Simple Solvent Extraction Research Articles

One-Pot Electrosynthesis of Gamma-Butyrolactone (GBL) from Furoic Acid

The catalytic valorization of biomass to afford synthetically useful small molecules is essential for sustainable biorefinery processes. Herein, we present a mild cascaded electrochemical protocol for converting furoic acid (FA), a common biomass-derived feedstock, into a versatile platform chemical, gamma-butyrolactone (GBL). All involved species participate in the desired redox pathway with high selectivity: FA was electrochemically oxidized with 84.2% selectivity to 2(5H)-furanone (2-FO), the olefin of which was then hydrogenated to yield GBL with 98.5% selectivity. We identified that a certain temperature is an important factor in enabling the one-pot reaction as it promotes thermal desorption of the key intermediate. The reaction was scalable to gram-scale, producing high-purity GBL isolated through a simple solvent extraction from a 500-mL electrolysis scale reaction.

One-Pot Electrosynthesis of Gamma-Butyrolactone (GBL) from Biomass-Derived Furoic Acid

An efficient catalytic method to transform biomass into value-added products is critical to promoting a sustainable future. Ideally, such a transformation should be carried out efficiently in mild conditions. Herein, we developed a mild one-pot electrochemical protocol for converting furoic acid (FA), a common biomass-derived feedstock, into a versatile platform chemical, gamma-butyrolactone (GBL). All involved species participate in the desired redox pathway with high selectivity: FA was electrochemically oxidized with 84.2% selectivity to 2(5H)-furanone, the olefin of which was then hydrogenated to yield GBL with 98.5% selectivity. We identified that a specific temperature is an essential factor in enabling the one-pot reaction as it promotes thermal desorption of the key intermediate. The reaction was scalable to gram-scale, producing high-purity GBL isolated through a simple solvent extraction from a 500-mL electrolysis scale reaction.

Mechanically Interlocked Water-Soluble Pd6 Host for the Selective Separation of Coal Tar-Based Planar Aromatic Molecules.

Research on the synthesis of catenated cages has been a growing field of interest in the past few years. While multiple types of catenated cages with different structures have been synthesized, the application of such systems has been much less explored. Specifically, the use of catenated cages in the separation of industrially relevant molecules that are present in coal tar has not been explored before. Herein, we demonstrate the use of a newly synthesized interlocked cage 1 [C184H240N76O48Pd6] (M6L4), formed through the self-assembly of ligand L.HNO3 (tris(4-(1H-imidazole-1-yl)benzylidene)hydrazine-1-carbohydrazonhydrazide) with acceptor cis-[(tmchda)Pd(NO3)2] [tmchda = ±N,N,N',N'-tetramethylcyclohexane-1,2-diamine] (M). The interlocked cage 1 was able to separate the isomers (anthracene and phenanthrene) using a simple solvent extraction technique. Using the same technique, the much more difficult separation of structurally and physiochemically similar compounds acenaphthene and acenaphthylene was performed for the first time with 1 as the host. Other noninterlocked hexanuclear Pd6 cages having a wider cavity proved inefficient for such separation, demonstrating the uniqueness of the interlocked cage 1 for such challenging separation.

Flexible Wood‐Based X‐Ray Scintillator Film Using Lead‐Free Cs3Cu2I5 Perovskite Nanoparticles

The prevalent use of unsustainable polymers in current X‐ray scintillators poses a significant environmental concern. The advancement of biodegradable X‐ray scintillators holds promise in mitigating escalating environmental issues tied to electronic or medical waste and carbon footprints. Herein, a biodegradable and flexible X‐ray scintillation film is presented employing lead‐free 0D Cs3Cu2I5 perovskite nanoparticles integrated into densified‐delignified wood (Cs3Cu2I5@D‐Wood). The Cs3Cu2I5@D‐Wood film demonstrates precise and detailed X‐ray imaging capabilities, achieving a high spatial resolution of 10 line pairs per millimeter (lp·mm−1). To minimize the environmental impact associated with disposal, metal and halide ions (e.g., Cs+, Cu+, I−) from Cs3Cu2I5@D‐Wood can be easily retrieved by a simple solvent extraction process. The approach showcases the potential of biodegradable wood‐based X‐ray scintillation screens as alternatives to conventional, plastic‐based screens. This offers a significant contribution to environmental sustainability by reducing electronic or medical waste.

One-pot redox cascade paired electrosynthesis of gamma-butyrolactone from furoic acid

The catalytic valorisation of biomass to afford synthetically useful small molecules is essential for sustainable biorefinery processes. Herein, we present a mild cascaded electrochemical protocol for converting furoic acid, a common biomass-derived feedstock, into a versatile platform chemical, gamma-butyrolactone. In the platinum(+)|nickel(−) electrode paired undivided cell, furoic acid is electrochemically oxidised with 84.2% selectivity to 2(5H)-furanone, the olefin of which is then hydrogenated to yield gamma-butyrolactone with 98.5% selectivity. The final gamma-butyrolactone yield is 69.1% with 38.3% Faradaic efficiency and 80.1% carbon balance when the reaction is performed with 100 mM furoic acid at 80 °C at +2.0 VAg/AgCl. Mechanistic investigation revealed the critical temperature and electrolyte pH conditions that maximise the production and protection of the key intermediate, furan radical, promoting its transition to 2(5H)-furanone rather than self-polymerising. The reaction is scalable, as 2.1 g of 98.1% pure gamma-butyrolactone is isolated through a simple solvent extraction.

Analysis of iron-rich hydrochloric acid solutions for uranium, thorium, rare-earth elements and other heavy metals

A simple solvent extraction method is described for the separation of trace elements including uranium (U), thorium (Th) and rare-earth elements (REEs) from industrially processed iron-rich hydrochloric acid solutions. Iron (Fe) causes severe spectral interference during the analysis of trace elements using inductively coupled plasma optical emission spectrometer (ICP-OES) and U by light-emitting diode (LED)-based fluorimeter (LEDF). The spectral interferences of Fe on trace elements are studied and documented. Sequential solvent extractions using methyl isobutyl ketone (MIBK) effectively removed the highly interfering Fe from these processed acid solutions, thereby enabling accurate and sensitive determination of Cd, Zn, Pb, Co, Ni, Cr, V, Cu, Sr, Zr, Ti, REEs including radioactive elements like U and Th. Solvent extraction parameters like the number of extractions, aqueous-organic ratio and acidity have been optimized for removal of Fe. The accuracy of the method has been established by analyzing synthetically prepared hydrochloric acid solutions by spiking-recovery method. Ion exchange separation of REEs using Dowex 50 × 8 cation exchange resin has been also studied and reported. The precision obtained has been well within ± 10% RSD for elements having concentration above 10 mg L−1 and ± 15% for elements having concentration below 10 mg L−1 for replicate (n = 5) measurements.

Simplified solvent extraction process for high-purity Ni/Co mixed solution for lithium–ion batteries

ABSTRACT The demands for Ni-based raw materials increase as Ni–Co–Mn ternary cathode materials become the main axis of the battery industry. Conventional hydrometallurgical process to produce raw materials from Ni ore for battery application is as follows: (i) leaching of metal ions by acid, (ii) solvent extraction process to extract target metals, and (iii) crystallization process to produce final single-metal compound as powder products. The conventional solvent extraction process is a three-circuit process comprising impurity removal, Co extraction, and Ni extraction circuits. Unlike conventional process, in this work, we suggest a simplified two-circuit process to simultaneously extract Ni and Co to produce Ni/Co mixed solution for cathode material precursor production. Accordingly, the efficiency of site utilization can be maximized by reducing the investment cost for the manufacturing process and downsizing mixer-settler facilities. Further, eco-friendly effects such as reducing the consumption of titrants and cutting down the process costs and wastewater discharge can be realized.

Simple and fast quantification of cannabinoids in animal feeds by liquid chromatography-tandem mass spectrometry.

There is growing interest in using hemp materials as animal feed ingredients, which may raise safety concerns because of the potential transfer of active cannabinoids to the resultant products of animal origin. Hence, the detection and identification of cannabinoids in feeds would be useful. We developed a simple, fast, and sensitive method for simultaneous quantification of 4 major cannabinoids in animal feeds by liquid chromatography-tandem mass spectrometry (LC-MS/MS). We used a simple solvent extraction and dilution approach to extract cannabinoids from the feed matrix. We validated the method in 2 types of cattle feeds with acceptable intra-day and inter-day accuracy (87.5-116%) and precision (< 15%). The limit of detection was 0.05 µg/g, and the limit of quantification was 0.1 µg/g. Furthermore, the method was able to identify and quantify cannabinoids in cattle feeds mixed with hempseed cake as well as in several different hempseed materials, demonstrating its potential in veterinary laboratory applications.

Novel Liquid Chromatography–Tandem Mass Spectrometry Method for Analysis of 102 Pesticides and Five Mycotoxins Regulated by the State of Colorado in Dried Hemp

A novel liquid chromatography–tandem mass spectrometry (LC–MS/MS) method with a dual electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) source was developed for analyzing 102 pesticides and five mycotoxins that are regulated by the state of Colorado in hemp. The limit of quantitation (LOQ) of the 102 pesticides and five mycotoxins met Colorado state action limit requirements for these analytes in a hemp matrix. For this study, 88 out of 102 pesticides and all five mycotoxins were analyzed using LC–MS/MS with an ESI source, whereas the remaining 14 pesticides were determined using LC–MS/MS with an APCI source. A simple, fast, green, and cheap acetonitrile solvent extraction method was used to extract the pesticides and mycotoxins from the hemp matrix with good extraction efficiency in the range of 80–120%. A hemp matrix is challenging and causes matrix effects such as ion suppression or enhancement. We optimized the LC method and added 30 internal standards to reduce and compensate for these matrix effects to obtain method accuracy in the range of 70–120%. The ionization mechanism of nonpolar pesticides (normally analyzed by gas chromatography–tandem mass spectrometry [GC–MS/MS]) with an APCI ion source was elucidated.

Tunable and functional phosphonium-based deep eutectic solvents for synthesizing of cyclic carbonates from CO2 and epoxides under mild conditions

Carbon dioxide (CO2) conversion into carbonates is one of the important ways to reduce carbon emissions. In this study, several phosphonium-based functional deep eutectic solvents (DESs) were prepared as catalysts for the synthesis of cyclic carbonates under mild conditions. The research showed that under mild conditions (60 °C, 0.8 MPa, 4 h, and 3.5 mol% catalyst loading), 1-ethylamine-3-butylphosphine bromide−diethylene glycol ([P4,4,4,2NH2][Br]-DEG) DES catalyst can achieve 96% propylene carbonate (PC) yield. In addition, the DES catalyst can be recovered by simple solvent extraction, and the PC yield does not decrease significantly after five cycles. Finally, in situ FT-IR and density functional theory (DFT) were used to provide a potential reaction mechanism for the cycloaddition reaction. Mechanism studies show that synergistic catalysis between quaternary phosphine ionic liquids (ILs) and ethylene glycol (EG)/DEG promotes CO2 conversion to cyclic carbonate.

An environment-friendly approach using deep eutectic solvent combined with liquid-liquid microextraction based on solidification of floating organic droplets for simultaneous determination of preservatives in beverages.

With the increase in environmental protection awareness, the development of strategies to reduce the use of organic solvent used during the extraction process has attracted wide attention. A simple and green ultrasound-assisted deep eutectic solvent extraction combined with liquid-liquid microextraction based on solidification of floating organic droplets method was developed and validated for the simultaneous determination of five preservatives (methyl paraben, ethyl paraben, propyl paraben, isopropyl paraben, isobutyl paraben) in beverages. Extraction conditions including the volume of DES, value of pH, and concentration of salt were statistically optimized through response surface methodology using a Box-Behnken design. Complex Green Analytical Procedure Index (ComplexGAPI) was successfully used to estimate the greenness of the developed method and compare with the previous methods. As a result, the established method was linear, precise, and accurate over the range of 0.5-20 μg mL-1. Limits of detection and limits of quantification were in the range of 0.15-0.20 μg mL-1 and 0.40-0.45 μg mL-1, respectively. The recoveries of all five preservatives ranged from 85.96% to 110.25%, with relative standard deviation less than 6.88% (intra-day) and 4.93% (inter-day). The greenness of the present method is significantly better compared with the previous reported methods. Additionally, the proposed method was successfully applied to analysis of preservatives in beverages and is a potentially promising technique for drink matrices.

Study of some alcohol amounts in commercial alcoholic disinfectant solutions using gas chromatography with flame ionization detection

A simple solvent extraction method was used to analyze alcohol-based hand rubs (ABHRs) using gas chromatography with a flame ionization detector. 79 samples including 68 liquid and 11-gelled ABHRs were analyzed in the Food and Drug Laboratories Research Center of Mashhad, Iran. 17 samples had methanol, 50 samples had the correct percentage of alcohol (60-80%), and 12 samples had the incorrect percentage of alcohol (&lt;60%). The RSD% of methanol, ethanol, and isopropanol were as 2.28, 2.18, and 1.52, respectively. The relative recoveries for methanol, ethanol, and isopropanol were 102.5, 97.8, and 114, respectively. All experiments were repeated three times. The limit of detection and the limit of quantification for methanol, ethanol, and isopropanol were obtained as 0.22, 0.24, 0.10 (%) and 0.71, 0.82, 0.68 (%), respectively.

Analysis of Near 400 Pesticides in Tea via LC–MS/MS: Simple Sample Preparation and APCI to Improve Analyte Coverage

As regulatory laboratories search for and implement consolidated methods for multiple matrix and analyte classes, compound lists increase to hundreds or thousands of targets. Multi-instrument approaches are often relied upon to analyze all pesticide targets, with the workload split between liquid chromatography–mass spectrometry (LC–MS) and gas chromatography–mass spectrometry (GC–MS) instrumentation. In this work, a simple solvent extraction approach was coupled with dual source electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) modes on an LC–tandem mass spectrometry (MS/MS) instrument to analyze 395 analytes extracted from black tea (345 compounds via ESI and 50 compounds via APCI, along with the internal standards). Excellent method performance (defined as an accuracy of 70–120% and a precision of &lt;20% at one of two validation levels) was achieved for over 93% of analytes, including compounds normally analyzed by GC–MS, such as trifluralin, chlorfenson, chlormephos, fenchlorphos, etridiazole, and others. This approach can allow the consolidation of a pesticide method to a single instrument or significantly reduce the workload of a complementary GC–MS method.

Endothermic solvent extraction of copper (II) with furfuryl thioalcohol from sulfate medium

A simple solvent extraction method was developed to extract copper (II) from sulfate solution. The extraction of copper (II) with furfuryl thioalcohol was investigated. The effect of variables such as aqueous phase pH, furfuryl thioalcohol concentration, temperature, stripping reagents, and diluents was investigated. The extraction data revealed that using 15% (v/v) furfuryl thioalcohol with aqueous solution containing 0.5 mol L-1 Na2SO4, equilibrium pH 5.5, and phase ratio organic phase: aqueous phase (O:A) of 1:1 resulted in 98.20 percent extraction of copper (II) without nickel coextraction (II). Extraction isotherm results show that the extraction procedure is endothermic, with ΔH = 28.542 kJ mol-1 and ΔS = 41.740 J K-1 mol-1. Using 2.0 M H2SO4, copper loaded in organic phase was stripped at a rate greater than 99 percent.

Extraction of aromatic compounds from silver banana peel (Musa sapientum): qualitative and sensory approach

Silver banana (Musa sapientum) is one of the most consumed fruits in Brazil, and the country is its fourth largest producer in the world. The use of banana peel as a raw material in the industry can help in the production of natural aromas containing substances that resemble the fruit itself, and is therefore a valuable destination to be given to an organic waste that is generated in abundance. To make this application feasible, the extraction of aromatic substances from the peel of silver banana by isopropanol was tested in this work. Analyzes were performed by gas chromatography with mass spectrometry, aiming to characterize both the peel extract obtained experimentally and a commercial banana aroma available on the market. The analysis of the extracts showed that several substances associated with the banana aroma were extracted, at variable proportions, indicating that the extraction technique with isopropanol was effective in obtaining aromatic compounds relevant to the banana aroma from its peel. In turn, the comparison between the composition of the extract obtained from the banana peel and the commercial aroma of this fruit indicated the presence of an important aromatic compound in common: isoamyl acetate, which has a sweet and fruity sensory descriptor, with banana and pear characteristics. The recovery of this compound, which is already widely used in the flavor industry, confirmed the potential of the application of simple solvent extraction technology in this industrial sector, enabling the reuse of banana waste.

Identification and Quantification of Bisphenols in Water by Dissipation followed by Silylation using Gas Chromatography-Mass Spectrometry Analysis

Bisphenols are important endocrine disruptors, which were widely used in the variety of food packing and storage materials which often come into contact with various food products packed in them. The presence of bisphenols in water is harmful for the health of humans as well as aquatic animals and also, they accumulate over a period of time. Hence, the present work aimed to develop a simple and accurate GCMS-SIM method for the quantification of bisphenols in packaged drinking water as well as the water samples collected in river and lakes in Andhra Pradesh state of India. Bisphenols were extracted by simple solvent extraction with acetonitrile and silylated by N,O-bis (trimethylsilyl)trifluoro acetamide and analyzed by GC-MS. Various parameters that affect the recovery of the analytes were carefully optimized and the developed method was validated. The recoveries of the analytes were in the range of 80-120 % with quantification limit of 1 ng/L. The calibration curve was linear in the concentration range of 5 ng/L to 10 μg/L. The method was applied for the quantification of bisphenols in packaged drinking water at room temperature and at 50 ºC at various time intervals. The results proved that the water sample kept at room temperature doesn’t shows peaks corresponding to bisphenols. The water sample exposed to 50 ºC for 30 days bisphenols content 10, 12, 22 and 8 ng/L respectively for bisphenol G (BPG), bisphenol F (BPF), bisphenol E, (BPE) and bisphenol A (BPA) whereas the same sample at 180 days of exposer shows 60, 51, 61 and 22 ng/L respectively confirms that the leaching of plastic due to temperature increases the bisphenols level. Among the real time samples studied, the bisphenols level was observed to be very high in Kolleru Lake and it is having 17, 14, 8 and 12 ng/L of BPG, BPF, BPE and BPA, respectively confirms that due to high plastic pollution the bisphenols level was high in these samples. Hence, it can be concluded that the method can be suitable for the analysis of bisphenols in drinking water as well as in wastewater samples.

Molecular cartography of residue pesticides on grape surface in 3D by ambient ionization tandem mass spectrometry.

Thermal desorption-electrospray ionization tandem mass spectrometry (TD-ESI/MS/MS) was used to characterize the residual pesticides that were collectedfromthe surface of a grapewithmetallic sampling probes. Fungicides, insecticides, and miticides were detected, where results were validated by simple solvent extraction followed by gas chromatography tandem mass spectrometry and liquid chromatography tandem mass spectrometry analyses. To explore the distribution of pesticide residues on grape surfaces, 149 locations of a grape surface were collected and followed by TD-ESI/MS/MS analysis. The molecular cartography was then generated from analysis of residual pesticides on the grape surface in 3D.

A LC-MS/MS method with electrospray ionization and atmospheric pressure chemical ionization source for analysis of pesticides in hemp

BackgroundPesticide testing for hemp has traditionally focused on techniques like QuEChERS with dSPE and SPE which demand time-consuming sample preparation, typically resulting in poor recovery rates for some pesticides, and requires the use of both LC-MS/MS and GC-MS/MS based instruments to cover the analysis for all regulated pesticides. In this study, we describe a streamlined approach for working with LC-MS/MS featuring a dual electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) sources using solvent extraction for faster and easier sample preparation and with 80–120% recovery for the analysis of all of 66 pesticides (regulated by California state in cannabis) with low detection limits in hemp.MethodsA simple solvent extraction with acetonitrile was used to extract pesticides from hemp. A LC-MS/MS system with dual ESI and APCI source was used to determine sensitivity for the analysis of 66 pesticides in hemp matrix, 62 pesticides were analyzed using an 18-min LC-MS/MS method with an ESI source and the other 4 pesticides were measured using a 6-min LC-MS/MS method with an APCI source.ResultsThe limit of quantitation (LOQ) of all 66 pesticides in hemp was in the range of 0.0025–0.1 μg/g which was well below the California state action limits of these analytes in cannabis products. A simple, fast, and cost-effective solvent extraction method was used for sample preparation to get good recovery in the range of 80–120% with RSD less than 20%. The unique ionization mechanism of chlorinated pesticides such as pentachloronitrobenzene using the LC-MS/MS system with an APCI source was elucidated. The proficiency test report generated with the LC-MS/MS method showed acceptable results for all of 66 pesticides in hemp with all of th z scores less than 2 with no false positives and negatives. The stability data collected over 5 days showed RSD less than 20% for 66 pesticides in hemp, and this demonstrated the robustness of the LC-MS/MS system used in this work.ConclusionsA LC-MS/MS method with dual ESI and APCI sources was developed for the analysis of 66 pesticides in hemp. The recovery of all pesticides from a hemp matrix was in the acceptable range of 80–120% with RSD less than 20%.

Water-dispersible chlorophyll-based fluorescent material derived from willow seeds for sensitive analysis of copper ions and biothiols in food and living cells

The environmental risk of artificial synthetic dyes sparked interest in exploring high-security fluorescent materials for suitable analysis applications. Chlorophyll-based fluorescent material is a good candidate but subjects to inferior dispersibility and low fluorescence efficiency in water. In this work, we successfully prepared a water-dispersible chlorophyll-based fluorescent material through simple solvent extraction of willow seeds. Compared to other conventional sources of chlorophyll, such as willow leaves, metasequoia, and green algae, only the chlorophyll-based material from willow seeds (C-WS) can retain good near-infrared fluorescence performance with an emission wavelength of 677 nm in the water phase, which can promote the practical application of chlorophyll-based fluorescent materials. An “on-off-on” sensing system was constructed based on C-WS for the highly sensitive and selective detection of Cu2+ and biothiols in aqueous solution. The limit of detection for Cu2+ and GSH can reach 1.2 nM and 92 nM, respectively. Furthermore, the proposed system was successfully used in the detection of Cu2+ in real water samples and biothiols in food samples, and successfully applied for the visualization of intracellular Cu2+ and biothiols in Hela cells.

Electrocatalytic and stoichiometric reactivity of 2D layered siloxene for high‐energy‐dense lithium–sulfur batteries

AbstractLithium–sulfur batteries (LSBs) have emerged as promising power sources for high‐performance devices such as electric vehicles. However, the poor energy density of LSBs owing to polysulfide shuttling and passivation has limited their further market penetration. To mitigate this challenge, two‐dimensional (2D) siloxene (2DSi), a Si‐based analog of graphene, is utilized as an additive for sulfur cathodes. The 2DSi is fabricated on a large scale by simple solvent extraction of calcium disilicide to form a thin‐layered structure of Si planes functionalized with vertically aligned hydroxyl groups in the 2DSi. The stoichiometric reaction of 2DSi with polysulfides generates a thiosulfate redox mediator, secures the intercalation pathway, and reveals Lewis acidic sites within the siloxene galleries. The 2DSi utilizes the corresponding in‐situ‐formed electrocatalyst, the 2D confinement effect of the layered structure, and the surface affinity based on Lewis acid–base interaction to improve the energy density of 2DSi‐based LSB cells. Combined with the commercial carbon‐based current collector, 2DSi‐based LSB cells achieve a volumetric energy density of 612 Wh Lcell−1 at 1 mA cm−2 with minor degradation of 0.17% per cycle, which rivals those of state‐of‐the‐art LSBs. This study presents a method for the industrial production of high‐energy‐dense LSBs.