Simultaneous Separation Research Articles

A simultaneous isotope separation enhancement: Integration of the D isotope enrichment process and the O18 isotope enrichment process

Nowadays, the two isotope enrichment processes that employ water as the raw material are the ones for O18 isotope enrichment and D isotope enrichment, both of which disregard the interactions between their processes and fail to account for the full potential of D isotope. Therefore, an integration process is established in this paper. To achieve the full utilization of the D isotope in this process, an improved H2O-H2S dual-temperature isotope exchange system (IGS) is developed as the mass exchanger to transfer the D isotope obtained from the normalization of the heavy oxygen water distillation product in the hot section to the cold section. Through the simultaneous enhancement strategy, the IGS process requires 0.284531 mol/hr of feed to produce 0.2018 mol/hr of D isotope while about 30,266 times of feed is required for conventional GS process under the same process condition. Consequently, the D isotope enrichment process can be changed from factory scale to lab scale. The heavy water and heavy oxygen water products can be produced by the cold and hot sections of the IGS process, respectively, making the recovery ratio of 99.98% and the wastewater ratio of 0%.

Triblock copolymers as versatile constituents of double stimuli-responsive ionic-liquid-based aqueous biphasic systems

This work proposes the use of triblock copolymers as structurally versatile constituents to develop double stimuli-responsive aqueous biphasic systems (ABS) comprising ionic liquids (ILs). Phase diagrams of ABS comprising cholinium acetate ([Ch][C2O2]) and triblock copolymers composed of polyethylene oxide (PEO) and polypropylene oxide (PPO) with adjustable compositions of PEO, 20% (PE 6200) and 40% (PE 6400), were determined by the cloud point titration method at several temperatures (25–45 °C) and pH (5–7). These ABS present, for all the tested pH conditions, a Lower Critical Solution Temperature (LCST)-like behavior. However, only ABS with PE 6400 copolymer exhibit a simultaneous response to both stimuli. Compared to the homologous homopolymer polypropylene glycol (PPG), and despite their lower capacity to form ABS, copolymers with an adequate content of PEO provide a stronger response to the simultaneous action of pH and temperature. The results obtained highlight the value of an appropriate adjustment of the polymer structure/monomer composition in the development of ABS with double response to temperature and pH. The enhanced tailoring ability of the proposed systems is demonstrated with the simultaneous separation of two dyes by the application of the studied stimuli.

Simultaneous quantification of (E) and (Z) isomers of rilpivirine and four degradation products in bulk and tablets by reversed-phase ultra-high-performance liquid chromatography and confirmation of all by molecular weight.

The (E)-isomer of rilpivirine is an approved antiretroviral drug used to treat human immunodeficiency virus. A simple, fast, accurate, and precise analytical method is required to confirm the quality, purity, efficacy, and safety of drug substances and drug products containing rilpivirine. This research article offers a comprehensive ultra-high performance liquid chromatography method for the simultaneous separation and quantification of (E) and (Z) isomers of rilpivirine, including two amide impurities, one nitrile impurity, and one dimer impurity, in both bulk and tablet forms. After complete validation, the proposed reversed-phase ultra-high-performance liquid chromatography method has proven to be simple, fast, linear, accurate, and precise, with a lower limit of quantification and detection of 0.05 and 0.03μg/ml, respectively, for all six analytes. Separation was achieved on a Waters Acquity ethylene bridged hybrid Shield RP18 (150×2.1mm, 1.7μm) column maintained at 35.0°C using a gradient elution of acetonitrile and 0.05% formic acid in 10mM ammonium formate at a flow rate of 0.30ml/min. A systematic forced degradation study on the undissolved rilpivirine revealed the formation of acid-base hydrolyzed amide impurities (Impurity-A and Impurity-B), oxidative nitrile impurities (Impurity-C), and Z-isomer and dimer impurities of rilpivirine (Impurity-D and Impurity-E) due to alkaline hydrolysis and photodegradation. The proposed method is primarily appropriate for applications requiring the precise determination of desired and undesired isomers of rilpivirine and its degradation products, such as those involving the safety, efficacy, and quality roles of rilpivirine in bulk and tablet forms. Additionally, the proposed ultra-high-performance liquid chromatography method in combination with a mass spectrometer and photo-diode array detector is helpful for the confirmation and correct identification of all analytes.

Simple high-performance liquid chromatography-ultraviolet method for simultaneous separation and detection of 14 bisphenol pollutants in building materials.

A high-performance liquid chromatography-ultraviolet method was developed for rapidly and simultaneously analyzing novel and typical bisphenols in building materials, including bisphenol S, diphenolic acid, bisphenol F, bisphenol E, bisphenol A, bisphenol B, bisphenol AF, bisphenol AP, bisphenol C, bisphenol FL, bisphenol Z, bisphenol BP, bisphenol M, and bisphenol P. By using a Kromasil 100-5 C18 column, these bisphenols were completely separated in 40min via gradually increasing the concentration of methanol in the mobile phase from 45 to 80% during the elution process. In particular, this method achieved the synchronous analysis of bisphenol S, diphenolic acid, bisphenol FL, bisphenol BP, and bisphenol M through HPLC, which were difficult to separate and had to be identified and detected through mass spectrometry. The limits of detection of the method ranged from 0.002 to 0.040mg/L for these 14 bisphenols, with a precision of less than 4.9% (n=7, c=0.05mg/L). The analytical results for five types of building materials (phenolic, epoxy, polycarbonate, polyester, and polysulfone resins) indicated that the proposed method is appropriated for the rapid measurement of bisphenols in real samples.

Simultaneous measurement of amino acid enantiomers in the serum of late-life depression patients using convenient LC–MS/MS method with Nα-(5-fluoro-2,4-dinitrophenyl)-l-leucinamide Derivatization

D-amino acids may be indicators of late-life depression but separation and quantification of enantiomers which differ only by optical rotation sign remain challenging due to their identical physical and chemical properties. A convenient LC-MS/MS method was developed for the simultaneous measurement of l- and d-amino acids based on the chiral derivatization reagent, Nα-(5-fluoro-2,4-dinitrophenyl)-L-leucinamide, and conventional octadecylsilane reversed-phase column. Methanol was used as the extraction solvent and a single-step derivatization reaction using volatile triethylamine eliminated the requirement for desalination prior to LC-MS/MS. Simultaneous separation and identification of 21 amino acids and the enantiomeric compositions of the 18 chiral proteogenic entities were achieved. Low limits of detection (0.03–4.0 nM), wide linear range (0.01–20 μM), good precision (RSDs < 10 %) and negligible matrix effects indicated the suitability of the method. Application of the method to the quantification of serum chiral amino acids in late-life depression patients (n = 40) and controls (n = 35) found a total of 17 L-amino acids, 14 D-amino acids, DL-asparagine, glycine and γ-aminobutyric acid. The statistical evaluation showed significant differences of glycine, L-threonine and D-methionine between late-life depression patients and controls, indicating that these are potential biomarkers of late-life depression.

Abstract 6611: Harnessing the power of multiomics from a single sample to explore tumor heterogeneity and advancing immuno-oncology research

Abstract The omics era has greatly expanded the repertoire of approaches available for researchers and clinicians to unravel the complexity behind cancer onset in humans: Next Generation Sequencing (NGS) approaches can characterize genomes, epigenomes, transcriptomes and proteomes of patient samples. Advanced DNA barcoding and automated microfluidics can take this to the next level, enabling multiomic characterization of single cells. Peripheral blood mononuclear cells (PBMCs) offer a window into the immune system that, when combined with these omics tools, can provide an insight into immune cells mediating anti-tumor responses in cancer patients. Here we detail a workflow using a single blood draw to rapidly produce a diverse set of multiomics results including genomics, epigenomics, transcriptomics and proteomics. This starts with automated sample handling and processing of the primary blood draw to ensure high viability and yield of PBMCs, along with simultaneous plasma separation and collection. These samples are then aliquoted and simultaneously processed for automated and semi-automated whole exome sequencing, single-cell RNA sequencing, methylation sequencing and Olink proteomics assay. Germline and somatic mutations can be detected using whole exome or whole genome sequencing with deep coverage, whereas methylation, ATAC or ChIP sequencing can be used for epigenetic characterization of the same sample. While bulk expression offers a high-level transcriptomics profile, single-cell transcriptomics facilitates detection of gene expression changes in each individual cell type, allowing for analysis of rare cell types including circulating tumor cells. Olink proteomic assays can be utilized for both biomarker discovery and validation, with highly targeted or broad-spectrum panels. With this robust workflow and advanced robotics for sample handling and processing to minimize potential batch effects, all these datatypes can be produced within days of primary sample collection using minimal sample amounts. High throughput integrative omics workflows, as described here, are useful in gaining a multidimensional view of cancer and advance immunotherapies by characterizing immune cell modulation in tumor progression, and can be expanded for use in tumor/normal analysis, evaluation of metastases and exploration of tumor microenvironment. Citation Format: Bhagyashree S. Birla, Andrea O'Hara, Elizabeth Louie, Ben Niu, Haythem Latif, Vanessa Tumilasci, Yang Han, Yongjun Fan, David Corney, Pranay Vishwanath, Wei Wang, Alfredo Staffa, Ilaria DeVito, Laure Turner, Chris Mozdzierz, Peter Nowacki, Ginger Zhou. Harnessing the power of multiomics from a single sample to explore tumor heterogeneity and advancing immuno-oncology research. [abstract]. In: Proceedings of the American Association for Cancer Research Annual Meeting 2023; Part 1 (Regular and Invited Abstracts); 2023 Apr 14-19; Orlando, FL. Philadelphia (PA): AACR; Cancer Res 2023;83(7_Suppl):Abstract nr 6611.

Development of UPLC method for simultaneous assay of some COVID-19 drugs utilizing novel instrumental standard addition and factorial design

A green, rapid, and simple RP-UPLC method was developed and optimized by full factorial design for the simultaneous separation of oseltamivir phosphate, daclatasivir dihydrochloride, and remdesivir, with dexamethasone as a co-administered drug. The separation was established on a UPLC column BEH C18 1.7 µm (2.1 × 100.0 mm) connected with a UPLC pre-column BEH 1.7 µm (2.1 × 5.0 mm) at 25 °C with an injection volume of 10 µL. The detector (PDA) was set at 239 nm. The mobile phase consisted of methanol and ammonium acetate (8.1818 mM) in a ratio of 75.7: 24.3 (v/v). The flow rate was set at 0.048 mL min−1. The overall separation time was 9.5 min. The retention times of oseltamivir phosphate, dexamethasone, daclatasivir dihydrochloride, and remdesivir were 6.323 ± 0.145, 7.166 ± 0.036, 8.078 ± 0.124, and 8.572 ± 0.166 min (eight replicates), respectively. The proposed method demonstrated linearity in the ranges of 10.0–500.0 (ng mL−1) and 0.5–30.0 (µg mL−1) for oseltamivir phosphate, 50.0–5000.0 (ng mL−1) for dexamethasone, 25.0–1000.0 (ng mL−1) and 0.5–25.0 (µg mL−1) for daclatasvir dihydrochlorde, and 10.0–500.0 (ng mL−1) and 0.5–30.0 (µg mL−1) for remdesivir. The coefficients of determination (R2) were greater than 0.9999, with percentage recoveries greater than 99.5% for each drug. The limits of quantitation were 6.4, 1.8, 7.8, and 1.6 ng mL−1, and the limits of detection were 1.9, 0.5, 2.0, and 0.5 ng mL−1 for oseltamivir phosphate, dexamethasone, daclatasivir dihydrochloride, and remdesivir, respectively. The proposed method was highly precise, as indicated by the low percentage of relative standard deviation values of less than 1.2% for each drug. The average content and uniformity of dosage units in the studied drugs' dosage forms were determined. The average contents of oseltamivir phosphate, dexamethasone, daclatasivir dihydrochloride, and remdesivir were nearly 93%, 102%, 99%, and 95%, respectively, while the uniformity of dosage unit values were nearly 92%, 102%, 101%, and 97%. Two novel methods were established in this work. The first method was used to assess the stability of standard solutions. This novel method was based on the slope of regression equations. The second was to evaluate the excipient's interference using an innovative instrumental standard addition method. The novel instrumental standard addition method was performed using the UPLC instrument program. It was more accurate, sensitive, time-saving, economical, and eco-friendly than the classic standard addition method. The results showed that the proposed method can estimate the tested drugs' concentrations without interference from their dosage form excipients. According to the Eco-score (more than 75), the Green Analytical Procedure Index (GAPI), and the AGREE criteria (total score of 0.77), the suggested method was considered eco-friendly.

Density separation of petrous bone powders for optimized ancient DNA yields.

Density separation is a process routinely used to segregate minerals, organic matter, and even microplastics, from soils and sediments. Here we apply density separation to archaeological bone powders before DNA extraction to increase endogenous DNA recovery relative to a standard control extraction of the same powders. Using nontoxic heavy liquid solutions, we separated powders from the petrous bones of 10 individuals of similar archaeological preservation into eight density intervals (2.15 to 2.45 g/cm3, in 0.05 increments). We found that the 2.30 to 2.35 g/cm3 and 2.35 to 2.40 g/cm3 intervals yielded up to 5.28-fold more endogenous unique DNA than the corresponding standard extraction (and up to 8.53-fold before duplicate read removal), while maintaining signals of ancient DNA authenticity and not reducing library complexity. Although small 0.05 g/cm3 intervals may maximally optimize yields, a single separation to remove materials with a density above 2.40 g/cm3 yielded up to 2.57-fold more endogenous DNA on average, which enables the simultaneous separation of samples that vary in preservation or in the type of material analyzed. While requiring no new ancient DNA laboratory equipment and fewer than 30 min of extra laboratory work, the implementation of density separation before DNA extraction can substantially boost endogenous DNA yields without decreasing library complexity. Although subsequent studies are required, we present theoretical and practical foundations that may prove useful when applied to other ancient DNA substrates such as teeth, other bones, and sediments.

A comprehensive method of ionic liquid screening and experimental verification for simultaneous separation of multiple sulfides from oil

Ionic liquid (IL) as the extractant has shown an excellent performance in oil desulfurization. However, it is still a great challenge to select an appropriate IL that can simultaneously remove multiple sulfides from oils due to enormous ILs' quantities. In this work, an ILs' screening method based on the fuzzy comprehensive evaluation function and COSMO-RS method was developed for oil extraction desulfurization. Four typical aromatic thiophene sulfides – thiophene (TS), benzothiophene (BT), dibenzothiophene (DBT), and 4,6-dimethyldibenzothiophene (4,6-DMDBT) were considered as the removal targets, and n-heptane was chosen as the model oil. By this method, a single IL – 1-butyl-3-methylpyridinium dicyanamide ([BMPy][DCA]) was selected from 702 ILs for removing the four sulfides from n-heptane. Liquid-liquid equilibrium (LLE) data of n-heptane + TS/BT/DBT/4,6-DMDBT + [BMPy][DCA] systems at 298.15 K were measured and then correlated by the NRTL equation. A data processing method for LLE experimental indices, distribution coefficient and selectivity, was proposed for their crossed curves and different measuring ranges to facilitate the comparison of ILs' extraction performance. The comprehensive experimental indices based on this processing method were compared with the comprehensive predicted indices obtained by screening. The results showed a consistent trend between the two, and the excellent desulfurization performance of [BMPy][DCA] was confirmed. The separation mechanism was then analyzed through the quantum chemistry method. The results showed that the interactions of four sulfides with either n-heptane or [BMPy][DCA] both were the van der Waals interaction and steric effect. The [BMPy][DCA] could attract the sulfides more potently than the n-heptane, demonstrating the extraction's mechanism and characteristics. The stronger itself interactions of BT, DBT and 4,6-DMDBT as solid sulfides limited their solubility in liquid–liquid two phases. In addition, the decomposition of interaction energy showed that the attraction between the sulfides and the [BMPy][DCA] was dominated by dispersion, assisted by electrostatics, and equipped with a small amount of induction. The essence of repulsion between them was the exchange-repulsion.

Pengaruh Surfaktan terhadap Pemisahan Logam Transisi Periode Pertama Menggunakan Metode Emulsion Liquid Membrane

First row transition metals are heavy metals that are very abundant in their compound form and widely applied in industrial fields because of their unique physical and chemical properties. These industrial activities often produce waste that still contains toxic transition metal. To overcome that problems, the transition metal must be separated by an effective and efficient method, that is the emulsion liquid membrane (ELM) because simultaneous separation process. ELM is a separation method that involves three phases. The determinant of the success of the ELM process is the stability of the emulsion which depends on the concentration and type of the surfactant used. Types of surfactants that can be used in the first row transition metal separation using the ELM method are non-ionic surfactants such as Span 80, a mixture of Span 80-Tween 80 and Polyamine ECA 4360J. Therefore, this review article aims to determine the effect of concentrations and type of that surfactants on emulsion stability and extraction efficiency in the separation of first row transition metals using the ELM method.Keywords: First row transition metals, emulsion liquid membrane, surfactant

Structured electroplating sludge derived membrane for one-step removal of oil, metal ions, and anions from oil/water emulsions

The effective simultaneous treatment of hazardous waste sludge and complex oil/water emulsions in one way is urgently desired but still a challenging issue. Herein, this work for the first time presents a green and efficient strategy to fabricate an electroplating sludge (ES) derived multifunctional self-supporting membrane for the one-step removal of emulsified oils, soluble metal ions, and anions in complex oily wastewater. Due to low cost of ES and sustainability of the solvent selected in fabrication process, the large-scale application of the membrane is easily to promote. The assembled hierarchical nanostructure endowed robust underwater superoleophobicity of the membrane even under various corrosive aqueous environments, as well as excellent ultra-low oil adhesion and anti-oil-fouling performance, without chemical modification. Significantly, the multifunctional membrane possessed desirable simultaneous separation efficiency for five typical oil-in-water emulsions (>99.4%, high oil/water selective wettability), including crude oil-in-water emulsion with high viscosity (>99.6%), Cu2+ (>96.1%, surface complexation and ionic exchange), and Cl- (>92.7%, electrostatic attraction). Therefore, this green, low-cost, and multifunctional membrane not only allows the large-scale resource utilization of hazardous waste sludge, but also effectively solves the problems of complex oily wastewater purification.

Development of HPLC-CAD method for simultaneous quantification of nine related substances in ursodeoxycholic acid and identification of two unknown impurities by HPLC-Q-TOF-MS

Ursodeoxycholic acid has gained increasing attention due to its recent discovery of the preventive effect on SARS-CoV-2 infection. Ursodeoxycholic acid has been included in various pharmacopoeias as an old drug, and the latest European Pharmacopoeia lists nine potential related substances (impurities A∼I). However, existing methods in pharmacopoeias and literature can only quantify up to five of these impurities simultaneously, and the sensitivity is inadequate, as the impurities are isomers or cholic acid analogues lacking chromophores. Herein, a novel gradient RP-HPLC method coupled to charged aerosol detection (CAD) was developed and validated for the simultaneous separation and quantification of the nine impurities in ursodeoxycholic acid. The method proved sensitive and allowed the quantification of the impurities as low as 0.02 %. Relative correction factors of the nine impurities were all within the range of 0.8–1.2 in the gradient mode by optimizing chromatographic conditions and CAD parameters. In addition, this RP-HPLC method is fully compatible with LC-MS due to the volatile additives and high percentage of the organic phase, which can be directly used for the identification of impurities. The newly developed HPLC-CAD method was successfully applied to commercial bulk drug samples, and two unknown impurities were identified by HPLC-Q-TOF-MS. The effect of CAD parameters on the linearity and correction factors was also discussed in this study. Overall, the established HPLC-CAD method can improve the methods in current pharmacopoeias and literature and contributes to understanding the impurity profile for process improvement.

A new multiresidue thin layer chromatography–ultraviolet detection method for the rapid determination of six herbicides residue applied as ready mix formulation for rice

AbstractThe purpose of this study was to develop a new multiresidue thin‐layer chromatography analysis method for the simultaneous analysis of herbicides in soil and plant samples. A new liquid‐liquid extraction method was also developed for the extraction and identification of herbicides from the soil, rice grain, and straw samples. The thin layer chromatography‐ultra violet technique with silica gel 60 F254 thin layer chromatography plates, using a solvent system consisting of ethyl acetate, hexane, benzene, and methanol was found to be most effective in simultaneous separation and identification of all herbicides with retention factor in the range of 0.21–0.91. The impurities and matrix effects from soil, water, grain, and straw were minimal and did not interfere with the identification of any targeted herbicide. The method developed is found suitable to detect residues of herbicides in the soil, rice grains, and straw samples with a limit of determination of 0.1–0.01 mg/kg. The validation parameters of the developed method were satisfactory and therefore can be successfully used for the simultaneous determination of the herbicides in the soil, water, and plant samples. This method can also be used to determine these herbicides in other environmental samples as well as in Forensic analysis of biological/non‐biological samples.

Speciation of Fe(II) and Fe(III) in Chinese Yellow Rice Wine Using Direct Immersion Dual-Drop Microextraction Coupled with Graphite Furnace Atomic Absorption Spectrometry (GFAAS)

A new direct immersion dual-drop microextraction (DIDDME) procedure is described for Fe(III) and Fe(II) speciation followed by detection with graphite furnace atomic absorption spectrometry. This method is based upon the selective reaction of 1-(2-pyridylazo)-2-naphthol (PAN) and N-benzoyl-N-phenylhydroxylamine (BPHA) with Fe(II) and Fe(III) to form complexes at pH 1.5. Two solvent drops that contain PAN and BPHA were concurrently immersed in a sample solution for simultaneous separation of Fe(III) and Fe(II), respectively. This method eliminated time-consuming and labor-intensive oxidation of Fe(II) or reduction of Fe(III), which may provide incomplete conversion and contamination. Using the optimal conditions, the detection limits were 0.067 ng mL−1 and 0.054 ng mL−1 for Fe(II) and Fe(III) with relative standard deviations of 6.0% and 5.1%, respectively. Enrichment factors of 300-fold were obtained. The procedure was successfully utilized for the determination of Fe(II) and Fe(III) in Chinese yellow wine. To evaluate accuracy of this method, a rice certified reference material was analyzed and the result was in good agreement with the certified value.

Combination of multifunctional cotton fabrics derived from different steps during one preparation process to efficiently integrate superhydrophobicity, antibacterial property and photocatalysis for multi-purpose water purification

The discharge of wastewater containing oil and dye has caused serious water pollution, and it is difficult to achieve simultaneous oil-water separation and dye degradation with a single material. Herein, two multifunctional fabrics were prepared from different steps during one preparation process for the first time, as to the best of our knowledge, by simple chemical oxidation polymerization and dipping. Ag nanoparticles were introduced by reduction of polypyrrole (PPy) after the in-situ deposition of PPy on cotton (namely, CF-PPy/Ag). Then, CF-PPy/Ag was immersed in the polydimethylsiloxane (PDMS) solution to achieve wettability modification (namely, PDMS@CF-PPy/Ag). PDMS@CF-PPy/Ag not only showed good durability and superhydrophobicity, but also own excellent antibacterial property (>99.99 %) against E. coli and S. aureus. The fabric exhibited excellent oil-water separation performance and recyclability, with a high separation efficiency (>98.5 %) after 50 cycles. Meanwhile, CF-PPy/Ag could be applied for dye degradation due to the excellent antibacterial and photocatalytic activity. The degradation efficiencies of CF-PPy/Ag for methyl blue and methyl orange were 90.1 % and 95.2 %, respectively, after 90 min of simulated sunlight irradiation. More importantly, we further designed a simple device that combined both CF-PPy/Ag and PDMS@CF-PPy/Ag, which could simultaneously achieve efficient oil-water separation and dye degradation. Therefore, we believe that the efficient strategy of combining multifunctional cotton fabrics derived from different steps during one preparation process for multi-purpose purification of water can provide a promising solution for the treatment of complex water pollution and a new idea for the collaborative application of multifunctional fabrics in the field of oil-water separation.

Fractionation of a Three‐Particle Mixture by Brownian Sieving Hydrodynamic Chromatography

AbstractParticles ranging in size from a few nanometers (exosomes or viruses) to a few micrometers (bacteria or red blood cells) can be sorted using a size‐based separation process. One of the simplest techniques is provided by hydrodynamic chromatography (HDC) which typically requires long channels to achieve adequate resolution. A new separation mechanism based on a Brownian sieving effect coupled with HDC has recently been proposed to overcome these limitations. An efficiency improvement of up to 2000 % has been predicted for a two‐size mixture. The aim of this work is to study and optimize a modified geometry useful for obtaining the simultaneous separation of a three‐size diluted suspension. The results suggest a significant performance improvement, up to 3000 %, over the standard HDC.

Simultaneous determination of all aminobutyric acids by chiral derivatization and liquid chromatography-tandem mass spectrometry.

Aminobutyric acids include eight structural or stereoisomers that exhibit a wide range of biological activities. Recent evidence on some low abundant isomers have increased the demand for highly selective analysis of all the isomers; however, simultaneous separation of all the aminobutyric acid isomers has not been successful yet, except for a specialized method that uses multiple separation columns and a split of samples. In this study, we developed a new analytical method using chiral derivatization and liquid chromatography-tandem mass spectrometry to separate all the aminobutyric acid isomers in a single separation column. All the diastereomeric derivatives were resolved in a C18 column, and the derivatives showed characteristic fragmentation patterns in tandem mass spectrometry. By using the method, we analyzed the isomers in the Arabidopsis thaliana seeds and revealed the existence of three low abundant isomers, i.e., D-, L-β-aminoisobutyric acid, and D-β-aminobutyric acid. The proposed method uses a commercially available chiral derivatizing reagent and a broadly used column; therefore, it can be widely used in biological and food analyses.

Biphasic alcoholysis coupled with high-speed countercurrent chromatography for high performance on separating phorbol from Croton tiglium Linn extracts.

Phorbol is a tetracyclic diterpenoid found inEuphorbia tirucalli,Croton tiglium, andRehmannia glutinosa, and is nuclear of various phorbol esters. The rapid obtaining of phorbol with high purity highly contributes to its application, such as synthesizing phorbol esters with designable side chains and particular therapeutic efficacy. This study introduced a biphasic alcoholysis method for obtaining phorbol from croton oil by using polarity imparity organic solvents in both phases and established a high-speed countercurrent chromatography method for simultaneous separation and purification of phorbol. The optimized operation conditions of biphasic alcoholysis were a reaction time of 91min, a temperature of 14°C, and a croton oil-methanol ratio of 1:30 (g:ml). The phorbol during the biphasic alcoholysis was 3.2-fold higher in content than that obtained in conventional monophasic alcoholysis. The optimized high-speed countercurrent chromatography method was using the ethyl acetate/n-butyl alcohol/water at 4.7:0.3:5 (v:v:v) with Na2 SO4 at 0.36g/10ml as the solvent system, using the mobile phase flow rate of 2ml/min, the revolution of 800r/min, under which the retention of the stationary phase was achieved at 72.83%. The crystallized phorbol following high-speed countercurrent chromatography was obtained as high purity of 94%.

Sustainable extraction of ligustilide and ferulic acid from Angelicae Sinensis Radix, for antioxidant and anti-inflammatory activities

The 2030 Agenda for Sustainable Development envisions a rational use of energy and resources in all technological processes. However, in the extraction methods of compounds from medicinal plants and herbs, there is an urgent to reduce the use of organic solvents and increase the energy efficiency of these methods. Therefore, a sustainable extraction method (enzyme and ultrasonic co-assisted aqueous two-phase extraction, EUA-ATPE) of simultaneous extraction and separation of ferulic acid and ligustilide from Angelicae Sinensis Radix (ASR) was developed by integrating enzyme-assisted extraction (EAE) with ultrasonic-assisted aqueous two-phase extraction (UAE- ATPE). The effects of different enzymes, extraction temperature, pH, ultrasonic time, liquid-to-materials ratio, etc., were optimized by single-factor experiments and central composite design (CCD). Under the optimum conditions, the highest comprehensive evaluation value (CEV) and extraction yield were obtained by EUA-ATPE. Furthermore, recovery (R), partition coefficient (K), and scanning electron microscopy (SEM) analysis revealed that enzyme and ultrasonic treatment improved mass transfer diffusion and increased the degree of cell disruption. Besides, the EUA-ATPE extracts have shown great antioxidant and anti-inflammatory activity in vitro. Finally, compared to different extraction methods, EUA-ATPE achieved higher extraction efficiency and higher energy efficiency due to the synergistic effect between EAE and UAE-ATPE. Therefore, the EUA-ATPE provides a sustainable method for extracting bioactive compounds from medicinal plants and herbs, contributing to Sustainable Development Goals (SDG), including SDG-6, SDG-7, SDG-9, SDG-12, and SDG-15.

Facile biphasic system of γ-valerolactone/saline water for effective lignocellulose fractionation

Herein, novel γ-valerolactone (GVL)/saline water biphasic system was first introduced to depolymerize the recalcitrant structure of moso bamboo for further comprehensive utilization. Notably, as the main constituent of saline water, NaCl was initially investigated as control group to discuss the synergistic effect between NaCl and GVL. More than 90.7% of cellulose could be preserved under the optimum condition, followed by 97.9% of hemicellulose and 93.4% of lignin being separated, respectively. Meanwhile, the solvation effect of solvent molecules on lignin units was also verified by molecular dynamics simulation. Interestingly, more than 95.2% of hemicellulose and 86.8% of lignin were separated with 87.6% of cellulose preserved when saline water was directly introduced. This study exhibited an efficient process for simultaneous separation of sugars and lignin in lignocellulose, which provides an eco-friendly and environmentally benign method for biorefinery.