J Sep Sci [JOURNAL]
Sun
200 papers
Stick-Core-Shell Magnetic Dummy Molecularly Imprinted Polymers for the Determination of Aspartame in Food Sample.
Yao B, Huang L, Li C … +7 more , Cheng L, Zhao C, Chen Z, Wang A, Qin D, Bai S, Gao L
J Sep Sci · 2025 Nov · PMID 41204639 · Publisher ↗
Trace detection of aspartame molecules is crucial for the safety management of additives in food. We developed a convenient synthetic method to prepare magnetic dummy molecularly imprinted polymers, innovatively using ca...
Trace detection of aspartame molecules is crucial for the safety management of additives in food. We developed a convenient synthetic method to prepare magnetic dummy molecularly imprinted polymers, innovatively using carbon nanotubes as the stick carrier of the adsorptive material, which can not only improve the physicochemical stability of the material, but also allow the magnetic microsphere core to disperse due to the presence of carbon nanotubes, thereby enhancing the adsorption performance of the material. Molecularly imprinted polymers were fixed as the shell on magnetic carbon nanotubes to improve the adsorption capacity of the adsorptive material for aspartame molecules. Aspartame in food was enriched by the developed magnetic solid-phase extraction method, followed by detection using LC-MS/MS. Meanwhile, the adsorption mechanism of aspartame by magnetic dummy molecularly imprinted polymers was discussed. Due to its strong selectivity and molecular recognition ability for aspartame, an ultra-low limit of detection was achieved after treatment with magnetic dummy molecularly imprinted polymers using the magnetic solid-phase extraction method, with a detection limit of 0.001 ng/g. This adsorption material can be reused five times. The developed method showed high applicability in detecting aspartame in various different food samples on the market, indicating that the method can be used for real samples to achieve trace detection of aspartame in food.
Preparation of Magnetic Poly(N-Isopropylacrylamide-4-Vinylphenylboronic Acid) Thermosensitive Microcryogel for Immunoglobulin G Purification.
Çimen D, Yılmaz F, Denizli A
J Sep Sci · 2025 Nov · PMID 41199502 · Publisher ↗
In this study, poly(N-isopropylacrylamide-4-vinylphenylboronic acid) thermosensitive microcryogels with different magnetic amounts were prepared for immunoglobulin G (IgG) purification. After, the prepared magnetic therm...
In this study, poly(N-isopropylacrylamide-4-vinylphenylboronic acid) thermosensitive microcryogels with different magnetic amounts were prepared for immunoglobulin G (IgG) purification. After, the prepared magnetic thermosensitive microcryogels were characterized by scanning electron microscopy, Fourier transform infrared attenuated total reflectance spectroscopy, electron spin resonance spectrometer, and optical microscopy. IgG binding capacities were investigated using aqueous IgG solutions prepared at varying concentrations. The maximum IgG binding capacity of poly(N-isopropylacrylamide-4-vinylphenylboronic acid) thermosensitive microcryogels prepared with different magnetic amounts was calculated as 137 mg/g for microcryogels containing 23.0 mg FeO, 72.0 mg/g for microcryogels containing 11.5 mg FeO, 48.6 mg/g for microcryogels containing 5.62 mg FeO, and 39.2 mg/g for microcryogels without FeO at pH 7.4 phosphate solution and 40°C. It was observed that poly(N-isopropylacrylamide-4-vinylphenylboronic acid) thermosensitive microcryogels can be reused ten times. According to the adsorption results, the adsorption of IgG onto the prepared magnetic poly(N-isopropylacrylamide-4-vinylphenylboronic acid) thermosensitive microcryogels fits the Langmuir isotherm model (Q: 147 mg/g, R: 0.9976). After optimizing the experimental conditions, the purity of the eluted IgG was confirmed by sodium dodecyl sulfate polyacrylamide gel electrophoresis. The developed microcryogels combine thermoreactivity with magnetic properties for efficient IgG purification, offering tunable binding capacities using boronic acid-based affinity.
Impact of Host Cell DNA and Chromatin on Virus-like Particle Analysis by Light Scattering in Asymmetrical Flow Field-flow Fractionation.
Bacher J, Jakob LA, Mesurado T … +4 more , Lali N, Zollner A, Jungbauer A, Pereira Aguilar P
J Sep Sci · 2025 Nov · PMID 41172063 · Full text
The development of virus-like particle (VLP) production processes is often constrained by the extensive number of analytical methods required for their quantification and characterization, as well as the significant labo...
The development of virus-like particle (VLP) production processes is often constrained by the extensive number of analytical methods required for their quantification and characterization, as well as the significant labor demands associated with these techniques. Asymmetrical flow field-flow fractionation (AF4) coupled with in-line detectors, such as ultraviolet (UV) and multi-angle light scattering (MALS), presents a promising label-free and rapid approach to simultaneously assess the quantity and quality of VLP samples. While AF4-MALS has been widely applied for bionanoparticle characterization and quantification in final products and process development, the influence of host cell-derived impurities on the outcome of the analysis remains underexplored. This study investigates the impact of host cell-derived impurities, particularly host cell DNA and chromatin, on AF4-MALS-DLS analysis of both unpurified and purified VLP samples, using HIV-1 gag VLPs produced in CHO cells as a model system. Our results demonstrate that DNA, chromatin, and VLPs can co-elute due to their overlapping size distribution, which, if overlooked, may lead to imprecise determination of VLP concentrations in early process samples and inaccurate yield calculations at later stages. Nevertheless, for total particle quantification, AF4-MALS was shown to be a suitable surrogate for nanoparticle tracking analysis, as the 90° light scattering peak area exhibited a strong linear correlation with total particle concentration. This substitution enables faster sample processing and reduces sample volume requirements. Additionally, our findings highlight the importance of particle concentration and method parameter selection, particularly the detector flow rate, when characterizing samples based on hydrodynamic radius (R). Underestimation of R due to high detector flow rates was proposed as the possible explanation for the higher-than-expected shape factors obtained for VLPs. These results emphasize the need for further optimization of AF4 methods to improve the separation of VLPs from host cell impurities and to ensure reliable characterization of bionanoparticles in complex mixtures.
Cell Metabolomics Reveals the Hepatotoxic Mechanism of Copper in Normal Rat Liver Cells Using Reversed-Phase and Hydrophilic Interaction Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry.
Liu P, Zhang S, Jiang Y … +4 more , Wu H, Cao S, Wu H, Zhou A
J Sep Sci · 2025 Nov · PMID 41172059 · Publisher ↗
Copper (Cu) is an essential trace element for maintaining normal cellular functions; however, excessive Cu accumulation has been confirmed to induce hepatotoxicity, while the metabolic mechanisms underlying Cu-induced he...
Copper (Cu) is an essential trace element for maintaining normal cellular functions; however, excessive Cu accumulation has been confirmed to induce hepatotoxicity, while the metabolic mechanisms underlying Cu-induced hepatotoxicity remain unclear. In this study, an innovative integrated separation strategy was established, combining hydrophilic interaction liquid chromatography (HILIC) and reversed-phase liquid chromatography (RPLC), coupled with quadrupole-time-of-flight mass spectrometry (Q-TOF/MS), to systematically resolve metabolomic perturbations in CuCl-exposed rat BRL-3A hepatocytes. Based on their complementary separation mechanisms-HILIC enables efficient retention and separation of polar metabolites via hydrophilic interactions, while RPLC separates nonpolar/weakly polar lipid molecules based on hydrophobic interactions-this analytical strategy significantly expanded the coverage of detectable metabolites and improved the reliability of metabolite identification through cross-validation between the two chromatographic platforms. The results showed that a total of 25 metabolites with significant changes were identified when BRL-3A cells were exposed to 50 µM CuCl (with a cell viability of 85%). These changes were mainly enriched in metabolic pathways such as glutathione metabolism (characterized by a significant decrease in the GSH/GSSG ratio, p < 0.01), arachidonic acid (AA) metabolism (a 42% reduction in AA, p < 0.05), and glycerophospholipid metabolism (a 1.8-fold increase in the levels of lysophospholipids [LysoPCs/LysoPEs], p < 0.05). These findings reveal that oxidative stress, membrane structure damage, and energy metabolism imbalance are the core mechanisms of Cu-induced hepatotoxicity. The integrated liquid chromatography-mass spectrometry (LC-MS) analytical framework established in this study not only provides a novel molecular perspective for elucidating the mechanisms of Cu-induced hepatotoxicity but also demonstrates the application potential of advanced complementary separation technologies in the risk assessment of environmental pollutants.
A Review of LC-NMR Methods and Applications for Pharmaceutical and Natural Product Analysis.
Menard NRC, Schug KA
J Sep Sci · 2025 Nov · PMID 41172058 · Publisher ↗
The separation and identification of components in complex mixtures is a requirement for any aspect of modern chemistry. The hyphenated technique of liquid chromatography (LC)-nuclear magnetic resonance spectroscopy (NMR...
The separation and identification of components in complex mixtures is a requirement for any aspect of modern chemistry. The hyphenated technique of liquid chromatography (LC)-nuclear magnetic resonance spectroscopy (NMR) allows the combination of the separation capabilities of a liquid chromatograph with the structure elucidation capabilities of NMR. As this technique has developed, many approaches have been implemented, and this review aims to discuss these while addressing some of the practical considerations. An examination of the supporting strategies for LC-NMR is discussed, such as the development of solvent suppression methods, the design of more specialized NMR cells, or further hyphenation to other instrumentation such as a mass spectrometer. A sampling of relevant pharmaceutical and natural product applications is discussed that serve to highlight the utility of this technique and its relevancy and current status in the field.
Sensitive Profiling of Human Milk Oligosaccharides in Human Colostrum and Breast Milk by Capillary Electrophoresis-Mass Spectrometry.
Smolkova D, Rusin M, Dobrowolska-Iwanek J … +2 more , Woźniakiewicz M, Lavicka J
J Sep Sci · 2025 Nov · PMID 41171001 · Full text
Human milk oligosaccharides are pivotal for shaping the infant gut microbiome and immune development, yet their structural diversity hampers routine identification and quantification. We report an optimized capillary ele...
Human milk oligosaccharides are pivotal for shaping the infant gut microbiome and immune development, yet their structural diversity hampers routine identification and quantification. We report an optimized capillary electrophoresis-mass spectrometry workflow that enables sensitive, isomer‑selective profiling of 10 biologically relevant human milk oligosaccharides in colostrum and early‑lactation breast milk. Human milk oligosaccharides were first neutralized to stabilize sialic acids and derivatized with Girard's reagent P, introducing a permanent positive charge to enhance electrophoretic resolution and electrospray ionization efficiency. Separation in a linear‑polyacrylamide‑coated capillary (0.25 M formic acid, 30 kV) and mass spectrometry detection with a nanoCEasy interface achieved baseline resolution of all targets except positional isomers lacto-N-difucohexaose I/II. Incorporation of Girard's reagent P‑labeled maltoheptaose as an internal standard improved migration time precision to < 0.5% RSD and reduced peak‑area repeatability to 9%-25% RSD. Limits of detection were 0.8-290 ng/mL, corresponding to fg-pg on‑column amounts and outperforming precedent APTS-based CE/LIF methodologies. Application to colostrum and milk samples from a single donor (1-3 months postpartum) revealed pronounced variation. Colostrum was dominated by 2'‑fucosyllactose and fucosylated lacto-N-fucopentaose isomers, whereas sialylated human milk oligosaccharides were present in smaller amounts. Longitudinally, 2'‑fucosyllactose remained the most abundant species, while lacto-N-fucopentaose and lacto-N-neotetraose/lacto-N-tetraose diminished markedly by Month 3. The presented capillary electrophoresis-mass spectrometry platform delivers reasonably fast (< 70 min), high‑sensitivity human milk oligosaccharide fingerprinting from minimal sample volumes and is readily adaptable to large‑cohort studies, offering new opportunities to elucidate the nutritional dynamics of the maternal milk glycome during lactation.
Unmasking the Thermodynamic Void Volume in the Minor-Disturbance Method: Clarifying Its Physical Meaning and Relation to the Geometrical Void.
Tsui HW, Dai FJ, Yang CC
J Sep Sci · 2025 Oct · PMID 41159295 · Publisher ↗
The minor-disturbance method is a convenient route to adsorption isotherms, but the thermodynamic void volume extracted from its data is often taken-sometimes uncritically-to be the column's geometrical void. Here, we in...
The minor-disturbance method is a convenient route to adsorption isotherms, but the thermodynamic void volume extracted from its data is often taken-sometimes uncritically-to be the column's geometrical void. Here, we investigate the thermodynamic void volume using an adsorption-dividing-plane framework. This framework clarifies that the choice of any hold-up volume implicitly defines a Gibbs-like dividing surface, which in turn determines the thermodynamic meaning of the resulting isotherm. Experiments were performed on two contrasting media: a cyano-silica normal phase with C-C alcohols and acetone, and an octyl-bonded reversed phase with acetonitrile, methanol, and acetone, each probed at 15 or more bulk concentrations. On the cyano column, all solutes yielded an identical thermodynamic void volume (≈2.98 mL), indicating the dividing plane aligns with the silica surface and the resulting isotherms represent true surface excess. In contrast, the thermodynamic void volume on the octyl-bonded column was solute-dependent (acetonitrile > acetone > methanol), reflecting probe-specific penetration into the bonded phase rather than the physical void volume. Negative branches observed in the high-concentration excess isotherms of acetonitrile and acetone are rationalized by a conceptual three-zone concentration profile in which brush-induced depletion exceeds interfacial adsorption. Reprocessing the reversed-phase data with a single, fixed void volume shifted the excess isotherms as predicted while leaving the total-uptake isotherms unchanged, demonstrating that total adsorption is independent of the definition of the excess dividing plane when the saturation point is used to define the dividing surface. The study clarifies the physical meaning of the thermodynamic void volume: it equals the geometrical void only for phases with negligible bonded layers, but becomes probe-specific on densely bonded reversed-phase materials, where it serves as a quantitative indicator of brush penetration. A fixed dividing plane is therefore essential for meaningful cross-solute comparison of excess isotherms and for reliable interpretation of minor-disturbance data.
Comparative Study on Chiral Separation of Afoxolaner on Polysaccharide-Based Chiral Stationary Phases by Supercritical Fluid Chromatography and High-Performance Liquid Chromatography.
Xia C, Zhu R, Fan YX … +4 more , Lin JS, Xu GP, Zhang WG, Fan J
J Sep Sci · 2025 Oct · PMID 41159220 · Publisher ↗
Supercritical fluid chromatography (SFC)-based chiral separation has been considered as one of the green, highly efficient, and precise methods for the resolution of new chiral pharmaceuticals. Herein, a comparative stud...
Supercritical fluid chromatography (SFC)-based chiral separation has been considered as one of the green, highly efficient, and precise methods for the resolution of new chiral pharmaceuticals. Herein, a comparative study of chiral separation of afoxolaner on polysaccharide-based chiral stationary phases (CSPs) by SFC and high-performance liquid chromatography (HPLC) has been conducted. First, effects of chromatographic conditions on chiral separation of afoxolaner by SFC, including CSPs, modifier types and ratios, flow rate, column temperature, and back pressure, have been discussed in detail. Cellulose tris(4-methylbenzoate)-coated CSP demonstrated the best separation performance for afoxolaner by SFC with the resolution of 2.37 among five CSPs. Afoxolaner enantiomers were eluted at 3.53 min and 4.54 min under the optimized SFC conditions, respectively, and the total analysis time was less than 6 min, much shorter than that by HPLC. Subsequently, molecular docking studies revealed that hydrogen bonds and halogen bonds formed by afoxolaner and CSPs dominated the selective interaction for the separation of afoxolaner. Additionally, hydrophobic effects and π-π stacks between afoxolaner and chiral selectors enhanced the resolution of afoxolaner. Moreover, quantitative determination results of afoxolaner by SFC showed good linearity relationships (R > 0.999) between concentration of enantiomers and the corresponding chromatographic peak area in the range from 0.025 to 0.800 mg/mL, and the limit of quantification of enantiomers was 0.025 mg/mL. In brief, SFC separation would offer a green alternative to overcome potential technical bottlenecks in the resolution of new chiral pharmaceuticals.
Development of a Direct Sampling Module for Compact Capillary Liquid Chromatography.
Doupsas N, Morse M, Powell M … +8 more , Alimuddin M, Braganza J, Elleraas J, Wang W, Yanovsky A, Lee ML, Richardson PF, Grinias JP
J Sep Sci · 2025 Oct · PMID 41159212 · Full text
The automation of reaction monitoring analysis can greatly improve the capability to obtain real-time feedback on reaction progress and aid in method optimization. Liquid chromatography (LC) is a widely used analytical t...
The automation of reaction monitoring analysis can greatly improve the capability to obtain real-time feedback on reaction progress and aid in method optimization. Liquid chromatography (LC) is a widely used analytical technique for organic reaction monitoring, but the large size of the instrumentation can make online analysis difficult and impractical. Compact and miniaturized LC instrumentation provides the opportunity to simplify the process of analyzing samples at the reaction site, but the smaller scale of capillary LC columns is often incompatible with commercial reaction sampling systems designed to work with larger volumes. Here, a compact sampling module (CSM) designed to automate sample collection from a variety of reaction devices with volumes that are compatible with capillary LC is reported. The design and operation of the system are described, as well as example uses within a conventional medicinal chemistry setting. Specifically, the real-time analysis of both standard reactions in flow and batch settings with sampling performed by the CSM is described. Furthermore, the utility of the module in analyzing photoredox-based reactions, which are currently experiencing significant growth within drug discovery, is described. Performance of the system is compared to a traditional benchtop LC instrument that is currently used as the primary platform for standard reaction analysis, with a repeatability comparison between the systems demonstrating averages of 0.8%RSD (percentage relative standard deviation) for retention time and 2.5%RSD for peak area on the compact system and 1.4 and 9.4%RSD, respectively, for the benchtop system. The average observed carryover using the compact LC with CSM was also lower than the benchtop LC (0.3% and 1.5%, respectively), although detection limits were higher due to the shorter pathlength on-column ultraviolet-absorbance flow cell used in this work.
Countercurrent Separations as Effective Purification Techniques for Iridoids.
Ramos-de-la-Peña AM, Guimarães Leitão G, Méndez-Merino E … +1 more , Contreras-Esquivel JC
J Sep Sci · 2025 Oct · PMID 41147422 · Publisher ↗
Countercurrent separation (CCS) is a powerful technique for natural products purification in which the components of the sample are partitioned between two immiscible liquids. Iridoids are natural compounds with remarkab...
Countercurrent separation (CCS) is a powerful technique for natural products purification in which the components of the sample are partitioned between two immiscible liquids. Iridoids are natural compounds with remarkable biological and pharmacological activities that have been purified by CCS, with high potential to be scaled up. This review provides CCS fundamentals, a critical consideration of existing studies focused on iridoid purification, and elucidating factors that can improve the processing, such as solvent system selection, processing parameters, and sample pretreatment, which are highly relevant for separation. This review highlights the use of CCS in the purification of iridoids, providing fundamental insights to better understand the CCS technique's contribution to purification improvement. By identifying the process key parameters and addressing issues, the implementation on an industrial scale of CCS for iridoid recovery could be facilitated, with high potential in the food, pharmaceutical, and cosmetic fields.
Synthesis of Magnetic Azo-Linked Covalent Organic Polymer for Rapid Extraction of β-Agonists in Swine Urine Samples.
Liao Q, Xiang J, Yuan L … +1 more , Zhang D
J Sep Sci · 2025 Oct · PMID 41126580 · Publisher ↗
The illegal use of β-agonists as feed additives can harm animal-derived food safety. In this study, a detection method for β-agonists in swine urine was established by the combination of azo-linked covalent organic polym...
The illegal use of β-agonists as feed additives can harm animal-derived food safety. In this study, a detection method for β-agonists in swine urine was established by the combination of azo-linked covalent organic polymer-miniaturized magnetic solid-phase extraction. The main factors that affect the extraction procedure were optimized. The designed adsorbent had good reusability, reproducibility, and stability. Under optimal conditions, the method achieved a good linear correlation coefficient (> 0.99) and a low detection limit (0.01 µg/L). The recoveries of the proposed method in swine urine samples for the simultaneous determination of β-agonists were in the range of 84.3%-99.4%, and the relative standard deviations were less than 6.5%.
Bioanalytical Uncertainty Assessment of Ultra-High-Performance Liquid Chromatography-High Resolution Mass Spectrometry Method for Caffeine and Lidocaine in Equine Antidoping: A Dual Perspective on Bottom-up and Top-Down Approaches.
El-Ghaly W, El Kamli T, Zaari Lambarki L … +7 more , El Hamdani M, Lahkak FE, Benmoussa A, Balouch L, Bakkali F, Saffaj T, Jhilal F
J Sep Sci · 2025 Oct · PMID 41126565 · Publisher ↗
The quality of quantitative results in bioanalysis requires not only a validated analytical method but also a rigorous estimation of measurement uncertainty. This study examines the challenges associated with the impleme...
The quality of quantitative results in bioanalysis requires not only a validated analytical method but also a rigorous estimation of measurement uncertainty. This study examines the challenges associated with the implementation of two distinct approaches in equine anti-doping control for the assessment of uncertainty associated with an ultra-high-performance liquid chromatography-high resolution mass spectrometry quantitative method for caffeine and lidocaine in horse urine. The bottom-up approach, based on the ISO Guide to the Expression of Uncertainty in Measurement (ISO GUM), was compared to the top-down approach using β-content, γ-confidence tolerance intervals (β,γ-CCTI) via F-test. The key limitation of the ISO GUM method was accurately quantifying the various uncertainty components; it gives standardized uncertainty estimates but requires detailed assumptions and modeling about error sources. The direct application of the GUM method imposes the beforehand correction of the matrix effect to provide reliable results. Parallelly, the chemometric approach β,γ-CCTI offers more flexible and realistic estimations. Four combinations of β and γ were investigated to assess their influence on uncertainty interval width: β = 66.7% and 80%; γ = 90% and 95%; and the method was evaluated under repeatability and intermediate precision conditions through the use of advanced computation that adjusts for matrix effects and proves more straightforward for capturing variability inherent in experimental data. The top-down approach is a reliable alternative for routine use and, particularly, for ensuring compliance with regulatory requirements, with the fact that a known proportion β of future results will be within predefined acceptance limits.
Enrichment of Kaempferol-3-O-Sophoroside From Saffron Petals Using Macroporous Resin: Static Adsorption Characteristics and Dynamic Optimization Based on Analytical Hierarchy Process-Entropy Weight Method-Response Surface Methodology.
Huo X, Wang L, Li L … +7 more , Zhu W, Xu Q, Zhao X, Yin X, Wu L, Zhou Y, Huang J
J Sep Sci · 2025 Oct · PMID 41124108 · Publisher ↗
An efficient strategy was developed for the enrichment of kaempferol-3-O-sophoroside from saffron petal extract. The macroporous resin of XAD-1600N was selected due to its highest adsorption and desorption capacities for...
An efficient strategy was developed for the enrichment of kaempferol-3-O-sophoroside from saffron petal extract. The macroporous resin of XAD-1600N was selected due to its highest adsorption and desorption capacities for kaempferol-3-O-sophoroside. Static adsorption characteristics and dynamic enrichment parameters of this resin were systematically investigated through scientific experiments and analysis. The adsorption characteristics were found to be in good agreement with the pseudo-second-order model, as well as the Freundlich and Langmuir models. The thermodynamics analysis exhibited that this adsorption process was a spontaneous exothermic reaction. Furthermore, the dynamic enrichment for kaempferol-3-O-sophoroside was optimized using a combination of analytical hierarchy process-entropy weight method-response surface methodology, and the comprehensive scores based on desorption rate, recovery rate, and purity. The recommended operation parameters included sample loading rates (2.3-3.7 BV/h), ethanol concentrations (49%-69%), and elution flow rates (1-3 BV/h). After the enrichment process, the purity of kaempferol-3-O-sophoroside from saffron petals extract increased over fivefold after enrichment with acceptable recovery. It is anticipated that this study will contribute to the large-scale development and utilization of kaempferol-3-O-sophoroside from the saffron petals, thereby providing a theoretical basis for natural products enrichment.
Revealing the Formula Pattern of Congming Decoction by Ultra-High-Performance Liquid Chromatography Coupled With Quadrupole-Orbitrap Mass Spectrometry From the Perspective of Chemical Constituents, In Vitro, and In Vivo Properties.
Tang S, Wu Y, Wang R … +8 more , Li Y, Li J, Peng Y, Liu S, Men L, Hou Z, Liu Z, Liu Z
J Sep Sci · 2025 Oct · PMID 41122827 · Publisher ↗
The Congming decoction (CMD) is a classic traditional Chinese medicine formula, composed of Poria cocos (Schw.) Wolf, Polygalae Radix, and Acori Tatarinowii Rhizoma. The material basis for the rationality of CMD's compat...
The Congming decoction (CMD) is a classic traditional Chinese medicine formula, composed of Poria cocos (Schw.) Wolf, Polygalae Radix, and Acori Tatarinowii Rhizoma. The material basis for the rationality of CMD's compatibility remains unclear in both in vitro and in vivo studies. The relationship between its components and therapeutic efficacy still presents a research gap. Therefore, this study aims to reveal the co-extraction dissolution patterns, metabolic regularity in vitro, and absorption and distribution characteristics in vivo of CMD, thereby exploring the scientific connotation of formulation. Utilizing ultra-high-performance liquid chromatography coupled with quadrupole-orbitrap mass spectrometry technology, a total of 183 constituents were identified in CMD, with 72 recognized as differential compounds before and after combination, suggesting that co-boiling enhances the solubility of active ingredients. In vitro intestinal microbiota results indicated that combination reduced metabolism rates, allowing for greater absorption as the prototype. In vivo analysis identified 62 constituents within rat plasma and tissues; comparing content differences among groups found that the combinations regulate hepatic metabolism and enhance distribution of effective components, potentially serving as a significant material basis for treating Alzheimer's disease (AD). Furthermore, a targeted network pharmacology strategy was established to explore the mechanism of CMD in treating AD. This study clarified the chemical composition, metabolic patterns in vitro, and distribution rules in vivo regarding CMD, and also compared variations before and after composition. It provided new insights into the rationality of CMD's compatibility in the treatment of AD from multiple dimensions and levels.
Qualitative and Quantitative Comparisons on the Chemical Constituents in the Stems of Acanthopanax senticosus and A. sessiliflorus by Liquid Chromatography Combined With Multi-detectors.
Liang HZ, Huang CL, Lai CC … +7 more , Wang MY, Yu DX, Chen XJ, Song J, Gao Y, Guo BL, Ma BP
J Sep Sci · 2025 Oct · PMID 41088501 · Publisher ↗
Acanthopanax senticosus Harms (ASH) is widely used in traditional Chinese medicine for its beneficial properties; however, its related species, A. sessiliflorus Seem (ASS), has emerged as a market substitute due to decli...
Acanthopanax senticosus Harms (ASH) is widely used in traditional Chinese medicine for its beneficial properties; however, its related species, A. sessiliflorus Seem (ASS), has emerged as a market substitute due to declining ASH resources. To systematically compare the chemical constituents in the stems of two plants, a multi-detector analytical approach was developed in the present study by combining ultra-/high performance liquid chromatography (U-/HPLC) with quadruple time-of-flight mass spectrometry (Q-TOF-MS), ultraviolet detector (UV), and charged aerosol detection (CAD). First, the chemical constituents of ASH and ASS were detected by UHPLC-Q-TOF-MS, and a total of 120 compounds, including phenylpropanoids, triterpenoids, organic acids, etc., were identified. Among them, syringin, the Chinese Pharmacopoeia-designated quality marker for ASH, was determined via HPLC-UV, and it was found that the indicator was present in ASH at a concentration ranging from 0.06% to 0.13%, while ASS showed no detectable levels. Moreover, a semi-quantitative fingerprint method was developed based on UHPLC-CAD for the comparison of multi-component. The results revealed notable variations in the multi-component profiles of the two plants. Furthermore, the established fingerprint method was successfully applied for the differentiation of ASH samples adulterated with ASS. In sum, these findings underscore the significant chemical differences between ASH and ASS, emphasizing the need to prevent ASS adulteration in ASH-derived products.
Investigating a Novel Non-Destructive Identification Technique for Prehistoric Adhesives With Dynamic Headspace Coupled to Comprehensive Two-Dimensional Gas Chromatography-Mass Spectrometry.
Lokker A, Stefanuto PH, Cnuts D … +2 more , Rots V, Focant JF
J Sep Sci · 2025 Oct · PMID 41088499 · Publisher ↗
Adhesives were used by prehistoric humans for attaching a handle to a stone tool, to improve tool use. Remains of these adhesives preserve on stone tools until today. Chemical analysis of these residues is essential for...
Adhesives were used by prehistoric humans for attaching a handle to a stone tool, to improve tool use. Remains of these adhesives preserve on stone tools until today. Chemical analysis of these residues is essential for an improved understanding of how humans exploited their natural environment, stone tool manufacturing and use. However, chemical analysis is not straightforward, the highly degraded residue and the precious artefacts impose limitation. In this study a novel (semi-) non-destructive identification technique for prehistoric hafting adhesives is reported; dynamic headspace sampling coupled to comprehensive two-dimensional GC-MS. The dynamic sampling results in a full characterization of the volatile profile of the adhesives. A major advantage is that the whole stone tool, with the adhering adhesive, can be analyzed. Moreover, good results are obtained using only slightly elevated temperatures, which avoids heat damage to the stone tools. Nonetheless, the established biomarkers for prehistoric adhesives are not extracted with this method. Therefore, a non-targeted analytical approach combined with multivariate analysis is utilized. In this approach, the chromatogram of an unknown sample is compared to a database of known samples. In this study a start of an adhesive database is made with 14 different adhesives divided over 4 adhesive classes. The identification capability of this technique is further evaluated using six experimental stone tools, with different adhesives adhered to them and subjected to UV-induced degradation. The large stone pieces could not fit in the automated sampling station, thus, a manual sampling set-up was build. It was found that the sampling strategy did not affect the volatiles extracted and that comparison with the database was possible. The tar samples were the least affected and could be easily identified while the resin samples were more degraded and identification was difficult. This technique is promising for non-destructive adhesive identification on prehistoric stone tools.
Development of an HPLC-HRMS Method for the Identification and Semi-Quantitation in River Water Samples of the Transformation Products Originated From Heterogeneous Photocatalysis of Antipsychotic Drugs.
De Rosa E, Arpaia S, Michelina SV … +4 more , Oliva F, Medana C, Calza P, Dal Bello F
J Sep Sci · 2025 Oct · PMID 41086034 · Full text
The environmental occurrence of psychiatric drugs is a growing concern due to their widespread use and persistence in aquatic systems. In this study, haloperidol and aripiprazole, two commonly prescribed antipsychotic ag...
The environmental occurrence of psychiatric drugs is a growing concern due to their widespread use and persistence in aquatic systems. In this study, haloperidol and aripiprazole, two commonly prescribed antipsychotic agents, were selected as model compounds to investigate their photocatalytic modification and assess the formation of transformation products (TPs). A high-performance liquid chromatography-high-resolution mass spectrometry (HPLC-HRMS) method was developed for the identification and structural elucidation of TPs generated via TiO-mediated heterogeneous photocatalysis in ultrapure water. Reverse-phase chromatographic separation was achieved using an octadecyl silica column as the stationary phase, with formic acid and acetonitrile as the mobile phase. The total run time of 37 min provided adequate resolution for the separation of the main TPs isomers. TPs annotation was carried out using orbitrap technology, operated at a resolving power of 60 000 for all experiments. Including isomers, a total of 32 haloperidol TPs and 13 aripiprazole TPs were identified, with proposed fragmentation pathways established through targeted MS experiments. The method was then applied to the analysis of real river surface water samples collected from the Po and Sangone Rivers in Northern Italy over a 3-month period. Following solid-phase extraction (SPE), both parent compounds and TPs were recognized and semi-quantified by retention time, exact mass, and MS spectral data. Haloperidol and aripiprazole were detected at maximum concentrations of 27 and 67 ng L, respectively. To assess the potential biological impact, in vitro cytotoxicity tests were conducted on normal (BEAS-2B) and oncogenic (BEAS G12C) human bronchioalveolar epithelial cell lines. Although the parent drugs exhibited negligible toxicity at the tested concentrations, haloperidol TPs induced marked cytotoxic effects in both cell models. These results highlight the necessity of including TPs in environmental monitoring and toxicological assessments.
Direct Determination of Glucosamine and Its Isomers in Pharmaceutical Formulations by Capillary Electrophoresis With Amperometric Detection.
Li D, Liu J, Zheng R … +1 more , Chu Q
J Sep Sci · 2025 Oct · PMID 41086030 · Publisher ↗
The studies have shown that glucosamine (GluN) and mannosamine (ManN) are important nutrients for the formation of chondrocytes, while galactosamine (GalN) is a hepatotoxin with high selectivity. Therefore, the separatio...
The studies have shown that glucosamine (GluN) and mannosamine (ManN) are important nutrients for the formation of chondrocytes, while galactosamine (GalN) is a hepatotoxin with high selectivity. Therefore, the separation and detection of aminosaccharide isomers are of critical significance for pharmaceutical quality monitoring. In this work, a novel method was established for the separation and direct determination of GluN and its isomers (GalN and ManN) based on capillary electrophoresis with amperometric detection. The critical factors affecting electrophoretic separation and electrochemical detection were investigated in detail. Under the optimum conditions, three aminosaccharide isomers and their precursor monosaccharides (glucose, galactose, and mannose) can achieve baseline separation. The limits of detection reached 0.070-0.23 µg/mL (S/N = 3), showing good linearity within two orders of magnitude (R > 0.99), and the recovery data were in the range of 96.0%-107.8%. This developed method has been applied for the analysis of aminosaccharide pharmaceuticals in different dosage forms. This proposed method is simple to operate, requires no derivatization, and is environmentally friendly, providing an alternative method for the direct determination of aminosaccharides in pharmaceutical formulations. Furthermore, the greenness and eco-friendliness of this developed method were assessed by the green analytical procedure index, analytical greenness, and analytical eco-scale tools.
Automated Matrix Dilution Injection Method Utilizing Online Auto-Injection Program for Matrix-Matched Calibration for the LC-MS/MS Analysis of Multiple Pesticide Residues.
Jeong WT, Kim D, Lee SH … +1 more , Noh HH
J Sep Sci · 2025 Oct · PMID 41073369 · Publisher ↗
The introduction of mass spectrometry in the analysis of pesticide residues has significantly enhanced analytical efficiency, reduced analysis times, and enabled ultra-trace detection. However, the matrix effect-wherein...
The introduction of mass spectrometry in the analysis of pesticide residues has significantly enhanced analytical efficiency, reduced analysis times, and enabled ultra-trace detection. However, the matrix effect-wherein target analytes experience interference from the matrix during ionization-remains a critical issue. In multiresidue pesticide analysis via LC-MS/MS, matrix effects are typically addressed by preparing calibration standards through the dilution of matrix extracts with buffers (organic solvents) or by diluting the sample, which must be manually performed by the analyst. This study developed an automated matrix dilution injection (AMDI) method that leverages the autosampler built-in automatic dilution injection feature in liquid chromatography (LC) to prepare matrix-corrected dilutions and quantify analytes without manual manipulation. The AMDI method was validated by analyzing 71 pesticides in four agricultural commodities, where linearity, accuracy, and precision were assessed using two LC systems with different performances (HPLC-MS/MS and UHPLC-MS/MS). The AMDI method exhibited superior linearity in UHPLC analyses compared with conventional matrix-matched calibration standards. Furthermore, most of the pesticides analyzed exhibited measurement accuracies of 70%-120% and precision with relative standard deviations below 10%.
Key Considerations for Sustainable Separations in Countercurrent Chromatography.
Martins GR, da Cruz IL, Freire AAF … +5 more , França MMM, Silva ASD, Hewitson P, Ignatova S, Costa FDN
J Sep Sci · 2025 Oct · PMID 41073367 · Publisher ↗
Countercurrent chromatography (CCC) is a liquid-liquid separation technique in which compounds are separated on the basis of partitioning between two immiscible phases. Besides having inherent advantages-high loading cap...
Countercurrent chromatography (CCC) is a liquid-liquid separation technique in which compounds are separated on the basis of partitioning between two immiscible phases. Besides having inherent advantages-high loading capacity, easy scale-up, and sample recovery with no chemical degradation-that position CCC as an alternative to conventional chromatographic methods, it can also be sustainable, especially when methodologies are optimized, including the use of eco-friendly solvents, high sample loading, and solvent recycling. This review highlights the green potential of CCC by integrating green chemistry principles through low solvent consumption, reduced waste, and the use of bio-based solvents, such as aqueous two-phase solvent systems and deep eutectic solvents, to align CCC with sustainable chromatographic approaches. Moreover, the technique's ability to recycle solvent phases and process crude extracts with minimal sample preparation boosts its environmental benefits. Despite these advantages, several challenges limit the widespread adoption of CCC, particularly in industrial settings. Patent analysis indicates that although CCC is commonly used to purify natural products, its role in sustainability-driven innovations remains relatively limited. The selection of biphasic solvent systems is a critical bottleneck, often requiring extensive experiments, which can result in excessive solvent use. Advances in computational methods have improved the selection of solvent systems, allowing for a more resource-efficient approach. By modeling phase interactions, these computational tools can predict partition coefficients and optimize solvent compositions, consequently reducing experimental waste. Future research should focus on integrating CCC into large-scale sustainable workflows to enhance its environmental viability in natural product chemistry.
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