focus is on refining the synthesis process of sodium valproate to enhance production efficiency, reduce costs, and increase the accessibility of this crucial medication. By exploring various synthetic routes and optimizing reaction conditions—such as temperature, pressure, and solvent selection. The study aims to develop a more efficient and cost-effective manufacturing process. Special attention is given to the environmental impacts of the synthesis methods, seeking to establish greener and more sustainable practices. The study also discusses advancements in drug formulations, including the development of new therapeutic indications and combination therapies that could potentially improve patient outcomes. Future research directions include optimizing sodium valproate’s molecular structure, investigating its use in personalized medicine, and minimizing its side effects. Through meticulous analysis and innovative approaches, this research contributes to the ongoing development of sodium valproate, ensuring its efficacy, safety, and environmental sustainability in pharmaceutical production.

Optimizing the Extraction Efficiency of Flaxseed Gum Using a Response Surface Methodology Approach.

The extraction of gum from natural raw materials is of increasing importance in various industries, including food, pharmaceuticals, and cosmetics, particularly due to their emulsifying properties and potential applications as stabilizers and thickeners. This study presents an insight on the influence of changing parameters like reagents and operating condition on yield and some properties of the flax (Linum usitatissimum L.) seed gum. The extraction conditions were meticulously examined using a full factorial design, highlighting the significant impact of pretreatment, seed preparation, and solvent selection on the extraction yield. A response surface methodology (RSM) was then applied to optimize the water/benzoic acid ratio of the pretreatment step, the ethyl alcohol/water ratio, and the medium pH of the extraction method, resulting in a maximum yield of 14.47%. Furthermore, detailed analyses of the chemical and emulsifying properties of the gum were conducted showing emulsifying capacities over 94%, offering promising application prospects, particularly in the food industry.

Технология производства защитных антикоррозионных материалов из жиросодержащих отходов

The processing of fat-containing waste from meat-packing enterprises that cannot be landfilled is an urgent problem. The authors developed the technology of processing fat-containing waste in a chemical reactor in one step, without dividing the technology into two steps: triglyceride hydrolysis and fatty acid amide production. The technology for processing fat-containing waste was tested in a laboratory plant. The target product obtained was analyzed using IR spectroscopy. As a result, the structural formula was clarified, functional groups were determined, and chemical intermediates in the synthesis process were identified. The proportions of the reagents were determined: technical fat in the amount of 65.3‑72.4 wt%, monoethanolamine - 14.5‑17.0 wt% and boric acid - up to 100 wt% of the mixture. The reaction time was 1.5 h. The protective effect was selected as a quality control indicator of the surfactant obtained. Solvent selection was carried out for producing anticorrosive materials. I‑20 industrial oil, diesel fuel and SN‑150 oil were selected as solvents. Electrochemical studies carried out on the AVTOLAB PGSTAT302N potentiostat-galvanostat made it possible to determine the mechanism of action of the surfactant as a corrosion inhibitor. Its optimum concentration was found to be 15%, with a protective efficiency of 99.33%. To increase the protective anticorrosive efficiency of the surfactant, the tests were carried out in a humidity chamber for 60 days on St3 steel plates. The test results showed high efficiency of the surfactant used as a corrosion inhibitor, with the Z value of more than 90%.

Separation and Purification Residual Salt from Glycerine Pitch from Waste of Refined Glycerine Production

The glycerol refining process produces 5%wt/ton waste in the form of glycerine pitch (GP) and has the potential to pollute the environment if not properly handled and expensive handling costs. In this study, GP was characterized by its chemical composition and spectroscopic analysis using FTIR and UV-Vis. The sodium chloride content of 15-30% contained in GP was separated and purified by solid-liquid extraction. Solvent selection (methanol, ethanol and acetone), solvent ratio (1:3, 1:5 and 1:10) and extraction time (10, 15 and 30 min) were evaluated using one factor at the time (OFAT) method. The methanol was found to be the optimum solvent and the best ratio at 1:5 produced sodium chloride purity around 81%. However, the effect of extraction time was declared not significant with a pvalue above 0.05. The TOC result of residual salt was 44 ppm and residual methanol content was not detected after heating. The integrated process of separation and purification of residual salt from GP is easy to apply and zerowaste potential in organic waste after extraction can be achieve by combustion in boiler with a calorific value obtained of 3000-3200 cal/g.

A solvent-selection strategy for the hydrogenation reaction inside a tubular-flow reactor through a statistical approach

Solvent selection is crucial for optimizing reaction outcomes of various reactions.

Solvent selection based on a conceptual process design by combining cost evaluation and life cycle assessments for developing new reaction pathways

Solvent selection combined with conceptual process design is the key to developing sustainable chemical production.

Ultrasound-assisted nucleation and growth of hydroxyl-protected and ligand-free Cs3Cu2X5 nanocrystals with bright luminescence.

The commercial applications of lead halide perovskites are hindered by their negative environmental impact and inherent instability. Consequently, developing environmentally friendly copper-based perovskite materials is crucial for future solid-state lighting and display applications. In this study, an ultrafast high-power ultrasonic synthesis strategy was utilized to achieve uniform nucleation and growth of Cs3Cu2X5 (X = Cl, Br, I) nanocrystals (NCs) that possess remarkable luminescence properties, hydroxyl protection, and ligand-free characteristics. These Cs3Cu2X5 NCs exhibited a tunable spectral range spanning from 446 to 525 nm, accompanied by photoluminescence quantum yields (PLQYs) varying from 0.2% to 79.2%. The spectral attributes of the NCs were effectively controlled by modulating the halide type and composition. It is worth noting that density functional theory (DFT) calculations offer valuable insights into the synthesis of NCs and the selection of suitable alcohol solvents. Moreover, we successfully fabricated an efficient and stable white light-emitting diode (WLED) with a high luminous efficiency of 23 lm W-1 and CIE color coordinates of (0.3266, 0.3487). Our work provides a new strategy to synthesize Cs3Cu2X5 NCs and holds promise for their potential application in display and lighting devices.

Optimization of Phenolic in Extraction Kasturi Mango Leaves (Mangifera casturi Kosterm.) with Taguchi Method

Kasturi mango (Mangifera casturi Kosterm.) is one of specific germplasm in South Kalimantan which in the category threatened with extinction. This plant has active metabolites such as phenolic groups which potentially to be bioactive. The active substance in the extract is usually obtained using the extraction method. Extraction is a method widely applied to the separation of compounds from plants to be used as raw materials products. Selection of the appropriate solvent and method is important to get optimal compound. The purpose of this study was to optimize phenolic extraction from Kasturi mango leaves using Taguchi method. The research method used consisted of 9 treatments with factors of temperature, time, and ethanol concentration. The extraction process was carried out on wet and dry samples of Kasturi mango leaves using digestion method with 50% ethanol at 50 ºC for 60 minutes. The result of determining the optimal solid solvent ratio (SSR) was get on dry samples with SSR ratio 1:5 and phenolic content 16995.8 mg/L. For the results of optimization phenolic extraction of dry samples Kasturi mango leaves with Taguchi method, the highest phenolic content obtained was 19407.8 mg/L with use of 30% ethanol at 70 ºC for 60 minutes.

Morphology optimization via pre-aggregation and miscibility matching in PM6:L8-BO ternary organic solar cells.

To elucidate the mechanism by which pre-aggregation and miscibility matching govern the active layer morphology in non-fullerene organic solar cells, chloroform (CF) and o-xylene (OX) were used as solvents, while D18 and N2200 were incorporated as third components into the PM6:L8-BO system. The incorporation of D18 enhanced device performance, whereas the addition of N2200 reduced device performance. Based on surface energy analysis, the free energies of pure components and binary blends in different solvents were calculated, showing that the Gibbs free energies of D18, PM6 and L8-BO exhibited better pre-aggregation matching. Employing the melting point depression method, the Flory-Huggins interaction parameters of D18 : L8-BO (1 : 6) and N2200 : L8-BO (1 : 5) blends were calculated. The results revealed that the miscibility of the samples cast with CF was superior to those cast with OX. Atomic force microscopy (AFM) and transmission electron microscopy (TEM) observations revealed that D18 could induce L8-BO to aggregate and crystallize to form a nanofiber architecture, leading to an optimized phase separation. Attributing to the desirable miscibility of D18 with L8-BO, the D18:L8-BO nanostructures could be dispersed within an amorphous PM6 matrix, forming a double-fibril network morphology that facilitated charge transfer and enhanced device performance. In contrast, N2200 was immiscible with L8-BO, which led to the formation of a suboptimal morphology exhibiting excessive aggregation or excessive dispersion, resulting in a deterioration in charge transfer and device performance. The investigation of pre-aggregation matching in solvents, and miscibility matching of the components could provide guidance for the rational selection of appropriate solvents and suitable third components towards high-performance ternary organic solar cells.