J Chromatogr A [JOURNAL]
Sun
200 papers
Controllable preparation of honeycomb supermacroporous core-shell SiO coated with cellulose-derivate and investigation of confinement effect on chiral separation performance.
Hu Y, Zhu M, Zhang M … +5 more , Ma S, Tang S, Lyu H, Wei Y, Ou J
J Chromatogr A · 2026 Jul · PMID 42096850 · Publisher ↗
The separation of enantiomers is of significant importance in pharmaceutical production and chemical synthesis. In this work, a novel kind of honeycomb supermacroporous core-shell SiO (HSC-SiO) was controllably synthesiz...
The separation of enantiomers is of significant importance in pharmaceutical production and chemical synthesis. In this work, a novel kind of honeycomb supermacroporous core-shell SiO (HSC-SiO) was controllably synthesized via an etching method. By precisely regulating the amounts of CTAB, ODA, and NHF, a hierarchical pore structure composed of a mesoporous framework and supermacroporous channels was successfully constructed. The optimized material, denoted as HSC-SiO-2, exhibited a specific surface area of 79.2 m·g, an average pore size of 6.1 nm, and a maximum pore size of 136 nm. Chiral stationary phases (CSPs) were prepared by coating cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC) onto the surface of aminofunctionalized HSC-SiO. Evaluation of the separation performance for twelve racemic compounds demonstrated that CSP-2, fabricated from HSC-SiO-2, possessed superior enantioselectivity, achieving baseline separation for eight analytes on a short 100 mm column. Specifically, it achieved an α of 2.75 and an Rs of 5.32 for metoprolol, an Rs of 3.04 for trans-stilbene oxide, and an Rs of 2.21 for benzoin. Comparative tests revealed that its resolution for trans-stilbene oxide was comparable to that of the commercial Chiralcel OD-H column (Rs = 3.01), while its Rs values for metoprolol and benzoin were markedly higher than those of the traditional fully porous silica-based CSP (Rs = 2.25 and 1.38, respectively). The performance enhancement is attributed to the hierarchical pore architecture with a favorable confinement effect, which provides a high surface area for sufficient chiral selector loading while enabling efficient mass transfer through the supermacroporous channels. This research offers a new design strategy for high-performance chiral separation supports, showing promising potential for applications in efficient enantiomer analysis and purification.
High-pressure hydrolysis: A rapid sample preparation strategy for amino acid analysis of complex biological matrices.
Li S, Meng L, Qin Z … +2 more , Zhang X, Gu Y
J Chromatogr A · 2026 Jul · PMID 42096849 · Publisher ↗
The extended acid hydrolysis step (typically 20-24 h) is a pervasive bottleneck in amino acid analysis, particularly for complex, protein-rich biological matrices. To overcome this, we developed and rigorously validated...
The extended acid hydrolysis step (typically 20-24 h) is a pervasive bottleneck in amino acid analysis, particularly for complex, protein-rich biological matrices. To overcome this, we developed and rigorously validated a novel high-pressure hydrolysis strategy. Complete protein hydrolysis in a challenging model matrix (Pheretima, a complex animal-derived material) was achieved in only 2 h (120 °C, saturated steam pressure of 0.12 MPa, ∼1.2 atm)-a > 90% reduction in time compared to the conventional approach. Critically, direct comparison with the 24-h gold-standard method confirmed analytical equivalence, with two one-sided t-tests (TOST) confirming equivalence for 15 out of 16 amino acids within the equivalence margin of ±5%. Coupled with a robust phenyl isothiocyanate (PITC) pre-column derivatization HPLC-UV protocol, the method demonstrated excellent performance: specificity, linearity (R > 0.99), precision (RSD < 2.5%), and accuracy (recoveries: 95.1-104.9%). Its practical utility was proven by the rapid generation of consistent chromatographic fingerprints and the revelation of statistically significant, origin-linked variations in key amino acids (e.g., proline, tyrosine, phenylalanine) from 13 sample batches. This work provides a significant advancement in sample preparation, offering a fast, reliable, and broadly applicable solution that can transform throughput in the amino acid profiling of complex biological materials.
High-performance countercurrent chromatography isolation of flavonoids from a cytotoxic extract of Andira parviflora (Ducke) waste wood from the Amazon region.
de Araújo IM, Flores SLG, Leitão GG … +9 more , Bright C, Pereira JVM, Guimarães CJ, Pessoa CDÓ, da Silva YC, Veiga Junior VFD, da Silva FMA, Hatori RT, Guimarães AC
J Chromatogr A · 2026 Jul · PMID 42096848 · Publisher ↗
Andira parviflora Ducke (Fabaceae), known as "sucupira vermelha", is mainly found in dryland forests of the Amazon region. Due to its large size and dense wood, the timber industry widely uses the species. Nevertheless,...
Andira parviflora Ducke (Fabaceae), known as "sucupira vermelha", is mainly found in dryland forests of the Amazon region. Due to its large size and dense wood, the timber industry widely uses the species. Nevertheless, there are few studies about the chemical composition of its residues from industrial wood processing. Some pterocarpans and isoflavone derivatives have already been reported in the literature. In this work, we report the isolation of phenolic compounds from the heartwood waste of A. parviflora, using high-performance countercurrent chromatography (HPCCC) associated with high-performance liquid chromatography coupled to ultraviolet spectroscopy (HPLC-UV), applied to the ethyl acetate fraction of its ethanol extract, which showed potential cytotoxic activity. The cytotoxic potential was evaluated against tumor cells astrocytoma, human colon carcinoma, prostate carcinoma, and promyelocytic leukemia cell lines. The purification of 4 g of the ethyl acetate fraction was carried out by reversed-phase HPCCC using a semipreparative 136 mL column and a non-linear step-gradient elution two biphasic solvent systems: hexane-ethyl acetate-methanol-water 1:3:1:3 v/v (step 1) and 1:2:1:2 v/v (step 2), with the aqueous phase of the both systems used as mobile phase. The HPLC-UV purification of fractions 4 and 17 afforded the two dihydrochalcone isomers of coatline A (compounds 1 and 2) from fraction 4, as well as isoliquiritigenin, (3), medicarpin, (4), and biochanin A (5). Compounds 1 and 2 are unprecedented in the species whereas compound 3 is being described for the first time in the genus. The use of preparative HPCCC prior to HPLC purification enabled the separation of three different classes of flavonoids from A. parviflora and simplified the samples before HPLC purification. Moreover, it reduced the overall cost of the process by minimizing solvent consumption, shortening processing time and enhancing sample recovery.
Normalized solvent-strength sensitivity for gradient separations: Comparing effective column lengths across reversed-phase and ion-exchange chromatography.
Fekete S, Vo C, Su WC
J Chromatogr A · 2026 Jul · PMID 42090910 · Publisher ↗
The linear solvent strength (LSS) model provides a robust framework for predicting retention in reversed-phase liquid chromatography (RPLC), but its extension to ion-exchange chromatography (IEX) requires normalization o...
The linear solvent strength (LSS) model provides a robust framework for predicting retention in reversed-phase liquid chromatography (RPLC), but its extension to ion-exchange chromatography (IEX) requires normalization of the solvent-strength coordinate. In this work, we introduce a dimensionless normalization for salt and pH gradients, enabling direct comparison of retention sensitivity across chromatographic modes. We define the universal solvent-strength sensitivity (S) as the product of the slope parameter and the gradient span in its respective coordinate, capturing the total change in retention factor across the gradient. This descriptor allows prediction of effective column length (L) and supports rational design of ultrashort columns for high-throughput separations. Using previously published and new experimental data, we demonstrate the applicability of S to monoclonal antibodies (mAbs), double-stranded DNA fragments, and single-stranded oligonucleotides and mRNA. Overall, the proposed normalization provides a unified approach to retention modeling across gradient modes and biomolecular classes, facilitating method transfer and accelerating analytical workflows.
Magnetic nitrogen-doped porous carbon sorbents derived from NH-MIL-88(Fe) for efficient extraction of chloramphenicol in honey samples.
Tang A, Cao Y, Guo M … +1 more , Lin B
J Chromatogr A · 2026 Jul · PMID 42090909 · Publisher ↗
Magnetic porous carbon (MPC) materials derived from metal-organic frameworks (MOFs) inherit the high porosity and tunable pore structure of MOFs and also endow the materials with magnetic response, demonstrating great po...
Magnetic porous carbon (MPC) materials derived from metal-organic frameworks (MOFs) inherit the high porosity and tunable pore structure of MOFs and also endow the materials with magnetic response, demonstrating great potential for magnetic solid-phase extraction (MSPE). However, MPCs obtained directly by carbonizing MOFs suffer from issues such as easy pore collapse and a single surface chemical functionality, which necessitate modification methods to improve their performance. The nitrogen-doping strategy offers unique advantages in charge distribution, the creation of active sites, alterations in surface chemical properties, and enhanced structural stability. Therefore, a magnetic nitrogen-doped porous carbon (MNPC) derived from NH-MIL-88(Fe) was developed as an MSPE adsorbent, combined with liquid chromatography, for sensitive determination of trace amounts of chloramphenicol in honey samples. The developed method exhibits a good linear relationship in the range of 0.05-50 μg·L, with R of 0.9999, LOD (S/N=3) of 0.005 μg·L, and LOQ (S/N=10) of 0.02μg·L. The spiked recovery rate ranged from 93.5% to 99.2%, and the RSD ranged from 1.3% to 10.7%. Therefore, this method has significant potential for routine monitoring of chloramphenicol residues in food safety supervision.
A rapid in-situ method based on liquid-phase nanoextraction for the determination of perfluorinated compounds in cerebrospinal fluid.
Zhang X, Cai L, Cui M … +6 more , Huang X, Piao H, Jin X, Shi X, Li D, Zou Y
J Chromatogr A · 2026 Jul · PMID 42090908 · Publisher ↗
Perfluorinated compounds (PFCs) are emerging pollutants with strong bioaccumulation and stability, and potential risks to human health. Biological samples are usually limited in volume and content trace levels of target...
Perfluorinated compounds (PFCs) are emerging pollutants with strong bioaccumulation and stability, and potential risks to human health. Biological samples are usually limited in volume and content trace levels of target analytes, thus requiring in-situ and minimally invasive detection techniques (such as solid-phase microextraction (SPME), microfluidic chip analysis, and in vivo sampling). However, conventional detection methods are difficult to achieve accurate qualitative and quantitative analysis of trace PFCs. In this study, a rapid, in-situ and green analytical method was developed by combining nanoconfined liquid phase nanoextraction (NLPNE) with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of 9 PFCs in cerebrospinal fluid. The interlaced carbon nanofibers (CNFs) form multi-dimensional network nanopores, which provide favorable structural basis for the construction of NLPNE systems. The carbon nanofibers/carbon fibers (CNFs/CFs) was used to confined methanol, which was packed into the needle tip to fabricate a portable needle-tip extraction device. The confined methanol enhanced the extraction efficiency of 9 PFCs. Key parameters affecting extraction performance were optimized (including confined fluid type and volume, extraction time, desorption solvent type and desorption time). Under optimal conditions, the method exhibited excellent linearity (r ≥ 0.9955) in the range of 0.1-500 μg L, with method limits of detection (MDLs) and limits of quantification (MQLs) ranging from 0.15 to 7.5 μg L and 0.50 to 24.98 μg L, respectively. The intra-day and inter-day relative standard deviations (RSDs) were ≤12.99%, and the recovery of PFCs in cerebrospinal fluid samples was 70.56%-119.12% with RSD ≤11.63%. Compared with traditional methods, this method has the advantages of short time, small organic solvent, and simple operation ability, providing a novel and reliable approach for the real-time rapid analysis of trace PFCs in small-volume complex biological samples.
Comprehensive exploration and comparison of chemical constituents of Paris polyphylla var. chinensis and Paris polyphylla var. yunnanensis through two-dimensional chromatography, metabolomic analysis and furostanosides quantitation.
Guan L, Ji L, Chen L … +3 more , Xiao S, Wang Z, Gao H
J Chromatogr A · 2026 Jul · PMID 42085960 · Publisher ↗
Paris polyphylla var. chinensis (PPC) and Paris polyphylla var. yunnanensis (PPY) were recognized as two legal species of Paridis Rhizoma in the Chinese Pharmacopoeia, exhibiting distinct chemical profiles primarily in t...
Paris polyphylla var. chinensis (PPC) and Paris polyphylla var. yunnanensis (PPY) were recognized as two legal species of Paridis Rhizoma in the Chinese Pharmacopoeia, exhibiting distinct chemical profiles primarily in terms of spirostanosides content. However, the chemical differences of other types of steroidal saponins remained unclear, comprehensive component comparison is lacking. In this research, an offline two-dimensional separation system (comprising HILIC and C) was established to thoroughly explore and compare the chemical components between PPC and PPY. Additionally, a nontargeted metabolomic approach utilizing high-resolution mass spectrometry was employed to identify differential metabolites. Consequently, a total of 444 metabolites were characterized, among which steroidal saponins were the most abundant components. Specifically, 394 steroidal saponins were identified based on their fragmentation patterns and chromatographic retention behaviors. The significant differences were observed in furostanosides and polyhydroxylated steroidal saponins between PPC and PPY. To enable quantitative analysis of furostanosides, the biosynthetic precursors of spirostanosides, a high-performance liquid chromatography method employing a HILIC column was developed for the first time. Similar to the profiles of spirostanosides, PPC contains a high abundance of proto-pennogenyl saponins, whereas PPY is rich in proto-diosgenyl saponins. These results facilitated a detailed understanding of chemical information of PPC and PPY, and improved quality control tactics of Paridis Rhizoma.
Preserving early harvested Zanthoxylum schinifolium quality flavor retention via integrated packaging temperature control.
Li X, Zhang W, Guo N … +6 more , Wang J, Deng J, Lian C, Zhou Y, Lettmann T, Li X
J Chromatogr A · 2026 Jul · PMID 42085959 · Publisher ↗
This study compared the effects of vacuum packaging (VP), nitrogen-filled packaging (NP), and Air condition packaging (AC) on the storage quality of fresh Zanthoxylum schinifolium Siebold&Zucc at 0 °C and 25 °C for 21 d....
This study compared the effects of vacuum packaging (VP), nitrogen-filled packaging (NP), and Air condition packaging (AC) on the storage quality of fresh Zanthoxylum schinifolium Siebold&Zucc at 0 °C and 25 °C for 21 d. The results showed that VP was the most effective in maintaining moisture, while NP was more conducive to maintaining green appearance and numbing substances (the highest content was found in the NP0 at 21 d, reaching 2.63 mg/g). The polyphenol content of fresh Z. schinifolium treated with three packaging treatments exceeded 110 (GAE mg/g) at 25 °C, and the flavonoid content remained above 489 (RE mg/g). A total of 41 volatile substances were identified, mainly consisting of olefins (87%), among which myrcene and linalool were key flavor components, jointly imparting spicy, earthy, and woody aromas. Correlation analysis showed that moisture was positively correlated with antioxidant activity and color, while linalool is positively correlated with polyphenol content and DPPH scavenging rate, and negatively correlated with elasticity. This study provides a theoretical basis for precise post harvest storage and quality control of Z. schinifolium.
Direct measurement of critical micelle concentrations of mPEG-PLA copolymers based on ultrafiltration combined with liquid chromatography tandem mass spectrometry.
Wang H, Wang X, Yao J … +1 more , Meng X
J Chromatogr A · 2026 Jul · PMID 42085958 · Publisher ↗
The critical micelle concentration (CMC) is a core parameter dictating the formation and stability of polymeric micelles in drug delivery. Conventional CMC determination methods, relying on indirect measurements, are con...
The critical micelle concentration (CMC) is a core parameter dictating the formation and stability of polymeric micelles in drug delivery. Conventional CMC determination methods, relying on indirect measurements, are constrained by issues such as limited sensitivity or potential interference. To overcome these limitations, this study established a method based on ultrafiltration coupled with liquid chromatography-tandem mass spectrometry (UF-LC-MS/MS) for directly determining the CMC of methoxy poly(ethylene glycol)-block-poly(D,L-lactide) (mPEG-PLA) with varying PLA chain lengths. The LC-MS/MS method exhibited good linearity, accuracy, and precision for the quantification of mPEG-PLA, mPEG-PLA, and mPEG-PLA. The optimized and validated ultrafiltration process ensured selective separation of micelles from unimers. By identifying the inflection point in the concentration of free mPEG-PLA in the tested sample, the CMC values were determined as 5.77 ± 0.16 μg/mL for mPEG-PLA, 3.02 ± 0.16 μg/mL for mPEG-PLA, and 1.86 ± 0.04 μg/mL for mPEG-PLA. These results were comparable to those from the conventional pyrene fluorescence probe assay, demonstrating that UF-LC-MS/MS is a robust tool for CMC determination of mPEG-PLA copolymers, with strong potential for broader application to other amphiphilic polymers.
Separation of rubidium isotopes by extraction chromatography with a retaining ion strategy.
Jiang Y, Li H, Cheng J … +2 more , Tang Z, Huang K
J Chromatogr A · 2026 Jul · PMID 42085957 · Publisher ↗
Currently, separation of rubidium isotopes relies predominantly on electromagnetic methods. However, operational complexity and prohibitive equipment costs severely limit its broader applicability and industrial scalabil...
Currently, separation of rubidium isotopes relies predominantly on electromagnetic methods. However, operational complexity and prohibitive equipment costs severely limit its broader applicability and industrial scalability. In this study, we propose a novel extraction chromatography method for rubidium isotope separation of using t-BAMBP-impregnated resin as the stationary phase and introducing K as retaining ion to increase the separation coefficient between Rb and Rb during elution process. Compared to conventional electromagnetic separation, this new extraction chromatography method features a simple operating condition and lower processing cost for rubidium isotope separation. According to the Stokes-Einstein relation, the lighter mass of Rb has a smaller effective hydrodynamic radius and consequently a higher diffusion coefficient compared to Rb. This intrinsic kinetic difference, combined with the subtle disparity in their distribution ratios on the t-BAMBP-impregnated resin, leads to a faster migration rate of Rb over Rb during chromatographic elution. The introduction of K as a retaining ion further prolongs the retention time and increases the plate number of adsorption-desorption cycles, thereby amplifying the longitudinal diffusion advantage of Rb. Under the optimized conditions, this synergistic effect from introduction of K as a retaining ion yields a maximum single-column separation factor of 1.00534. The current work achieves a breakthrough in rubidium isotope separation, which is beneficial for future industrial applications.
Same-source analysis of microplastics and polycyclic aromatic hydrocarbons in surface water using unified pretreatment, TD-GC/MS, and Py-GC/MS.
Qiu Y, Li M, Li Z … +1 more , Liu J
J Chromatogr A · 2026 Jul · PMID 42070464 · Publisher ↗
Microplastics can accumulate hydrophobic organic pollutants, but microplastic identification and PAH analysis are often conducted using separate subsamples or different pretreatment routes, which weakens the corresponden...
Microplastics can accumulate hydrophobic organic pollutants, but microplastic identification and PAH analysis are often conducted using separate subsamples or different pretreatment routes, which weakens the correspondence between polymer type and co-occurring contaminants. Here, we established an application-oriented same-source analytical workflow for the joint analysis of microplastics and PAHs affiliated with the enriched microplastic-containing fraction in surface-water samples. The enriched sample obtained after unified pretreatment was analyzed by thermal desorption-GC/MS for affiliated PAHs and by pyrolysis-GC/MS for microplastics. By generating both types of information from the same enriched sample, this workflow reduces sample splitting and simplifies pretreatment prior to instrumental analysis. After fractionated filtration and density separation, the enriched microplastic-containing fraction was subjected to thermal desorption-GC/MS for PAH analysis and pyrolysis-GC/MS for microplastic fingerprint characterization. Applied to seven representative watershed sections, six polymers PMMA, PP, PET, PVC, PC, and PE were detected. Significant spatial heterogeneity in microplastic concentrations was observed across sampling sites, with the highest level at S6 (1.3 μg/mL) and the lowest at S2/S5. Polymer composition also varied markedly: PVC dominated in the middle reaches (S2-S4), while PET became the dominant polymer (>65%) in downstream sites (S6-S7). Twelve PAHs affiliated with the enriched microplastic-containing fraction were identified, with estimated ∑PAHs levels ranging from 10 to 500 ng/g, mostly low-ring species 60-80%. This workflow enables joint characterization of microplastic types and affiliated PAHs from the same enriched sample, providing an efficient analytical approach for integrated monitoring and comparative analysis at the watershed scale.
A rapid GC-MS method for the simultaneous determination of bupropion and hydroxybupropion in plasma using SALLME and microwave-assisted derivatization.
Neşetoğlu M, Al S, Neşetoğlu N … +2 more , Kul A, Sagirli O
J Chromatogr A · 2026 Jul · PMID 42070463 · Publisher ↗
Bupropion is widely used in the treatment of major depressive disorder and smoking cessation, and its clinical response is largely influenced by its active metabolite, hydroxybupropion. Due to significant pharmacokinetic...
Bupropion is widely used in the treatment of major depressive disorder and smoking cessation, and its clinical response is largely influenced by its active metabolite, hydroxybupropion. Due to significant pharmacokinetic variability and the therapeutic relevance of hydroxybupropion concentrations, reliable analytical methods suitable for therapeutic drug monitoring (TDM) are required. In this study, a rapid gas chromatography-mass spectrometry (GC-MS) method was developed for the simultaneous determination of bupropion and hydroxybupropion in human plasma using a novel sample preparation strategy termed KUL-SPEED (Kul's Ultra-fast, Low-step Sample Preparation with Efficient Extraction and Derivatization). The method integrates salt-assisted liquid-liquid microextraction (SALLME) with microwave-assisted trimethylsilylation in a unified workflow, eliminating solvent evaporation and reconstitution steps. Sample preparation and derivatization were completed within approximately 5 min, and chromatographic separation was achieved within an 8-minute total run time. Method validation was performed according to ICH M10 guidelines. Calibration was linear over 50-2000 ng/mL for bupropion and 250-2000 ng/mL for hydroxybupropion, with acceptable accuracy, precision, stability, and matrix effect results. The method was successfully applied to patient plasma samples, confirming its applicability for routine TDM. The KUL-SPEED approach may also be adaptable to other derivatizable analytes in biological matrices.
Electrospun polyvinyl alcohol/LDH nanofibers modified with sodium dodecyl sulfate as a coating for fiber-in-tube solid-phase microextraction of trace fungicides in cosmetic samples.
Pourhosseini S, Yamini Y, Nasrollahi SS
J Chromatogr A · 2026 Jul · PMID 42068825 · Publisher ↗
A sensitive analytical protocol was developed to quantify trace levels of three azole fungicides-ketoconazole (KZ), miconazole (MZ), and clotrimazole (CZ)-in cosmetic matrices. This method integrates fiber-in-tube solid-...
A sensitive analytical protocol was developed to quantify trace levels of three azole fungicides-ketoconazole (KZ), miconazole (MZ), and clotrimazole (CZ)-in cosmetic matrices. This method integrates fiber-in-tube solid-phase microextraction (FIT-SPME) with high-performance liquid chromatography and ultraviolet detection (HPLC-UV). The extraction medium utilized magnesium-aluminum layered double hydroxides (LDHs) intercalated with sodium dodecyl sulfate (SDS), prepared via urea hydrolysis. To fabricate the sorbent, this modified LDH was embedded within a polyvinyl alcohol (PVA) solution-chosen for its green chemistry attributes-and electrospun onto stainless steel substrates. To prevent dissolution in aqueous samples, the coating was thermally cross-linked using citric acid, ensuring robust mechanical stability. The device consisted of these coated fibers housed within a steel capillary, through which samples were circulated for equilibrium adsorption, followed by solvent desorption. A rigorous optimization process was conducted to determine ideal conditions for pH, ionic strength, flow rates, and timing variables. Performance metrics revealed low limits of detection (0.3-0.6 µg L) and high precision, with inter-day relative standard deviations (RSDs) not exceeding 6.2%. The technique displayed a broad linear dynamic range (up to 750.0 µg L) and satisfactory determination coefficients (R > 0.9913). Finally, the analysis of real samples, including shampoos, creams, and lotions, yielded relative recoveries ranging from 82% to 115%, confirming the method's reliability for complex formulations.
A high-performance thin-layer chromatography-bioautography-mass spectrometry approach for screening β-lactamase inhibitors from herbal medicines.
Si ZH, Kim MS, Li LN … +3 more , Yang L, Gu LH, Wang ZT
J Chromatogr A · 2026 Jul · PMID 42068824 · Publisher ↗
A high-performance thin-layer chromatography-bioautography (HPTLC-bioautography) method was developed for the rapid screening of β-lactamase inhibitors based on nitrocefin chromogenic hydrolysis. By integrating chromatog...
A high-performance thin-layer chromatography-bioautography (HPTLC-bioautography) method was developed for the rapid screening of β-lactamase inhibitors based on nitrocefin chromogenic hydrolysis. By integrating chromatographic separation with on-plate enzymatic detection, the proposed approach enables direct localization of β-lactamase inhibitory constituents from complex matrices while effectively minimizing matrix and sample color interference. Key experimental parameters were systematically optimized, and the method exhibited good flexibility by allowing screening against four different classes of β-lactamases through enzyme selection. Quantitative analysis was achieved by densitometric scanning at 525 nm, corresponding to the maximum absorption of the hydrolysis product. The method showed a limit of detection of 2 ng and a limit of quantification of 8 ng for the reference inhibitor tazobactam, along with satisfactory precision, repeatability, accuracy, and stability. The applicability of the method was demonstrated by screening extracts from twelve herbal medicines, leading to the identification of β-lactamase inhibitory zones in Perilla folium, Lonicera japonica Flos, and Lonicera Flos. Two active constituents were further characterized as rosmarinic acid and isochlorogenic acid A using online HPTLC-mass spectrometry, and their activities were verified by molecular docking and microplate-based enzymatic assay. Overall, the proposed HPTLC-bioautography strategy provides an efficient and selective analytical platform for the screening and characterization of β-lactamase inhibitors in complex natural products.
Impact of selector regioisomerism on mixed-mode retention and enantioresolution: Comparative evaluation of 3-chloro-4-methyl and 4-chloro-3-methyl substituted cellulose chiral stationary phases.
Pardo-Cortina C, Escuder-Gilabert L, Sagrado S … +2 more , Medina-Hernández MJ, Martín-Biosca Y
J Chromatogr A · 2026 Jul · PMID 42068823 · Publisher ↗
This study examines how selector regioisomerism affects retention and enantioselective performance on cellulose-based chiral stationary phases (CSPs) under aqueous-organic mixed-mode conditions. Two regioisomeric selecto...
This study examines how selector regioisomerism affects retention and enantioselective performance on cellulose-based chiral stationary phases (CSPs) under aqueous-organic mixed-mode conditions. Two regioisomeric selectors, cellulose tris(3‑chloro-4-methylphenylcarbamate) (Cell2) and cellulose tris(4‑chloro-3-methylphenylcarbamate) (Cell4), were evaluated using a library of 75 structurally diverse chiral compounds over a broad range of acetonitrile/water mobile phases. Both CSPs showed U-shaped retention profiles, consistent with a transition from reversed-phase retention to HILIC-like behavior in the organic-rich region. Quantitative analysis using the empirical HILIC induction factor (HF) and stoichiometric-displacement modeling indicated that, while global median induction was comparable, Cell2 induced a significantly stronger retention amplification for specific basic families at high acetonitrile contents. In contrast, Linear Solvent Strength analysis in the water-rich region suggested that the intrinsic hydrophobic contributions of both phases are statistically comparable for the subset of analytes exhibiting classical reversed-phase behavior. In enantioselective terms, Cell2 displayed the broader screening scope, particularly for flexible amine-containing analytes, whereas Cell4 provided higher resolving power for selected rigid and aromatic scaffolds. Remarkably, despite strong thermodynamic selectivity in the organic-rich region, practical maximum enantioresolution was systematically achieved within the highly aqueous RPLC domain for almost all chemical families, driven by favorable kinetic residence times. PCA-based descriptor mapping associated the Cell2 advantage in HF with analytes rich in hydrogen-bond-donor and hydroxyl functionalities, whereas the Cell4 advantage in resolution was associated with sterically demanding and more aromatic structures. Overall, the results support a practical data-driven structure-retention-resolution framework for selecting between these two regioisomeric polysaccharide CSPs according to analyte class and mobile-phase composition.
In-depth phospholipid profiling of lymphoma cells by HPLC coupled with trapped ion mobility spectrometry and high-resolution tandem mass spectrometry.
Wieland D, Schmitt A, Hailfinger S … +1 more , Hayen H
J Chromatogr A · 2026 Jul · PMID 42068822 · Publisher ↗
Lipids exhibit extensive molecular diversity and structural complexity, which poses major analytical challenges for comprehensive lipidomic profiling. Phospholipids, in particular, display extensive structural diversity...
Lipids exhibit extensive molecular diversity and structural complexity, which poses major analytical challenges for comprehensive lipidomic profiling. Phospholipids, in particular, display extensive structural diversity and isomerism. Given the limited lipidomic data available for lymphoma cells, this work focuses on comprehensive phospholipid screening, which inherently requires the characterization of isomeric species, including plasmalogens that have been implicated in oxidative stress and ferroptosis-related cell death. Therefore, we present an efficient isomer-selective workflow based on reversed-phase liquid chromatography (RPLC) coupled to trapped ion mobility spectrometry (TIMS) and high-resolution tandem mass spectrometry (HR-MS/MS). High-confidence structural lipid annotation is achieved through the integrated evaluation of chromatographic retention time (t), exact mass-to-charge ratio (m/z), collision cross section (CCS) and mobility-resolved MS/MS data. Applied to human lymphoma cell lipid extracts, the workflow enabled confident identification of 263 individual lipid species spanning 10 phospholipid and 2 sphingolipid subclasses, including the resolution of 63 isomeric species at the fatty-acyl compositional level. The multidimensional approach allowed partial discrimination of fatty-acyl compositional, sn- and double bond positional isomers. Notably, characteristic deviations in both retention time and ion mobility were observed for plasmalogens relative to alkyl-ether linked phospholipids, reflecting the unique physicochemical properties of the vinyl-ether linkage. These systematic offsets enabled confident plasmalogen assignment in representative cases, supported by authentic standards, co-chromatograms and mobility-resolved fragmentation data. Collectively, this streamlined analytical platform markedly expands phospholipidome coverage and provides enhanced structural resolution of complex lipid mixtures.
Efficient enrichment and sensitive detection of phthalates in edible oil and traditional medicinal crops using a fluoro-functionalized-COF-based solid-phase microextraction.
Liu Y, Zhu W, Gong M … +3 more , Gu S, Yang Q, Hou X
J Chromatogr A · 2026 Jul · PMID 42068821 · Publisher ↗
The residue of phthalates (PAEs) in edible products can cause endocrine disorders in the human body. In this study, a solid-phase microextraction (SPME) probe coated with fluoro-functionalized covalent organic frameworks...
The residue of phthalates (PAEs) in edible products can cause endocrine disorders in the human body. In this study, a solid-phase microextraction (SPME) probe coated with fluoro-functionalized covalent organic frameworks (F-COFs) was developed for the extraction of PAEs. The synthesized F-COFs coating exhibited excellent hydrophobicity and high thermal stability, making it suitable for adsorbing PAEs. The established F-COF-SPME-GC method achieved a green analytical chemistry score of 0.63 in terms of environmental friendliness. It also exhibited satisfactory linear ranges of 0.02-100 μg L for all PAEs (R²≥0.9901), and limits of detection (LODs) ranged from 0.010 to 0.019 μg L. The method was successfully applied to determine PAEs in six edible oils and six traditional medicinal crops, exhibiting relatively strong resistance to matrix interference. These results indicated that the F-COF-SPME probe provided significant promise for the efficient and robust adsorption and detection of PAEs in complex samples.
Corrigendum to "High-throughput mRNA poly(A) tail characterization through on-off retention ion-exchange chromatography" [Journal of Chromatography A, Volume 1776, 2026, 466928, ISSN 0021-9673].
Vo C, Lieu R, Fan Y … +3 more , Zhang K, Chen T, Su WC
J Chromatogr A · 2026 Jul · PMID 42067421 · Publisher ↗
Abstract loading — click title to view on PubMed.
Speciation of selenium through chromatography with atomic techniques.
Teixeira LSG, Ferreira SLC, Garrigues S … +1 more , de la Guardia M
J Chromatogr A · 2026 Jul · PMID 42061177 · Publisher ↗
This review article provides an overview of selenium speciation using chromatographic and atomic techniques, based on a survey of relevant studies published in the 21st century. Selenium is an essential element, but the...
This review article provides an overview of selenium speciation using chromatographic and atomic techniques, based on a survey of relevant studies published in the 21st century. Selenium is an essential element, but the narrow range between deficiency and toxicity makes determining its various chemical forms in many samples fundamental. The total selenium content is insufficient to understand its behavior, as its various species exhibit distinct physicochemical and toxicological properties. In general, organic forms, such as selenomethionine (SeMet) and methylselenocysteine (MeSeCys), are less toxic and more bioavailable than inorganic species and are also associated with beneficial health effects, such as antioxidant activity and potential disease-prevention benefits. Therefore, selenium speciation analysis in various matrices is fundamental to understanding its toxicity, bioavailability, biotransformation, and bioaccumulation, since different chemical species exhibit distinct biological behaviors. Strategies combining chromatographic and atomic detection techniques have been explored for selenium speciation, leveraging separation resolution and detection sensitivity to achieve selective methods with low detection limits and applicability to complex matrices. The most used techniques for speciation include high-performance liquid chromatography (HPLC) and gas chromatography (GC), typically coupled to inductively coupled plasma mass spectrometry (ICP-MS) or other atomic detectors, such as atomic absorption spectroscopy (AAS) and atomic fluorescence spectroscopy (AFS). In addition to reviewing the literature on chromatography-atomic techniques combinations, sample preparation, separation methods, and detectors were discussed. Applications in food, biological, and environmental samples are presented, highlighting the importance of speciation for evaluating selenium toxicity and bioavailability. This review indicates that significant challenges remain due to low analyte concentrations, the risk of interconversion between species, and the emergence of new demands, such as analyzing complex matrices of food, supplements, and biological samples. This shows that Se speciation is a dynamic, continually evolving field essential to analytical chemistry and understanding the effects of selenium on health and the environment.
Simultaneous determination of monochloramine and common anions in drinking water by mixed-mode ion chromatography with sequential UV absorbance and suppressed conductivity detection.
Mrabawani N, Mikhail IE, Shellie RA … +1 more , Paull B
J Chromatogr A · 2026 Jul · PMID 42061176 · Publisher ↗
A sensitive and rapid mixed-mode ion chromatography-based method for the simultaneous quantification of the disinfectant monochloramine and common inorganic anions within treated drinking waters is presented. The separat...
A sensitive and rapid mixed-mode ion chromatography-based method for the simultaneous quantification of the disinfectant monochloramine and common inorganic anions within treated drinking waters is presented. The separation was achieved on a high-capacity anion-exchange column (Dionex IonPac AS15, 4 mm x 250 mm) using a mixed-mode approach, which combined ion-exchange and ion-exclusion-based retention for the inorganic anions and monochloramine, respectively. An electrolytically produced potassium hydroxide eluent gradient was employed, with the method combining suppressed conductivity detection with in-house assembled 50-mm flow cell high-sensitivity UV absorbance detection. This configuration provides a five-fold enhancement in UV absorbance signal relative to a conventional 10-mm flow cell, substantially improving sensitivity for UV-absorbing species. Monochloramine is detected directly and without derivatisation, with an absorbance maximum at 240 nm. The optimised method was able to separate and quantify eight target analytes commonly monitored in treated drinking waters, namely fluoride, chloride, nitrite, bromide, nitrate, phosphate, sulphate, and monochloramine, all within a 13-minute runtime. The method was validated, demonstrating excellent linearity (r≥0.996) across a 7-point calibration range and high precision with %RSD consistently at or below 1.8 %. The LOD for monochloramine is 0.11 mg/L, while those for the other anions ranged from 1.5 µg/L for fluoride to 0.17 mg/L for nitrate. The method's limits of detection were well below the maximum levels recommended in World Health Organization (WHO) guidelines for drinking water. Notably, the system was selective for monochloramine detection in the presence of dichloramine.
About
- Frequency
- Sun
- Papers found
- 200
- RSS feed
- Subscribe