Effective Solvent System Research Articles

Method development and validation for the extraction and quantification of sesquiterpene lactones in Dolomiaea costus

Dolomiaea costus, commonly known as Indian costus, is a medicinal plant from the Asteraceae family. The root and powder of costus have been widely used to treat various health conditions. The primary bioactive compounds in this plant are sesquiterpene lactones, particularly costunolide and dehydrocostus lactone. This study aimed to establish a rapid, environmentally friendly, and cost-effective method for the high-throughput extraction and quantification of sesquiterpene lactones in Indian costus. Ultrasonic bath (UB) and UPLC/MS-MS were employed to extract and analyse 49 Indian costus samples. Aqueous ethanol was identified as the most effective solvent system for extracting and analysing sesquiterpene lactones. The extraction efficiency of the ultrasonic bath was comparable to that of the ultrasonic homogeniser while shaking showed the lowest efficiency. The environmentally friendly UPLC/MS-MS analysis revealed mean concentrations (±SD; μg/100 μg) of 1.00 (±0.39) for costunolide and 0.70 (±0.25) for dehydrocostus lactone. An inverse correlation was observed between sesquiterpene lactone content and sample colour. Most samples contained costunolide levels above the minimum limit (0.6 %) specified by the Chinese monograph, but only a few met the 1.8 % threshold for total sesquiterpene lactones. Given the importance of bioactive sesquiterpene lactones for medicinal efficacy, insufficient levels may result in diminished therapeutic value. Therefore, standardising Indian costus products is crucial to ensure quality and appropriate dosing. This study contributes to the standardisation of Indian costus, a vital step towards ensuring the efficacy and safety of herbal products.

Environmentally Friendly Leaching of Antimony from Mining Residues Using Deep Eutectic Solvents: Optimization and Sustainable Extraction Strategies

This paper focuses on the environmental leaching of antimony, a critical mineral, using deep eutectic solvents. Mining residues often contain embedded antimony, posing environmental risks. Deep eutectic solvents, known for being low in toxicity, cost-effective, and environmentally friendly, present a promising avenue for sustainable antimony extraction. The study focuses on optimizing the leaching process through experimental analysis by considering variables such as temperature, time, and percentage of solids. Different deep eutectic solvent (DES) compositions are being studied, including choline chloride with malonic acid, thiourea, and ethylene glycol in different molar ratios, to identify the most effective solvent system for antimony extraction. A sample, originally obtained from mining waste produced via the flotation of antimonite ore, was used to test these three types of DESs. By optimizing the leaching process by changing the ratio of solid and liquid components, as well as the amount of oxidizing agent up to 3 g, iodine, yields of up to 100% were achieved after leaching for 4 h at 100 °C. The aim of the study is to advance sustainable resource management by providing knowledge on an ecological and feasible method of extracting antimony from mine waste, leading to more conscious and efficient resource practices in the mining sector.

Investigation of Rational Design of Amine Solvents for CO2 Capture: A Computational Approach

Solvent selection and design are critical in the CO2 capture process as the choice of solvent directly impacts the cost of the process, capture efficiency, equipment size, and regeneration energy. In the present study, 1MPZ-PZ, PZ, PIP, DEEA and MEA-DEEA are analyzed in terms of interaction intensity (attractive and repulsive) and diffusivity by molecular dynamic simulation. A high intermolecular interaction intensity promotes CO2 absorption, while intra-molecular interaction intensity affects CO2 desorption during the regeneration process. Diffusivity is also an important factor for a fast CO2 uptake rate, which is desirable for efficient CO2 capture. The interpretation of diffusivity and intermolecular interaction intensity findings is conducted through mean square displacement and radial distribution function analysis, respectively. The order of interaction intensity in various amines is DEEA>MEA-DEEA>PIP>1MPZ-PZ. It shows that DEEA can increase the CO2 absorption rate as it shows the highest interaction intensity in pure and blended amine systems. The results of the intramolecular interaction intensity show that it is easier to regenerate DEEA, PIP, PZ, and 1MPZ than MEA. The temperature effect on the interaction intensity is revealed at higher temperatures, where the molecular structure becomes unstable due to higher thermal motion, which is the cause of lower interaction intensity. On the other hand, the mean square displacement analysis for the diffusivity rate shows that PZ shows the highest diffusivity rate compared to other selected solvents. The order of diffusivity rate in various pure and blended amine systems is PZ>PIP>1-MPZ-PZ>MEA-DEEA. The diffusivity of various amine solvent systems increases with temperature. As examined in this current research, assessing solvent characteristics holds significant importance in optimizing the most effective solvent system.

Quantitative Determination and Source Variation of Rutin in Fagopyrum Tataricum

Buckwheat (Fagopyrum sp.) is a traditional crop of Uttarakhand (India) known for its high Rutin content, a bioflavonoid with significant medicinal properties. This study explores the quantitative measurement of Rutin in various buckwheat varieties grown in different regions of Uttarakhand using Thin Layer Chromatography (TLC) and High-Performance Thin Layer Chromatography (HPTLC). Twelve seed sources of Fagopyrum tataricum from the Garhwal and Kumaon regions, along with Fagopyrum esculentum seeds for comparison, were collected. Preliminary phytochemical screening of the extracts revealed the presence of flavonoids, alkaloids, tannins, and carbohydrates, with methanolic extracts showing higher concentrations. TLC analysis was employed to determine the most effective solvent system for Rutin separation, leading to the identification of three samples with substantial Rutin content. HPTLC was then used for quantitative Rutin assessment, with a calibration curve established using standard Rutin solutions. The three selected samples, along with the standard, were applied to HPTLC plates, and the Rutin content was measured based on peak areas and peak heights. The sample collected from Joshimath, Uttarakhand, known as "JOG," exhibited the highest Rutin content. This study provides valuable insights into the phytochemical composition of buckwheat varieties in Uttarakhand, which can inform the development of high-quality functional foods. Rutin, a potent antioxidant with various health benefits, underscores the significance of buckwheat as a naturally occurring functional food source. The results contribute to understanding the Rutin-rich potential of buckwheat grown in Uttarakhand and its applications in functional foods and nutraceuticals. Further research in this field can promote the cultivation and utilization of buckwheat as a source of this valuable bioactive compound with numerous health benefits.

Exploring biotechnological approaches on in vitro callus induction and evaluation of biomedicinal properties of Cleome gynandra L.

In the present study, indirect organogenesis method was adopted for the production of callus from stem and leaf explants of Cleome gynandra using MS media. Production of callus using stem and leaf explants revealed that the highest dry biomass was achieved with the addition of IBA and 2,4-D in MS medium resulting in values of 180.33 and 190 mg, respectively. Antibacterial study inferred that methanol extract of C. gynandra callus exerted significantly pronounced inhibitory zones (8–16 mm) with minimal bacteriostatic (50–125 µg ml−1) and bactericidal (75–150 µg ml−1). Biofilm inhibitory activity revealed that callus extract surpassed leaf extract and showed > 80% biofilm inhibition, as confirmed by microscopic analysis. The callus extract also exhibited a relatively higher total phenolic content, while the leaf extract showed stronger antioxidant activity. Haemolysis analysis indicated that it was comparatively lower in callus extract and thus substantiating its biocompatibility. Phytochemical profile showed a meagre difference between the extracts. Cytotoxicity of the callus extracts against Artemia nauplii registered LC50 value of 53.71 µg ml−1. Partial purification and TLC bioautography evidenced Methanol: Acetone: Petroleum ether (8:1:1) as the most effective solvent system against the bacterial pathogens. GC-MS analysis substantiated benzofuran, sesquiterpenoids, fatty acids, diterpenes, hydrocarbons and alkanes as the major chemical constituents.

Formation and characterisation of biobased poly(butylene succinate) electrospun nanofibre scaffolds

This study demonstrates the fabrication of nonwoven nano and micro fibrous mats of biobased poly(butylene succinate) (PBS) by an electrohydrodynamic processing (electrospinning). The effects of polymer concentration applied electric field, solvent system on the morphology of the scaffolds were investigated. Optimal conditions for a stable electrospinning process were identified, with an effective solvent system chloroform/formic acid providing improved solubility and facilitating the production of uniform nano-sized fibres. A variety of fibrous morphologies was obtained, ranging from 0.17 µm to 4.54 µm in fibre diameter and 1.12–13.52 µm in pore diameter. It was found that co-solvent addition significantly affects solution properties and resultant fibre and pore sizes, while the intensity of the electric field appeared to play a less significant role due to the predominance of solution properties. Electrospinning did not alter chemical and thermal properties of PBS, but electrospinning and co-solvent presence reduced the polymer's crystallinity. These insights enhance our understanding of biobased PBS electrospinning and could potentially extend the range of applications for these fibres towards a more sustainable sector of polymer nonwovens, replacing the dependency from petroleum-based compounds.

Best effective solvent system for analysis of cosmetic products

In the past four decades, many articles have been published on the forensic examination of cosmetics, with ongoing efforts to develop newer solvent systems for HPLC and TLC evaluation. This experimental study aims to identify the best solvent system for the identification of facial cream evidence, which saves time, costs, and laborious work for forensic examiners, and to seek fast-tracking justice. The study focuses on determining the optimal solvent system for analyzing face creams (cosmetics) using TLC. Various cosmetic products, including Ponds Cream, Nivea, Garnier, and Lakme CC Cream, were collected from Indore for analysis. This experimental research is relevant to forensic science as it may help identify face creams found at crime scenes or on suspects or victims. Thus, it is crucial to identify all items, including face creams, at a crime scene to aid in criminal investigations. Out of five solvent systems, Toluene: Acetone: Benzene (9:1:1) and Toluene: Acetone produces effective and clear results with all four facial creams in TLC.

Lignocellulose hydrogels fabricated from corncob residues through a green solvent system

It is still a challenge to find an effective solvent system that can simultaneously dissolve the cellulose and lignin in biomass residues to fabricate lignocellulose hydrogels (LHs). Herein, corncob residues from furfural production were pretreated with alkaline peroxide to regulate the lignin content. The lignin/cellulose composites with various lignin content were then dissolved and regenerated by a green and facile ZnCl2/CaCl2 solvent system. The inorganic salt solvents were served as linkers and flexible LHs were obtained. Substrate material containing 10.75% lignin shows the best compressive stress (76.71 kPa). Inspired by its superior ionic conductivity, the hydrogels were assembled into a solid-state electrolyte for a zinc-ion hybrid supercapacitor. This research develops a feasible, simple, and low-cost route for lignin-containing hydrogel preparation and offers insights into the high-value application of agro-industrial lignocellulosic wastes.

Phytochemical screening and TLC fingerprinting of selected medicinal plant used for antilithiatic activity

The purpose of this study to investigate phytochemical screening and TLC fingerprinting of selected medicinal plant used for antilithiatic activity. Phytochemical tests were performed on plant extracts to determine the presence of several chemical elements such as Glycoside, Terpenoid, Flavonoids, Tannins, and other compounds that are responsible for the biological activity of the plant extract. To that end, ethanolic extracts of Nyctanthes arbor-tristis Linn. leaves are used for the chemical assays to be conducted primarily for the identification of various chemical components The most effective solvent system for TLC of Nyctanthes arbor-tristis Linn. leaves was discovered. Chloroform, benzene, and formic acid are all components of the ethanolic extract (50:40:10). Nyctanthes arbor-tristis Linn. leaves have received some TLC. In the presence of six different compounds with various Rf values in different colours, employing the iodine vapour as a detecting reagent, the ethanolic extract shows the presence of six compounds in the extract with different Rf values in different colours.

New insight and evaluation of secondary Amine/N-butanol biphasic solutions for CO2 Capture: Equilibrium Solubility, phase separation Behavior, absorption Rate, desorption Rate, energy consumption and ion species

• MAE + n-butanol + H 2 O system for CO 2 capture was first proposed. • The phase change mechanism and energy consumption of the system were investigated. • The influence of temperature on absorption capacity was explored. • The developed biphasic absorbent has excellent energy saving advantages. Effective phase-change solvent system, n-methyl-2-hydroxyethylamine (MAE) + water-insoluble alcohol + H 2 O, was developed for CO 2 capture. First, a preliminary screening of several alcohols was carried out and showed that the MAE/n-butanol/water system had the potential to become an excellent phase change absorbent. Then, through phase change experiment, absorption experiment, desorption experiment, and theoretical energy consumption analysis, the MAE:n-butanol:water ratio of 3:4:3 possessed the most impressive CO 2 capture performance. Theoretical calculation of CO 2 desorption energy consumption showed that in comparison with 30 wt% monoethanolamine (MEA), 50% of reboiler heat duty can be reduced in case of the 3:4:3 system. In addition, equilibrium phase diagram of the three components showed that concentration of n-butanol significantly affected the phase separation. The two-phase species distribution after phase separation was determined using Nuclear magnetic resonance spectroscopy (NMR). This work also shows that temperature has influence on absorption and desorption performance. Finally, the absorbent stability test during absorption–desorption process confirmed that MAE/n-butanol/water absorbent had a great potential for capturing CO 2 .

Carbon Dioxide Mediated Cellulose Dissolution and Derivatization to Cellulose Carbonates in a Low-pressure System

An effective switchable solvent system using carbon dioxide (CO2) and 2-tert-butyl-1,1,3,3-tetramethylguanidine (BTMG) for cellulose dissolution and derivatization was developed. High concentration cellulose solution (up to 10 wt%) could be achieved by dissolving microcrystalline cellulose rapidly, within 5 min, into DMSO in presence of BTMG and 1 atm CO2 at room temperature. The cellulose-carbonate anion intermediate was characterized by 1H and 13C NMR spectroscopies, emphasizing the generation of cellulose carbonate anions and protonated BTMG. Addition of organochlorides into the cellulose solution triggers a nucleophilic substitution with cellulose-carbonate anions, producing various cellulose benzyl carbonates and a cellulose-carbonate-ester with degree of substitution (DS) up to 1.83 at 1 atm CO2 pressure and room temperature. The activation energy (Ea) and Gibbs free energy change (ΔG) of CO2-mediated dissolution and nucleophilic substitution were calculated by density functional theory. The results showed that the nucleophilic substitution is the rate-limiting step.

γ‐Valerolactone: A Nontoxic Green Solvent for Highly Stable Printed Mesoporous Perovskite Solar Cells

Mesoscopic carbon‐based lead halide perovskite solar cells (CPSCs) represent a promising architecture for commercialization in the field of perovskite photovoltaics as they are stable, potentially low cost, and use easily scaled production methods. However, the use of toxic and psychoactive solvents such as dimethylformamide (DMF) and γ‐butyrolactone (GBL) currently limits their commercial viability: DMF introduces a significant health risk and GBL is subject to legal restrictions in many countries. The development of safe and effective solvent systems is therefore an essential step toward commercial viability. Herein, γ‐valerolactone (GVL) is presented as a nontoxic, biodegradable, green alternative to GBL for CPSC fabrication. Cells fabricated with a precursor concentration of 1.1 m and annealed at 45 °C exhibit comparable performance to standard GBL devices, achieving a champion power conversion efficiency (PCE) of 12.91% in a device of 1 cm2 active area. Herein, it is proven that GVL is a viable alternative to GBL for CPSCs and enables research in countries where GBL is legally restricted and makes large‐scale CPSC manufacture more sustainable.

Effective solvent system selection in the recrystallization purification of pharmaceutical products

AbstractThis treatment describes the details of a methodical three step algorithm for determining the best operating conditions for the recrystallization separations of solid mixtures for the chosen targeted solvent systems. Our algorithm was applied to effectively separate a representative pharmaceutical product (caffeine) from a related pharmaceutical product (theophylline). The limitations of such calculations with currently available, widely used predictive methods for computing solution thermodynamics without experimental data are directly examined. Also presented here is a novel two stage recrystallization procedure which can potentially dramatically improve the overall recovery yields of the desired products. These systematic selection calculations described herein should enable researchers to quickly screen many potential solvent systems and operating conditions and concentrate experimental efforts only on the most promising candidates for such purifications.

Asymmetric diglycolamide in BmimNTf2 as an effective solvent system for the uranyl extraction

The extraction behavior of uranyl from the nitric acid medium using an asymmetric diglycolamide, DMDODGA, in BmimNTf2 was studied. The effects of the concentration of HNO3, DMDODGA and temperature on the distribution ratio were discussed. The distribution ratio of uranyl into BmimNTf2 liquid is much higher than that into hydrocarbon diluents. The extraction mechanism was investigated by UV-visible spectroscopic and extraction experiments that all agree the cation-exchange mechanism. Formation of the 1:2 U/DMDODGA complexes was analyzed using the slope analysis method. In addition, uranyl can be effectively separated from perrhenate using DMDODGA-BmimNTf2 system.

Extraction of bioactive compounds from Catharanthus roseus and Vinca minor

The aim of this study was to extract and identify the major constituents, namely, the indole alkaloids, from two Apocynaceae medicinal plant family species, Catharanthus roseus and Vinca minor when using different solvents (the alcohol mixtures, the imidazolium-based ionic liquids (IL) and the novel choline- and menthol-based deep eutectic solvents (DESs)) in ultrasound-assisted processes. Special analytical protocols were developed for the analyses of the IL and DES extracts by liquid chromatography, as these solvents are generally regarded as interfering additives in liquid separation methods. The developed procedures enabled the study to detect and to compare the abundance of several alkaloids in these plants. The different solvents demonstrated varying extraction yields for the analysed alkaloids. In C. roseus, the concentrations ranged from 60.2–329.9 and 114.8–659.7 µg g−1 for catharanthine and vindoline, respectively. In the case of V. minor, the concentrations of vincamine ranged from 6.0–173.9 µg g−1. The obtained results have clearly shown the different extraction abilities of the used solvents for the separate classes of compounds. Therefore, there is a flexibility to select an effective solvent system for the specific extractions and separations of these compounds.

Comparative antioxidant and antimicrobial potentials of leaf successive extract fractions of poison bulb, Crinum asiaticum L.

Crinum asiaticum L. (family: Amaryllidaceae) is a widely used medicinal plant species having great ethnomedicinal values. The present study aimed to evaluate in vitro antioxidant and antimicrobial potentials of the leaf extracts of C. asiaticum with their phenolics content. The total antioxidant assay, 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging activity, and ferric ion reducing antioxidant power (FRAP) assays of the leaf crude aqueous extract and the five successive extract fractions were analyzed to evaluate their antioxidant potential. The antimicrobial potential was investigated against two gram-negative and one gram-positive bacteria strain by the disc diffusion method. The aqueous fraction of C. asiaticum (CaAq) showed relatively higher antimicrobial potentials than the crude aqueous extract (CaLAE), in terms of zone of inhibition, indicating the fact that serial extraction procedure can more successfully concentrate the specific bioactive components. Along with CaAq and CaLAE, CaEA fraction (ethyl acetate extract fraction) also exhibits antimicrobial activities probably due to the presence of terpenoids, phenolics, and flavonoids. It might be concluded that antioxidants and antimicrobial agents are available in the leaves of C. asiaticum where water and ethyl acetate might be the effective solvent systems to extract antimicrobial and antioxidant agents respectively.

The Roles of H2O/Tetrahydrofuran System in Lignocellulose Valorization.

Lignocellulosic biomass as a potential alternative to fossil resource for the production of valuable chemicals and fuels has attracted substantial attention, while reducing the recalcitrance of lignocellulosic biomass is still challenging due to the complex and cross-linking structure of biomass. Solvent system plays important roles in the pretreatment of lignocellulose, enabling the transformation of solid biomass to liquid fluid with better mass and heat transfer, as well as in the selective formation of target products. In particular, H2O/tetrahydrofuran (H2O/THF) system has recently been widely applied in lignocellulose valorization, which has been proved to exhibit outstanding efficiency for the conversion of lignocellulose, solubilization of the intermediates and products, and shifting reaction equilibrium, thereby significantly improving the yield and selectivity of target products, as well as the full utilization of lignocellulose. In addition, THF shows low toxicity, and is known as a renewable solvent which can be produced from bio-derived chemicals. Herein, this review concentrates on the advances of H2O/THF system in lignocellulose valorization in recent years. Several aspects relative to the roles of H2O/THF system are discussed as follows: the pretreatment of lignin, conversion of hemicellulose and cellulose components in lignocelluloses, and the promoting formation of valuable chemicals like furfural, 5-hydroxymethyl furfural (HMF), levulinic acid, and so on, as well as the inhibiting role in humins formation. This review might provide useful information for the design of effective solvent system in full utilization of lignocellulosic biomass.

Solvent Effects on Degradative Condensation Side Reactions of Fructose in Its Initial Conversion to 5-Hydroxymethylfurfural.

The degradative condensation of hexose, which originates from the C-C cleavage of hexose and condensation of degraded hexose fragment, is one of the possible reaction pathways for the formation of humins in hexose dehydration to 5-hydroxymethylfurfural (HMF). Herein, the impacts of several polar aprotic solvents on the degradative condensation of fructose to small-molecule carboxylic acids and oligomers (possible precursors of humins) are reported. In particular, a close relationship between the tautomeric distribution of fructose in solvents and the mechanism of degradative condensation is demonstrated. Typically, α-fructofuranose in 1,4-dioxane and acyclic open-chain fructose in THF favor the conversion of fructose to formic acid and oligomers; α-fructopyranose in γ-valerolactone or N-methylpyrrolidone favors levulinic acid and oligomers, whereas β-fructopyranose in 4-methyl-2-pentanone favors acetic acid and corresponding oligomers. This close correlation highlights a general understanding of the solvent-controlled formation of oligomers, which represents an important step toward the rational design of effective solvent systems for HMF production.

One-pot selective conversion of lignocellulosic biomass into furfural and co-products using aqueous choline chloride/methyl isobutyl ketone biphasic solvent system

This study investigated simultaneous lignocellulose fractionation and conversion in a one-pot reaction using an aqueous choline chloride/methyl isobutyl ketone (ChCl/MIBK) biphasic solvent system. Under the optimized condition (170 °C, 60 min, 0.6 wt% H2SO4, 10.7 wt% solid loading), the biphasic solvent solubilized 96% xylan in raw switchgrass, which was simultaneously converted to furfural with a yield of 84.04%. The biphasic solvent was also able to selectively extract lignin, which had a high purity (93.1%), and uncondensed moieties (i.e., Hibbert’s ketone), as well as decreased molecular weight and polydispersity index. The resultant pulp was enriched with cellulose (73.3%), which can be completely hydrolyzed into glucose within 48 h via enzymatic hydrolysis. Aqueous ChCl was successfully recycled and reused for atleast three cycles with similar performance in switchgrass fractionation. This study demonstrated that aqueous ChCl/MIBK biphasic system was an effective solvent system for co-production of furfural, high quality technical lignin and digestible cellulose for further upgrading.

Dissolution and transesterification of cellulose in γ-valerolactone promoted by ionic liquids

Ionic liquids act as promoters for the dissolution of cellulose in GVL and also as catalysts for cellulose derivatization in GVL, providing a green and effective solvent system for cellulose processing and derivatization.