J Sep Sci [JOURNAL]
Sun
200 papers
Hydroxyl-Mediated Adsorption Site Distribution on Titanium Dioxide@Covalent Organic Framework and Enhanced Selective Separation and Detection of Lead Ions.
Li W, Yang Y, You Y … +5 more , Xing C, Xia A, Guo J, Gao P, Dong L
J Sep Sci · 2026 Feb · PMID 41706030 · Publisher ↗
This work designs a titanium dioxide@covalent organic framework composite material (TiO-COF), which optimizes the distribution of lead adsorption sites by adjusting the position of hydroxyl groups in the COF, thereby enh...
This work designs a titanium dioxide@covalent organic framework composite material (TiO-COF), which optimizes the distribution of lead adsorption sites by adjusting the position of hydroxyl groups in the COF, thereby enhancing the separation efficiency of trace Pb ions. The composite material integrates the advantages of metal oxides and porous materials, optimizing the separation performance of Pb ions through a synergistic enhancement effect. Additionally, its multi-interface structural characteristics provide the material with multidimensional selectivity, resulting in a highly selective separation material. In selectivity experiments, the material demonstrated high adsorption selectivity for Pb ions compared to several other metal ions. Thermodynamic and kinetic simulation results prove that the adsorption of Pb ions by TiO-COF conforms to the pseudo-second-order kinetics and the Langmuir adsorption model. After multiple cycles of use, the material still maintains high adsorption efficiency, demonstrating its potential clean and green application value in the highly selective separation of metal pollutants. The constructed material was used for the separation and preconcentration of Pb ions, establishing a detection system for trace Pb ions. The detection limit of the method is 0.073 µg L (3σ/K, n = 9), with precision ranging from 0.55% to 11.7% (n = 11), and a linear range of 0.2-5 µg L, exhibiting strong anti-interference capability. The constructed method achieves the determination of lead ions in real samples, with recoveries ranging from 95% to 103%. Moreover, the standard material GBW08607 was analyzed through the constructed system, and the t-test shows that the calculated t-value is 2.01, which is less than the tabulated t-value of 2.57 (n = 6), proving the reliability of the method. It provides a potential alternative material for the separation and analysis of other environmental pollutants.
Transposition of the Complementary Developing Solvent Technique to Flash Chromatography: A Structured Step-Based Fractionation Strategy for Complex Plant Extracts.
Fauquet J, Ellatiff A, Palmieri C … +4 more , Duez P, Blankert B, Wells M, Nachtergael A
J Sep Sci · 2026 Feb · PMID 41693126 · Publisher ↗
The Complementary Developing Solvent technique, originally developed for high-performance thin-layer chromatography, employs solvent systems with distinct polarity ranges to achieve enhanced chromatographic resolution wh...
The Complementary Developing Solvent technique, originally developed for high-performance thin-layer chromatography, employs solvent systems with distinct polarity ranges to achieve enhanced chromatographic resolution while covering a broad chemical space. This study demonstrates the successful adaptation of low polarity developing solvent and high polarity developing solvent systems to normal-phase flash chromatography for systematic fractionation. The system suitability test used in high-performance thin layer chromatography, namely the Universal HPTLC Mix, enabled direct comparisons between high-performance thin layer chromatography and flash chromatography, demonstrating a conserved polarity-driven retention hierarchy across chromatographic scales. To confirm compound identities and elution order, each chromatographic peak was collected and analyzed by tandem mass spectrometry, with MS/MS spectra manually matched against reference standards. Quantitative chromatographic performance was benchmarked using effective peak capacity (Pc), yielding a value of 16.41 for the high-polarity developing system, indicative of a globally balanced separation. In addition, a systematic isocratic step fractionation strategy was implemented by segmenting each elution gradient (low polarity developing solvent and high polarity developing solvent) into seven predefined polarity windows. This strategy was applied on a crude methanolic extract of Sideritis scardica Griseb., confirming robust and reproducible fractionation boundaries in a complex botanical matrix. Collecting a single fraction per isocratic step significantly reduces the number of samples for subsequent analysis such as bioassays and untargeted metabolomic profiling, thereby accelerating natural product discovery and dereplication workflows.
Characterization of Chemical Components and Metabolites in Tongqiao Huoxue Decoction Based on UHPLC-QTOF MS Technology and Multi Level Intelligent Platform.
Chen P, Bai L, Zheng X … +3 more , Wang M, Dong P, Han H
J Sep Sci · 2026 Feb · PMID 41689256 · Publisher ↗
In this study, we addressed the longstanding challenge of elucidating the complex material basis of traditional Chinese medicine (TCM) formulas by establishing an integrated, multi-platform UHPLC-QTOF MS data-analysis wo...
In this study, we addressed the longstanding challenge of elucidating the complex material basis of traditional Chinese medicine (TCM) formulas by establishing an integrated, multi-platform UHPLC-QTOF MS data-analysis workflow for Tongqiao Huoxue Decoction (THD), a prescription widely used in the clinical treatment of cerebral infarction. Unlike conventional single-software pipelines that often suffer from incomplete spectral libraries, limited algorithmic coverage, and platform-dependent biases, our strategy combined UNIFI, MS-DIAL, QI, and FBMN to jointly process the data, thereby reducing the analytical blind spots and interference inherent to any single tool. This multi-angle identification system enabled a high-confidence characterization of 235 chemical constituents in THD and 101 in vivo metabolites detected in serum and urine samples of rats, while also revealing predominant metabolite classes potentially associated with THD's pharmacodynamic mechanisms in cerebral infarction. The resulting workflow demonstrated high accuracy, reproducibility, and efficiency, offering a rigorous and comprehensive solution for biological and medicinal sample analysis. Overall, this work not only deepens the understanding of THD's therapeutic material foundation, but also provides a novel, generalizable methodological paradigm that advances mass-spectrometry-based characterization of multi-component TCM prescriptions and their in vivo transformation profiles.
Development of a Validated High-Performance Liquid Chromatographic Method for Simultaneous Quantification of Critical Impurities in Trihexyphenidyl Hydrochloride.
Tang Y, Du J, Wang W … +8 more , Zhao L, Kuang S, Liu Y, Chao L, Huang Z, Yu L, Nie L, Chen Y
J Sep Sci · 2026 Feb · PMID 41674326 · Publisher ↗
In this contribution, an efficient high-performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of four impurities in trihexylphe idyl hydrochloride. The developed HPLC method wa...
In this contribution, an efficient high-performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of four impurities in trihexylphe idyl hydrochloride. The developed HPLC method was based on an octadecylsilane-bonded silica gel column (Agilent TC-C18 250 mm × 4.6 mm, 5 µm) as the stationary phase, and the solvents were sodium hexafluorophosphate 0.05 mol/L and methanol for the gradient elution at a flow rate of 1.0 mL/min, with the injection volume of 20 µL, the ultraviolet (UV) detection at a wavelength of 210 nm, and the column temperature of 30°C. Under the established chromatographic conditions, all four target impurities were completely eluted within 30 min. The proposed method demonstrates good specificity, precision, robustness, and accuracy for the quantification of the four critical impurities in trihexyphenidyl hydrochloride, and was successfully applied for the analysis of trihexyphenidyl hydrochloride in a pharmaceutical preparation.
Separation of Lower Polarity Components From Ganoderma lucidum Spores by a Combined Approach of Ultra-High Pressure Extraction and pH-Zone-Refining Counter-Current Chromatography.
Wang Y, Yu J, Guo L … +6 more , Guo Y, Zhong K, Zhao L, Yue T, Wang H, Feng W
J Sep Sci · 2026 Feb · PMID 41674323 · Publisher ↗
An integrated strategy combining ultra-high pressure-assisted extraction and pH-zone-refining counter-current chromatography was developed for the efficient extraction and separation of the lower polar constituents from...
An integrated strategy combining ultra-high pressure-assisted extraction and pH-zone-refining counter-current chromatography was developed for the efficient extraction and separation of the lower polar constituents from Ganoderma lucidum spores. The ultra-high pressure extraction parameters were optimized using response surface methodology, achieving a high extraction yield of 1.739% under mild conditions (liquid-to-solid ratio of 21 mL/g, pressure of 268 MPa, time of 7 min), demonstrating higher efficiency and avoidance of thermal degradation compared to conventional techniques. For separation, pH-zone-refining counter-current chromatography was employed for the crude ultra-high pressure extraction using n-hexane/ethyl acetate/methanol/water (20:3:4:1, v/v, 10 mM trifluoroacetic acid in the upper phase and 10 mM aqueous ammonia in the lower phase), yielding Compounds 1-3, Fraction I, and the eluted Fraction II. Subsequently, for Fractions I and II, pH-zone-refining counter-current chromatography was further carried out using n-hexane/ethyl acetate/methanol/water (6:5:4:2, v/v, 10 mM trifluoroacetic acid in the upper phase and 10 mM aqueous ammonia in the lower phase) and n-hexane/ethyl acetate/methanol/water (60:5:40:4, v/v, 10 mM trifluoroacetic acid in the upper phase and 10 mM aqueous ammonia in the lower phase) as the solvent systems, yielding Compounds 4-6 and 7-10, respectively. All these obtained 10 compounds were classified into seven fatty acids, one lipid, one terpenoid, and one phthalate ester, which were all characteristic of low polarity, especially for the fatty acids with chain lengths ranging from C to C. This integrated ultra-high pressure extraction and pH-zone-refining counter-current chromatography approach markedly outperforms conventional techniques by drastically shortening the extraction time and enabling a highly effective, large-scale separation. Consequently, the ultra-high pressure extraction and pH-zone-refining counter-current chromatography platform represents a robust and promising methodology for the systematic investigation of hydrophobic constituents from natural resources.
Integrating Optical Feedback Alignment and Fluidic Control for Multiphase Flow-Assisted In Situ 3D Printing.
Ramirez-Alvarado G, Passmann K, Romero-Rendon A … +1 more , Sun G
J Sep Sci · 2026 Feb · PMID 41674310 · Full text
Additive manufacturing is transforming how microfluidic devices are prototyped and fabricated. Among various 3D printing methods, stereolithography (SLA) has become a dominant technique for microfluidics due to its high...
Additive manufacturing is transforming how microfluidic devices are prototyped and fabricated. Among various 3D printing methods, stereolithography (SLA) has become a dominant technique for microfluidics due to its high resolution and design flexibility, with widespread use in lab-on-a-chip applications. However, intrinsic limitations of SLA printing, such as challenges related to multi-material integration and microstructure fabrication in enclosed channels, continue to hinder the development of more complex microsystems, especially for analytical separation and tissue engineering applications. In this paper, we present a multiphase flow-assisted in situ 3D printing method to address these challenges, developed based on our previously reported in situ 3D polymerization (IS-3DP) concept. Our method utilizes an aqueous two-phase system (ATPS) to generate sequential printing layers through controlled fluidic confinement and integrates an image-guided alignment system to enable precise projection of printing patterns in microchannels. We demonstrate that viscosity tuning of the ATPS printing and blocking phases enables dynamic control of layer thickness, allowing customized and adaptive design of the 3D structure slicing. The image-guided alignment system employs a homography transformation mechanism to map the projection and printing planes via image feedback, providing real-time mask alignment with microchannel geometries. We characterize the mapping accuracy and projection fidelity and demonstrate the capability of this method by direct in-channel fabrication of complex 3D microstructures such as pyramids, cuboids, bridge-like void structures, as well as multi-material patterns. We envision the multiphase flow-assisted in situ 3D printing to offer a versatile tool for spatially controlled, high-fidelity, and multi-material microfabrication within confined microchannels in novel lab-on-a-chip applications.
Rapid Identification of Chemical Components and Screening of Beta-Klotho Agonists From Trichosanthes pericarpium Aqueous Extract Based on Affinity Ultrafiltration and Liquid Chromatography-Tandem Mass Spectrometry.
Wang Y, Wang H, Wu M … +3 more , Gao X, Gao Y, Zhao P
J Sep Sci · 2026 Feb · PMID 41674308 · Publisher ↗
Trichosanthes pericarpium (TP), a natural product rich in pharmacologically active constituents, exhibits potential cardioprotective effects. This study employed a ligand fishing strategy combined with identification to...
Trichosanthes pericarpium (TP), a natural product rich in pharmacologically active constituents, exhibits potential cardioprotective effects. This study employed a ligand fishing strategy combined with identification to efficiently characterize the chemical ingredients of TP and rapidly screen for Beta-Klotho (βKlotho) agonists, utilizing affinity ultrafiltration combined high-performance liquid chromatography-mass spectrometry (AUF-LC-MS). As a result, a total of 59 compounds were tentatively characterized, and 7 potential ligands were fished out when βKlotho acted as the targeted protein. Subsequently, three representative angling compounds, including diosmetin-7-O-β-D-glucopyranoside, cucurbitacin B, and rutin, were further verified by molecular docking visualization analysis and in vitro activity validation assays. Cell viability assays demonstrated that all three aforementioned compounds significantly increase the viability of myocardial cells injured by ischemia and hypoxia. Furthermore, terminal deoxynucleotidyl transferase dUTP nick end labeling (TUNEL) assays demonstrated that these compounds significantly attenuated cardiomyocyte apoptosis. Collectively, this study establishes a novel strategy for the systematic characterization and screening of bioactive compounds in natural products, providing a solid foundation for the development of βKlotho agonists derived from TP.
An Integrated UHPLC-Q-Orbitrap-MS/MS and In Vitro Gastrointestinal Simulation Strategy for Characterizing the Chemical Constituents and Metabolites of Shaoyao RuanGan Decoction.
Li H, Ma T, Jin G … +9 more , Guan S, Li J, Huang P, Hu X, Chen S, Wang Z, Tian J, Li S, Zhang X
J Sep Sci · 2026 Feb · PMID 41674303 · Publisher ↗
Shaoyao Ruangan Decoction (SYRGD), a classic traditional Chinese medicine (TCM) preparation composed of over a dozen herbs, is widely used in the clinical treatment of liver cancer, hepatitis, and liver cirrhosis. In thi...
Shaoyao Ruangan Decoction (SYRGD), a classic traditional Chinese medicine (TCM) preparation composed of over a dozen herbs, is widely used in the clinical treatment of liver cancer, hepatitis, and liver cirrhosis. In this study, we elucidated the chemical basis of SYRGD and, for the first time, its in vivo metabolic pathways and dynamic gastrointestinal changes by combining ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-Q-Orbitrap-MS/MS) with the Simulator of the Human Intestinal Microbial Ecosystem (SHIME) model. Results revealed the identification of 101 constituents in SYRGD, primarily including flavonoids, terpenoids, organic acids, and alkaloids. Within the SHIME digestive fluids, 69 prototype components and 67 metabolites were identified, with the metabolic pathways primarily involving hydroxylation, oxidation, sulfation, and glucuronidation. Dynamic analysis showed that most prototype components were gradually absorbed or transformed, exhibiting a decreasing concentration gradient from the stomach to the colon. In contrast, many metabolites showed significant enrichment in the stomach and small intestine prior to their absorption or further transformation, indicating that metabolic reactions occurred throughout the entire digestive process. This study provides a comprehensive reference for the clinical application and further development of SYRGD. The systematic methodology is rapid, reproducible, overcomes the limitations of conventional animal or clinical trials, and establishes a precise research strategy for investigating the metabolism of other complex herbal medicines.
Molecularly Imprinted Polymer‒Solid-Phase Extraction Coupled With High-Performance Liquid Chromatography-Ultraviolet Detection for Selective Determination of Ketoconazole in Cosmetic Shampoo.
Nguyen VT, Tran TT, Vo TK … +2 more , Tran TTT, Trung HK
J Sep Sci · 2026 Feb · PMID 41674288 · Publisher ↗
A molecularly imprinted polymer (MIP) was successfully synthesized through precipitation polymerization for the purpose of selectively extracting ketoconazole (KCZ) from cosmetic shampoo matrices. The polymerization proc...
A molecularly imprinted polymer (MIP) was successfully synthesized through precipitation polymerization for the purpose of selectively extracting ketoconazole (KCZ) from cosmetic shampoo matrices. The polymerization process employed methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, azobisisobutyronitrile as the initiator, and KCZ as the template within an acetonitrile/acetic acid (9:1, v/v) solvent system. Conditions for synthesis were optimized to enhance efficiency. Material characterization, conducted via Fourier-transform infrared spectroscopy, scanning electron microscopy, and Brunauer-Emmett-Teller analysis, confirmed the successful formation of the polymer. The MIP demonstrated a maximum adsorption capacity of 1.90 mg/g and a recovery rate of 94.98%, which were significantly higher compared to those of the non-imprinted polymer (0.47 mg/g and 39.67%, respectively). The material exhibited high selectivity for KCZ over structurally similar compounds. A high-performance liquid chromatography method with ultraviolet detection was developed and validated utilizing the synthesized MIP as a selective sorbent. The method displayed excellent linearity over a concentration range of 0.05-500 µg/mL, with a limit of detection of 0.193 µg/g, and a limit of quantification of 0.643 µg/g. These parameters indicate approximately a tenfold enhancement in sensitivity relative to previously reported ultrasound-assisted extraction methods. The method demonstrated excellent precision (relative standard deviation ≤ 6.06%) and high recovery rates (80.41%-98.86%) in real samples. Consequently, this study establishes a cost-effective, selective, and highly efficient approach for the determination of trace levels of KCZ in cosmetic products.
A Chromatographic Approach for Simultaneous Quantification of Multiple Anticoagulants in Human Plasma Samples.
Guidetti F, Fernandes SR, Barreiros L … +1 more , Segundo MA
J Sep Sci · 2026 Feb · PMID 41674238 · Full text
Anticoagulants are essential drugs for preventing and treating thromboembolic conditions by inhibiting blood clot formation. Warfarin, a vitamin K antagonist, is among the most prescribed agents but presents limitations,...
Anticoagulants are essential drugs for preventing and treating thromboembolic conditions by inhibiting blood clot formation. Warfarin, a vitamin K antagonist, is among the most prescribed agents but presents limitations, including a narrow therapeutic window and a high risk of adverse events, requiring strict monitoring to ensure both safety and therapeutic efficacy. In contrast, direct oral anticoagulants such as dabigatran, rivaroxaban, and apixaban offer improved safety profiles and generally do not require routine monitoring. Nevertheless, monitoring is required in special clinical situations, including emergencies, renal dysfunction, or for high-risk patients. In this context, the present study aimed to develop an HPLC method with UV/Vis detection for the simultaneous quantification of four anticoagulant agents (warfarin, dabigatran, rivaroxaban, and apixaban) in human plasma. Efficient separation of the four target analytes involved the evaluation of several parameters, including column type (Kinetex core-shell C18, Chromolith RP-18e, and Chromolith Phenyl), elution conditions, and injection volume (10-50 µL). The best separation was achieved within 12 min using a monolithic phenyl column and gradient elution, at a flow rate of 2 mL/min. The method was validated and has shown to be selective, linear in the range of 0.50-5.0 µg/mL for dabigatran and warfarin and 0.25-5.0 µg/mL for rivaroxaban and apixaban, accurate (85.7%-115.0%), and precise (CV ≤ 9.4%) for both intra- and inter-day assays. LOD and LOQ in plasma were ≤ 0.2 and ≤ 0.5 µg/mL, respectively. Stability testing demonstrated that all analytes remained stable at room temperature for 24 h, with only dabigatran showing reduced stability after three freeze-thaw cycles. The proposed method enabled rapid and simultaneous quantification of four clinically relevant anticoagulants in plasma samples.
Chemical Characterization of Mediterranean Macroalgae With a Focus on Antioxidant Molecules Through the Use of Liquid Chromatographic Techniques.
Vento F, Trovato E, Rigano F … +3 more , Micalizzi G, Giuffrida D, Mondello L
J Sep Sci · 2026 Feb · PMID 41674198 · Full text
Seaweeds represent an excellent vegetable protein resource capable of supporting the objectives of the sustainable blue economy. Today, attention toward algae is growing, due to their applications, both in biofuel produc...
Seaweeds represent an excellent vegetable protein resource capable of supporting the objectives of the sustainable blue economy. Today, attention toward algae is growing, due to their applications, both in biofuel production and as an alternative source of healthy food and nutraceuticals. The objective of this work was to valorize marine macroalgae coming from the Mediterranean area in order to be able to expand their potential use in the nutraceutical and pharmaceutical industries, maintaining the circularity of financial and biological resources. Micronutrients with higher antioxidant activity were determined in 10 samples, specifically four red algae, four brown algae, and two green algae. In particular, vitamin C was analyzed using a reversed phase (RP)-HPLC system coupled to photodiode array (PDA) detection, following extraction with an acidified aqueous solution. Vitamin E analysis was performed using a normal-phase HPLC system, following extraction with n-hexane and taking advantage of the high selectivity and sensitivity of fluorescence detector. Vitamin B12 was extracted with an acidified solution of methanol and water and analyzed by RP-HPLC system coupled to PDA and MS, the latter operated under selected ion monitoring mode to increase instrumental sensitivity and selectivity. Finally, carotenoids and pigments were extracted with an acetone/methanol solvent mixture and analyzed by RP-HPLC system coupled to PDA and MS to exploit the complementarity between MS and UV spectra for identification purposes. Overall, the validated HPLC methods confirmed the presence of vitamin E in all the samples analyzed, with highest levels obtained in two brown algae, namely, Undaria pinnatifida (1.54 ± 0.08 mg/kg) and Himanthalia elongata (0.93 ± 0.02 mg/kg), whereas vitamins C and B12 were detected only in two macroalgae species, including the widely consumed Porphyra sp., commercially known as Nori. Finally, carotenoids were mainly determined in the largely consumed U. pinnatifida sample, commercially known as Wakame.
Supercritical Carbon Dioxide Extraction With Dimethyl Carbonate and Bio-Ethanol as Co-Solvents for the Determination of Pesticide Residues in Black Pepper by Low-Pressure Gas Chromatography-Triple Quadrupole Mass Spectrometry.
Arena A, Zoccali M, Mondello L
J Sep Sci · 2026 Feb · PMID 41655077 · Full text
The determination of pesticide residues in spices is analytically challenging due to their high content of essential oils and secondary metabolites that could interfere with detection and quantification. In this study, s...
The determination of pesticide residues in spices is analytically challenging due to their high content of essential oils and secondary metabolites that could interfere with detection and quantification. In this study, supercritical fluid extraction (SFE), using green co-solvents, was evaluated for the extraction of 44 pesticides from black pepper (Piper nigrum). The extraction performance of bio-ethanol (bio-EtOH) and dimethyl carbonate (DMC) was compared under mild operating conditions. Optimal recoveries were obtained with 10% DMC, yielding an average of 92.6% across 44 pesticides, comparable to 93.7% using bio-EtOH. Method performance was assessed by low-pressure gas chromatography-triple quadrupole mass spectrometry (LP-GC-QqQMS). Linearity was achieved over the tested range, with limits of detection (within the range 0.1-17.9 µg kg) and quantification (within the range 0.3-59.8 µg kg) always below European Union (EU) maximum residue levels (MRLs). Accuracy ranged from 74.4% to 107.7%, with intra-day precision between 0.8% and 16.1%. A pronounced matrix effect was observed (average ionization suppression: -47.6%). The application of the validated method to commercial black pepper samples revealed the presence of diphenylamine, quinalphos, and phosalone, with only quinalphos exceeding EU MRLs. These findings demonstrate that SFE with DMC as a co-solvent provides an efficient, greener, and reliable extraction approach for multi-residue pesticide analysis in a complex spice matrix. The combination of SFE with LP-GC-QqQMS supports the implementation of greener and high-throughput monitoring workflows for complex spice matrices.
Rational Design of Functional Metal-Organic Frameworks as Chromatographic Stationary Phases: From Synthesis to Advanced Applications.
Ma Y, Zhou Y, Li D … +3 more , Cui J, Ma X, Fu Q
J Sep Sci · 2026 Feb · PMID 41655072 · Publisher ↗
Metal-organic frameworks (MOFs) have emerged as highly promising stationary phases in chromatographic separation technologies due to their exceptional structural tunability, high surface areas, and tailored pore environm...
Metal-organic frameworks (MOFs) have emerged as highly promising stationary phases in chromatographic separation technologies due to their exceptional structural tunability, high surface areas, and tailored pore environments. However, the transformation of these intrinsic advantages into practical chromatographic performance is often hindered by kinetic mass-transfer limitations, hydrolytic instability, and restricted accessibility for bulky analytes. This review systematically summarizes recent advances in the design and application of MOFs for chromatography, focusing on three critical material development directions: nano-sized MOFs, highly stable MOFs, and hierarchically porous MOFs. We first summarize the synthesis strategies, scientific challenges, and representative breakthroughs for each category, highlighting the transition between material properties and performance. The subsequent discussion critically evaluates their applications in gas chromatography (GC), liquid chromatography (HPLC), and capillary electrochromatography (CEC), with a particular focus on structure-performance relationships and the realization of material stability and nanoscale effects into enhanced separation efficiency, selectivity, and operational lifetime. By bridging the gap between advanced material synthesis and practical separation needs, this review aims to provide a roadmap for the development of next-generation and high-efficiency MOF-based stationary phases.
Microscale Affinity Chromatography for Biointeraction Analysis: Strategies, Principles and Applications.
Hage DS, Pinky NS, Sajeeb BK … +6 more , Rahman MM, Olupathage H, Alim S, Kyei I, Zingler Z, Heenkenda S
J Sep Sci · 2026 Feb · PMID 41655070 · Full text
The analysis of interactions between biological agents or with surrounding chemicals is important in many areas of modern biochemical, biomedical, and environmental research. Microscale platforms based on affinity chroma...
The analysis of interactions between biological agents or with surrounding chemicals is important in many areas of modern biochemical, biomedical, and environmental research. Microscale platforms based on affinity chromatography have been shown to be a powerful set of tools for these studies. This approach makes use of an immobilized binding agent as a stationary phase in a microscale platform for either direct examination of the interactions of this agent with an applied target solute or as a secondary capture agent to probe a solution-phase interaction. This review will examine the various platforms and strategies that have been used in microscale affinity chromatography, or µAC, to characterize and study biointeractions. The general principles of µAC and schemes based on this approach will be examined, along with applications of this technique. Examples of approaches that will be considered will include zonal and frontal analysis methods, as well as a variety of schemes by which µAC can be employed in kinetic studies. In each case, the theory and principles of these methods will be provided along with examples of their use in biointeraction studies.
Selective Adsorption Behavior of Gallium Ions on Graphene-Based Surface Ion-Imprinted Material From Simulated Acid Leach Solution of Fly Ash.
Liu B, Zhang M, Chen M … +5 more , Qin L, Wang M, Fu D, Liu W, Liu X
J Sep Sci · 2026 Feb · PMID 41631531 · Publisher ↗
A graphene-based material for the selective adsorption of gallium ions has been prepared by combining ion-imprinting technology with adsorption. This material is capable of separating and extracting gallium ions from the...
A graphene-based material for the selective adsorption of gallium ions has been prepared by combining ion-imprinting technology with adsorption. This material is capable of separating and extracting gallium ions from the acid leachate of fly ash. Morphological and structural characterization of the material was performed using scanning electron microscopy and Fourier-transform infrared spectroscopy, which confirmed that the material possesses a three-dimensional structure and that functional monomers have successfully complexed with graphene oxide substrates. The maximum adsorption capacity of the material reaches 86.29 mg/g at a solution pH of 3. In the selective adsorption tests, the selective separation factors of gallium ions relative to aluminum, magnesium, iron, and calcium ions were 16.50, 49.50, 9.90, and 99.00, respectively. Meanwhile, the material maintained excellent adsorption capacity and structural stability in cyclic regeneration experiments, with no obvious dissolution loss observed. The adsorption mechanism of the material was analyzed via X-ray photoelectron spectroscopy, and the results indicated that it primarily involves cation exchange between carboxyl groups and gallium ions. This work demonstrates that the three-dimensional ion-imprinted hydrogel adsorbent plays a significant role in the selective adsorption of gallium ions and the subsequent solid-liquid separation.
Rambutan-Like Nickel Sulfide Modified With Carbon Nanospheres on Nickel Foam for Syringe Membrane Filter-Based Extraction of Nitroimidazoles.
Qin H, Yao W, Qiao L … +1 more , Yao X
J Sep Sci · 2026 Feb · PMID 41631530 · Publisher ↗
In the present work, nickel sulfide (NiS) was modified on the surface of Ni foams (NiF) by in-situ growth, and the prepared rambutan-like NiS/NiF materials were further decorated with carbon nanospheres. Subsequently, th...
In the present work, nickel sulfide (NiS) was modified on the surface of Ni foams (NiF) by in-situ growth, and the prepared rambutan-like NiS/NiF materials were further decorated with carbon nanospheres. Subsequently, the prepared C/NiS/NiF was loaded into a syringe filter and used for syringe membrane filter-based solid-phase microextraction (SMF-SPME) of five nitroimidazoles (NDZs), followed by high-performance liquid chromatography-ultraviolet detection. The metal affinity of divalent Ni (II) and the imidazole group could contribute to the selective adsorption to NDZs, and the structural porous support of Ni foams, the in-situ modified NiS, and carbon nanospheres facilitated the improvement of SMF-SPME efficiency. The main experimental parameters affecting the extraction efficiency were studied, including sample flow rate, adsorption cycle, salt concentration, pH of sample solution, the type and volume of desorption solvent. The selectivity of the adsorbent membrane C/NiS/NiF to NDZs was evaluated, and the interactions existing between the modified materials on Ni foam and NDZs were examined to probe the possible adsorption mechanism. Under the optimal conditions, the proposed method showed good linearity from 0.05 to 200 µg L and possessed low limits of detection within 0.01-0.05 µg L. The reproducibility and reusability of the C/NiS/NiF adsorbent were investigated, and the effective enrichment and determination of NDZs in water, milk, and honey samples were also carried out with recoveries of 79.3%-114.5%. This study provides a new strategy for the enrichment and determination of some NDZs in different samples.
Integrated Approach for Separation of 2-O-β-D-glucopyranosyl-L-ascorbic Acid From Lycium barbarum L. Fruit Using High-Speed Countercurrent Chromatography Coupled With Aqueous Two-Phase System.
Chen Y, Zhang H, Ma L … +5 more , Wang X, Yang J, Wang N, Pei D, Di D
J Sep Sci · 2026 Jan · PMID 41606432 · Publisher ↗
2-O-β-D-glucopyranosyl-L-ascorbic acid (AA-2βG), a natural ascorbic acid derivative discovered in Lycium barbarum L., has been demonstrated to exhibit multiple biological activities. This study developed an integrated ap...
2-O-β-D-glucopyranosyl-L-ascorbic acid (AA-2βG), a natural ascorbic acid derivative discovered in Lycium barbarum L., has been demonstrated to exhibit multiple biological activities. This study developed an integrated approach combining high-speed counter-current chromatography (HSCCC) and an aqueous two-phase system (ATPS) for the preparative isolation of AA-2βG from L. barbarum fruit. The solution system of ammonium sulfate/ethanol/water/acetonitrile (19.5:28.9:53.3:2.0, w/w) was established through systematic screening processes. To address the multi-parameter optimization challenges in HSCCC, this study employed the entropy weight method to calculate the information entropy and weight coefficients of five critical parameters, thereby establishing a comprehensive evaluation methodology for HSCCC separation efficiency. Subsequently, the response surface methodology was utilized to optimize HSCCC operational conditions. Under the optimized conditions, 2.66 mg of AA-2βG with a purity of 91.24% was successfully isolated from a 140 mg extract. Building on the optimized HSCCC conditions, an overlapping injection mode was implemented based on the conventional single-injection mode. Through cumulative purification of 700 mg extract, 10.65 mg of AA-2βG with an 84.53% purity was successfully obtained. Compared with the single-injection mode, this mode reduced separation time by 55.68% while decreasing solvent consumption by 36.22%. Finally, the antioxidant activity of AA-2βG was assessed through in vitro antioxidant activity experiments. These results demonstrate the synergistic potential of the HSCCC-ATPS integration as an efficient strategy for bioactive compound purification. The established protocol provides a robust method for AA-2βG preparation from Lycium barbarum L. fruit. Furthermore, it demonstrates the broader applicability of this hybrid technique in isolating bioactive constituents from complex biological matrices.
Quantitative Identification of Hydrolysis Products of Mustards by Novel Acetylation Method and Liquid Chromatography-High Resolution Mass Spectrometric Analysis.
Maloth RK, Maddala N, Venkata SLV … +3 more , Kanakala SSD, Ganji SK, Upadhyayula V
J Sep Sci · 2026 Jan · PMID 41606431 · Publisher ↗
A novel derivatization method was developed for the analysis of hydroxy degradation products of the Chemical Weapons Convention (CWC)-related chemicals present in aqueous and soil samples. The analytes were acetylated wi...
A novel derivatization method was developed for the analysis of hydroxy degradation products of the Chemical Weapons Convention (CWC)-related chemicals present in aqueous and soil samples. The analytes were acetylated with acetyl chloride and quantitatively identified by liquid chromatography-tandem mass spectrometry technique in electrospray ionization and atmospheric pressure chemical ionization modes. The acetylated products showed good separation and peak shapes with characteristic fragmentation. The developed method was validated, and the results showed linearity in the range of 1-5000 ng/mL quantities from aqueous and soil samples. The intraday and interday validation results show the deviation of less than 10% with greater than 90% recovery. The limit of detection and limit of quantification of the method, measured at a signal-to-noise ratio of 3:1 and 10:1, respectively, are in the range of 1-20 ng/mL. The developed method was applied to the analysis of samples given in the 56th and 57th official proficiency tests conducted by the Organization for the Prohibition of Chemical Weapons (OPCW), and the chemicals were successfully identified by the developed method.
Screening Potential Anti-Respiratory Syncytial Virus Substances From Forsythia suspensa Using a High-Expressing Fusion Protein Cell Membrane Chromatography.
Liu Y, Gao C, Li S … +2 more , Gao J, Wang N
J Sep Sci · 2026 Jan · PMID 41578427 · Publisher ↗
Respiratory syncytial virus (RSV) imposes a substantial health burden, particularly among pediatric and elderly populations. The RSV fusion (F) protein, a critical mediator of viral entry and syncytium formation, repres...
Respiratory syncytial virus (RSV) imposes a substantial health burden, particularly among pediatric and elderly populations. The RSV fusion (F) protein, a critical mediator of viral entry and syncytium formation, represents a promising and rational target for antiviral drug development. Forsythia suspensa (Lianqiao in Chinese), a traditional Chinese medicinal herb, has been empirically employed for decades in the prevention of viral infections; however, its pharmacologically active constituents remain poorly characterized. The present investigation developed a high-expression F protein cell membrane chromatography system, and integrated with UHPLC-MS, to screen pharmacological substances from FS and verified the anti-viral potential against RSV in vivo. Our study pinpointed Forsythoside A, Forsythoside B, Phillygenin, and Phillyrin as potential anti-RSV compounds in FS. The research findings suggest that Forsythoside A, Forsythoside B, and Phillygenin exhibit considerable suppressive effects on cell fusion induced by RSV, concurrently effectively diminishing the expression level of the F protein gene. In contrast, the inhibitory impact of Phillyrin seems relatively less potent. In conclusion, our findings provide a convenient, fast, and accurate method to screen potential anti-RSV ingredients in natural herbal medicines. These results may facilitate the development of RSV treatment.
Combining Fractionation and High-Resolution Mass Spectrometry Approaches to Characterize a Bio-Oil From Flax Shive Pyrolysis.
Imhoff T, Devaux J, Deschamps E … +5 more , Vievard J, Brandão PF, Afonso C, Duarte RMBO, Mignot M
J Sep Sci · 2026 Jan · PMID 41566680 · Publisher ↗
In a context where environmental concerns and circular economy drive innovation, co-products from the flax industry emerge as valuable lignocellulosic feedstocks. Pyrolysis of these biomasses generates bio-oils with comp...
In a context where environmental concerns and circular economy drive innovation, co-products from the flax industry emerge as valuable lignocellulosic feedstocks. Pyrolysis of these biomasses generates bio-oils with complex and highly oxygenated composition, which requires in-depth molecular characterization to optimize valorization processes. This study focuses on the molecular-level characterization of bio-oil derived from flax shives, a local co-product in Normandy. Size-exclusion chromatography (SEC) was used to fractionate the bio-oil into five distinct fractions based on apparent molecular size. The complete bio-oil and each SEC fraction were then analyzed by high-resolution mass spectrometry (Fourier-transform ion cyclotron resonance [FT-ICR MS] and Orbitrap MS) to identify and compare thousands of molecular formulae. A custom Python-based workflow was developed to align and annotate Orbitrap MS data using the FT-ICR MS dataset as a reference, allowing for rapid molecular formula assignment. Chemical class distribution, oxygen content, and Van Krevelen analysis revealed specific trends across fractions, indicating that SEC separation was influenced not only by molecular size but also by polarity and structural interactions. This approach offers a refined strategy for exploring the chemical complexity of lignocellulosic bio-oils and supports future efforts in their upgrading and application.
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