J Chromatogr A [JOURNAL]
Sun
200 papers
Preparation and applications of sulfonated hyper-crosslinked polymers for capture and enrichment of fluoroquinolones.
Zhang Y, Li M, Zhang X … +4 more , Zhang X, Shen J, Wei Y, Wang C
J Chromatogr A · 2026 Jul · PMID 42025606 · Publisher ↗
This study synthesized a sulfonated hyper-crosslinked polymer, BpBCMBP‑SOH, via Friedel-Crafts alkylation and post-sulfonation for the adsorptive removal and enrichment of trace fluoroquinolone antibiotics (FQs) from com...
This study synthesized a sulfonated hyper-crosslinked polymer, BpBCMBP‑SOH, via Friedel-Crafts alkylation and post-sulfonation for the adsorptive removal and enrichment of trace fluoroquinolone antibiotics (FQs) from complex matrices. The material, rich in sulfonic acid groups, exhibited rapid, high-capacity, and selective adsorption towards FQs, with maximum adsorption capacities of 924, 958, 889, and 848 mg·g for ofloxacin, lomefloxacin hydrochloride, enrofloxacin, and difloxacin hydrochloride, respectively, ranking among the top-tier of previously reported results for FQ adsorption. The adsorption process is predominantly governed by electrostatic interactions, with synergistic contributions from hydrogen bonding, π-π interactions, and hydrophobic interactions. Removal efficiencies of four FQs from aqueous solutions exceeded 95% within 1 min, and reached equilibrium within 10 min with removal efficiencies exceeding 97%. After five consecutive adsorption-desorption cycles, the material retained approximately 70% of its removal efficiency, indicating good reusability. The material was also used for enrichment of FQs in complex matrices. When coupled with high performance liquid chromatography, the detection of low concentration removal rate as low as 10 ng·mL, can be achieved through separation and enrichment in pure water and lake water. In complex matrices such as eggs and milk, the established analytical method exhibited recoveries of 89.3-116.6% for FQs, with intra-day and inter-day relative standard deviations (RSD) below 15%, and the detection limits ranging from 0.33 to 1.67 ng·mL, which underscores its applicability and reliability. This work offers a novel material and reliable methodology for the analysis of trace FQs in environmental and food safety monitoring.
Targeted and non-targeted screening of multi-class emerging contaminants in aquaculture products using LC-Q-Orbitrap HRMS.
Khaled O, Medhat M, Halawa E … +3 more , Gad N, Eissa F, Ryad L
J Chromatogr A · 2026 Jul · PMID 42019245 · Publisher ↗
Non-targeted screening methodologies have emerged as essential tools for comprehensive food safety surveillance, enabling detection of unanticipated contaminants beyond conventional targeted analysis. This study presents...
Non-targeted screening methodologies have emerged as essential tools for comprehensive food safety surveillance, enabling detection of unanticipated contaminants beyond conventional targeted analysis. This study presents the first comprehensive non-targeted high-resolution mass spectrometry screening platform for aquaculture products established in Egypt, integrating streamlined extraction protocols with liquid chromatography-quadrupole-Orbitrap high-resolution mass spectrometry (LC-Q-Orbitrap HRMS). A total of 213 samples encompassing eight commercially important aquaculture commodities-salmon, pangasius, basa, tuna, tilapia, shrimp, lobster, and crawfish-were analyzed for veterinary pharmaceuticals, prohibited compounds, environmental pollutants, and their transformation products. Non-targeted screening revealed 48 compounds spanning multiple chemical classes, including triphenylmethane dyes, polyethylene glycol derivatives, industrial chemicals, pharmaceutical residues, and nitroimidazole-related compounds. Crystal violet, a banned carcinogenic dye, was detected across all fish species except shrimp with frequencies ranging from 8% to 31%, with pangasius exhibiting the highest occurrence. Pangasius demonstrated the broadest contaminant diversity (46 compounds), followed by salmon (32 compounds), tilapia (25 compounds), and basa (25 compounds). These findings demonstrate the value of non-targeted approaches for identifying emerging contaminants and provide essential baseline data for risk-based monitoring programs, representing a significant advancement for regulatory food safety assessment in aquaculture matrices.
A pseudo-targeted pharmacokinetic study on traditional Chinese medicine formulae by the ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry integrated with scheduled multiple reaction monitoring platform: QiangHuoShengShi decoction as a case.
Guo J, Wen J, Shang Y … +5 more , Du K, Chen S, Li J, Wang X, Chang Y
J Chromatogr A · 2026 Jul · PMID 42019244 · Publisher ↗
QiangHuoShengShi decoction (QHSS), a classical prescription traditional Chinese medicine (TCMs), boasts a lengthy clinical history in treating various rheumatic diseases. No pharmacokinetic (PK) studies on QHSS were repo...
QiangHuoShengShi decoction (QHSS), a classical prescription traditional Chinese medicine (TCMs), boasts a lengthy clinical history in treating various rheumatic diseases. No pharmacokinetic (PK) studies on QHSS were reported to date while its in vitro and in vivo chemical fingerprints were comprehensively reported. This study aims to reveal the time-dependent changes in the concentrations of multi-known and -unknown components in rats after oral administration of QHSS, thereby offering insights for further research into its pharmacodynamic mechanisms. The prediction of multiple reaction monitoring (MRM) parameters for known and unknown analytes was first achieved using a standards-independent ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS/MS) method coupled with linear correlation analysis. Subsequently, specific parameters were then determined using single-factor optimization by the ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS). Finally, the concentrations of known and unknown analytes in plasma biosamples were determined using a built scheduled multiple reaction monitoring (sMRM) method. The sMRM parameters for 90 compounds were predicted and optimized. The pharmacokinetic parameters, including mean time to reach peak concentration (T, maximum plasma concentration (C, area under concentration-time curve (AUC), mean resident time (MRT), were characterized for 32 measurable components (17 with standard substances and 15 without standard substances). The pharmacokinetic parameters of 28 components from biosamples of the rheumatoid arthritis (RA) group were further compared with those from the normal group, revealing significant differences (either increased or decreased) in their PK parameters. A pseudo-targeted pharmacokinetic study of QHSS was successfully conducted by a standards-independent UHPLC-Q-TOF-MS/MS with UHPLC-sMRM-MS/MS method, which holds significant promise for subsequent research into the medicinal substances of QHSS. It can also serve as a powerful tool for multi-compounds pharmacokinetic study of more TCMs.
Automated solid-phase extraction coupled with heart-cutting two‑dimensional liquid chromatography for simultaneous quantification of thirteen fat-soluble vitamins in foods for special medical purposes.
Sun L, Li Q, Zhu S … +5 more , Sun Q, Zheng S, Feng T, Sheng H, Zhang S
J Chromatogr A · 2026 Jul · PMID 42019243 · Publisher ↗
A method based on heart‑cutting two‑dimensional liquid chromatography coupled with automated solid‑phase extraction was developed and validated for the simultaneous determination of thirteen fat‑soluble vitamins, includi...
A method based on heart‑cutting two‑dimensional liquid chromatography coupled with automated solid‑phase extraction was developed and validated for the simultaneous determination of thirteen fat‑soluble vitamins, including vitamins A, D₂, D₃, four tocopherols (α‑, β‑, γ‑, δ‑tocopherol), α‑tocotrienol, four β‑carotene isomers (all‑trans‑, 9‑cis‑, 13‑cis‑, 15‑cis‑β‑carotene), and lutein-in foods for special medical purposes (FSMP). The method integrates automated SPE sample purification with a two‑dimensional chromatographic separation that employs a C30 column in the first dimension and a PFP column in the second dimension. A heart‑cutting valve‑switching strategy was implemented to selectively transfer the vitamin‑D‑containing fraction from the first to the second dimension, thereby overcoming matrix interference and enabling accurate trace‑level quantification. The method demonstrated excellent performance: limits of detection (LODs) ranged from 0.01 μg/L (vitamin A) to 0.05 mg/L (tocopherols and α‑tocotrienol) and 0.001-0.005 mg/L (β‑carotene isomers), with corresponding limits of quantification (LOQs) from 0.03 μg/L to 0.15-0.015 mg/L. Spike recoveries for all analytes were between 88.5% and 108.2%, with intra‑ and inter‑day precision (RSD) below 5.0%. When applied to commercial FSMP samples, results showed good agreement (relative deviations < 10%) with established Chinese national standard methods. This sensitive, robust, and highly automated 2D‑LC‑SPE platform provides a reliable, high‑throughput solution for quality control, nutrition‑label compliance verification, and regulatory monitoring of FSMP products.
A ribonucleic acid mapping brainteaser: solving a ribonuclease 4 / ribonuclease A crossword using pre- and post-column digestion.
Morreel K, Vanluchene H, De Vos J … +3 more , Van Hoestenberghe E, Sandra P, Sandra K
J Chromatogr A · 2026 Jul · PMID 42019242 · Publisher ↗
Various modifications occur on both in vivo and in vitro produced messenger ribonucleic acid (mRNA), many of them defying identification by next generation sequencing (NGS). With the promising developments of therapeutic...
Various modifications occur on both in vivo and in vitro produced messenger ribonucleic acid (mRNA), many of them defying identification by next generation sequencing (NGS). With the promising developments of therapeutic/prophylactic mRNA, the urge to characterize all modifications arising during synthesis and storage becomes prevailing. Whereas sequencing of long nucleic acids by mass spectrometry (MS) is still in its infancy, unknown modifications are dealt with by MS rather than NGS. This necessitates the development of new MS-based RNA mapping strategies where oligonucleotides derived from a ribonuclease (RNase) digestion are identified via MS/MS spectral elucidation in a liquid chromatography-MS (LC-MS) set up. Here, a complementary LC-MS platform has been developed in which oligonucleotide identification is raised to full MS level by post-column RNase digestion of the oligonucleotides. A custom-built low-volume RNase A-bearing cartridge enabled successful oligonucleotide digestion without compromising separation efficiency. Combined with the in-house developed MSsenger software, chromatogram-aligned analysis of the LC-MS data from RNase 4-digested firefly luciferase mRNA using either the RNase A-bearing or a non-functionalized cartridge, was achieved. This allowed reconstitution of the mRNA from its RNase 4-derived oligonucleotides which were identified based on their RNase A digest signature. Exploration of the complex LC-MS data unveiled (i) the complementarity between conventional MS/MS-based sequencing and the post-column digestion approach, and (ii) the high sequence coverage reached by combining both methods. Being complementary to default RNA mapping methods, incorporation of post-column RNase digestion boosts sequence coverage and provides a new method for LC-MS-based localization of unknown modifications.
HPLC-PDA and LC-HRMS/MS-based quantitative and qualitative analysis of Glycosmis pentaphylla alkaloids, and investigation of their anticancer potential through network pharmacology.
Rajyaguru S, Teja PK, V K Y … +4 more , Das J, Madavi R, Sharma N, Chauthe SK
J Chromatogr A · 2026 Jul · PMID 42013794 · Publisher ↗
Glycosmis pentaphylla (Rutaceae) is a medicinal plant of ethnobotanical importance, noted for its diverse alkaloid content and therapeutic potential. This study integrates analytical chemistry and network pharmacology to...
Glycosmis pentaphylla (Rutaceae) is a medicinal plant of ethnobotanical importance, noted for its diverse alkaloid content and therapeutic potential. This study integrates analytical chemistry and network pharmacology to investigate its major alkaloids. A robust high-performance liquid chromatography method with photodiode array detection (HPLC-PDA) was developed and validated according to ICH Q2(R2) guidelines for the simultaneous quantification of eight key alkaloids (1-8) of G. pentaphylla. Quantitative analysis indicated that des-N-methylacronycine (3) was present at 17.24 mg/g in the root methanolic extract and 3.46 mg/g in the stem methanolic extract. Noracronycine (7) was present at 3.6 mg/g in the root hexane extract and 5.89 mg/g in the stem hexane extract. In the fruit extracts, kokusaginine (2) was the most abundant compound in the methanolic extract (36.23 mg/g), while 3-O-methoxyglycocitrine II (8) was the most abundant in the hexane extract (19.25 mg/g). To ensure specificity and unambiguous identification, qualitative characterization of the crude extract was performed using liquid chromatography-high-resolution mass spectrometry (LC-HRMS/MS). All eight alkaloids exhibited a unique fragmentation pattern consistent with radical cation chemistry. Protein-protein interaction (PPI) analysis identified 24 hub genes. Gene Ontology (GO) and KEGG pathway enrichment analyses indicated significant involvement of these hub genes in PI3K-Akt signalling, proteoglycan-mediated oncogenesis, and intracellular signal transduction. A compound-target-pathway network further highlighted 5-hydroxynoracronycine (5) as a potential anticancer lead compound. This study integrates analytical chemistry and systems pharmacology to enable quality assessment and mechanistic insights into the anticancer potential of G. pentaphylla alkaloids.
Application of the click analytical chemistry index for the assessment of endocrine-disrupting chemicals in cosmetics and personal care products.
Fuente-Ballesteros A, Jano A, Custodio-Mendoza JA … +4 more , Samanidou V, Mansour FR, Ares AM, Bernal J
J Chromatogr A · 2026 Jul · PMID 42013793 · Publisher ↗
Cosmetics and personal care products often contain parabens, phthalates, and bisphenols, compounds used as preservatives or plasticizers that may also migrate from packaging materials into the product. Their potential en...
Cosmetics and personal care products often contain parabens, phthalates, and bisphenols, compounds used as preservatives or plasticizers that may also migrate from packaging materials into the product. Their potential endocrine-disrupting effects have prompted stricter regulations and concentration limits. Given their occurrence and the complexity of cosmetic matrices, several extraction and chromatographic techniques have been developed to ensure reliable quantification. In this review, representative methods published from 2018 to 2025 focused on the determination of these compounds were evaluated using the click analytical chemistry index (CACI), a recently developed color-coded tool that integrates analytical performance, environmental impact, cost, and applicability within a single framework. CACI allows an objective and balanced comparison of analytical methods, emphasizing practicality and real-world feasibility. The obtained CACI scores ranged from 57 to 80, suggesting that the evaluated methodologies can be categorized as acceptable (50-75%) or highly practical (>75%). It is expected that the use of CACI will promote the development of more sustainable, practical, and user-oriented analytical strategies for the evaluation of chromatographic methods, not only for endocrine-disrupting chemicals in cosmetics and personal care products, but also for other substances of interest.
Sensitive high-performance thin-layer chromatography-acetylcholinesterase inhibition assay combined with S9 metabolization and high-resolution mass spectrometry for effect-directed analysis of food contact materials.
Azadniya E, Billerbeck K, Morlock GE
J Chromatogr A · 2026 Jul · PMID 42008900 · Publisher ↗
Effect-directed assay detection can prioritize potentially neurotoxic compounds within the vast chemical space of complex mixtures. For previously unknown (unknown unknowns) and chemically unidentified substances, a sens...
Effect-directed assay detection can prioritize potentially neurotoxic compounds within the vast chemical space of complex mixtures. For previously unknown (unknown unknowns) and chemically unidentified substances, a sensitive effect-directed detection is required. Hence, high-performance thin-layer chromatography hyphenated with the planar acetylcholinesterase (AChE) inhibition assay, including metabolization via the S9 liver system, was investigated for screening of potentially neurotoxic trace-level migrants and extracts from white polyurethane-coated tin cans. Two AChE inhibitor zones were detected. Their presence was confirmed using two independent substrates, i.e., naphthyl acetate/Fast Blue B salt and indoxyl acetate. Detected AChE inhibitor zones were identified as phthalic acid oligomers and linear alkyl sulfonic acids by high-resolution mass spectrometry. Their presence was verified by co-analysis of purchased or synthesized reference candidates.
QSRR-based insights into the chromatographic behaviour of phenolic derivatives on biomimetic stationary phases.
Singh YR, Vinci RL, Greber KE … +7 more , Nicman J, Gajewicz-Skretna A, Rigano F, Arena K, Mondello L, Cacciola F, Ciura K
J Chromatogr A · 2026 Jul · PMID 42001668 · Publisher ↗
A quantitative structure-retention relationship (QSRR) approach was employed to investigate the chromatographic behaviour of phenolic derivatives on biomimetic stationary phases. The study aimed to elucidate the molecula...
A quantitative structure-retention relationship (QSRR) approach was employed to investigate the chromatographic behaviour of phenolic derivatives on biomimetic stationary phases. The study aimed to elucidate the molecular determinants governing lipophilicity, membrane affinity, and protein binding using two complementary chemometric strategies: genetic algorithm-partial least squares (GA-PLS) and canonical correlation analysis (CCA). GA-PLS models, developed separately for each chromatographic endpoint, exhibited excellent predictive performance (R>0.95, Q>0.90) and revealed phase-specific determinants related to molecular topology, charge distribution, and lipophilicity. The CCA model, designed to integrate all chromatographic systems simultaneously, identified shared structural patterns driving retention across phases. Although slightly less predictive, it achieved high CCA (R>0.92) and maintained satisfactory external validity while offering superior interpretability. Mechanistic interpretation indicated that long-range steric and electronic complementarity, together with aromaticity and polarizability, governs the chromatographic behaviour of phenolic compounds across biomimetic systems. The findings demonstrate that GA-PLS and CCA provide complementary insights, with the former excelling in system-specific prediction and the latter enabling a unified understanding of cross-system molecular interactions. This study represents the first application of CCA to the simultaneous modelling of multiple biomimetic chromatographic systems, expanding the methodological scope of QSRR in bioanalytical research.
Uncovering the origin of impurities in supercritical fluid chromatography coupled to high-resolution mass spectrometry.
Bajramova A, Synefakis E, Larsen J … +3 more , Hjorth JL, Turner C, Sandahl M
J Chromatogr A · 2026 Jul · PMID 42001667 · Publisher ↗
Maintaining low background levels is essential for analytical instruments, such as in supercritical fluid chromatography (SFC) coupled to high-resolution mass spectrometry (HRMS). An approximate tenfold increase of the b...
Maintaining low background levels is essential for analytical instruments, such as in supercritical fluid chromatography (SFC) coupled to high-resolution mass spectrometry (HRMS). An approximate tenfold increase of the background was observed in our laboratory when a new CO cylinder with a dip tube was installed on a SFCHRMS system. Most analyte peaks were obscured. This study aimed to find the cause of the elevated background. Accordingly, the entire system was cleaned and each module, including the ion source, back pressure regulator, column, autosampler, solvent pumps, CO pump, and cylinder, were assessed. The troubleshooting suggested that the source of the contamination was the CO cylinder. A statistically significant (p < 0.05) elevation in the background was observed when liquid CO was used as mobile phase. The ions present above normal background levels were found to have m/z of 492.3439, 495.2934, 371.2434, and 490.3381. Annotation of the most abundant ion (m/z of 490.3381) based on m/z, isotope pattern, fragmentation pattern, and collision cross section, suggested structures resembling derivatives of sphingo- and glycolipids. A possible source could be degradation products formed during bioethanol production, the process from which the CO in the cylinder originates. Noteworthily, another SFCHRMS system that uses condensed gaseous CO instead of liquid CO, has so far not resulted in any contamination-related issues. To prevent contamination in sensitive SFC-HRMS systems, it is essential to assess the purity of the CO₂ before use, especially if liquid CO from a cylinder with dip tube is used.
Imidazolium-based ionic conjugated microporous polymer as a versatile SPE adsorbent for trace triazine herbicides in water and juice samples.
Li N, Hao YJ, Mu W … +8 more , Duan J, Wang X, Zhao LX, Jiang HL, Chen X, Cai Y, Zhao RS, Wang X
J Chromatogr A · 2026 Jul · PMID 41999696 · Publisher ↗
Efficient monitoring of triazine herbicide residues is essential for safeguarding environmental and food safety. In this work, an innovative imidazolium-functionalized ionic conjugated microporous polymer (Im-CMP) was de...
Efficient monitoring of triazine herbicide residues is essential for safeguarding environmental and food safety. In this work, an innovative imidazolium-functionalized ionic conjugated microporous polymer (Im-CMP) was developed through Sonogashira-Hagihara coupling polymerization, and for the first time utilized as an adsorbent for solid-phase extraction (SPE) to enrich seven triazine herbicides from environmental water and fruit juice samples. Comprehensive characterizations confirmed that Im-CMP possessed a stable porous structure, high thermal stability, abundant π-π conjugated framework, and excellent hydrophilicity (water contact angle: 25.1°) derived from imidazolium ionic moieties, which solved the defect of poor aqueous dispersibility of traditional neutral CMPs. Density functional theory calculations and independent gradient model analysis revealed that the high extraction capacity of Im-CMP for triazine herbicides was dominated by efficient π-π stacking interactions, with synergistic contributions from directional weak interactions including C-H···π and N-H···π. Under optimized conditions, the established Im-CMP-SPE-HPLC-MS/MS method exhibited a wide linear range (0.25-250 ng·L⁻¹), low detection limits (0.03-0.11 ng·L⁻¹), high enrichment factors (387-554), and satisfactory recoveries (77.4-110.7%) with good precision. Additionally, the Im-CMP adsorbent demonstrated excellent reusability for nine cycles and consistent batch-to-batch reproducibility. This work not only provides a rational design strategy for ionic-functionalized porous adsorbents for sample pretreatment, but also establishes a sensitive, reliable and practical analytical method for the trace monitoring of triazine herbicides in complex environmental and food matrices, and further expands the application of ionic conjugated microporous polymers in the field of pesticide residue analysis.
Practical considerations for optimizing untargeted metabolomics with Synapt XS HRMS: A tutorial.
Kaiser L, Riester O, Deigner HP
J Chromatogr A · 2026 Jul · PMID 41999695 · Publisher ↗
Metabolomics, the systematic study of small molecules in biological samples, has rapidly emerged as a key discipline for understanding metabolism across organisms. LCHRMS displays the dominant technique for global metabo...
Metabolomics, the systematic study of small molecules in biological samples, has rapidly emerged as a key discipline for understanding metabolism across organisms. LCHRMS displays the dominant technique for global metabolomics due to its high resolution and fast detection. In addition, some instruments offer the option of separating analytes based on their mobility in a carrier gas (ion mobility separation). However, transferring existing protocols between instruments is often limited by differences in hardware, ion mobility capabilities, and instrument generations. In particular, traveling wave ion mobility spectrometry (TWIMS) can induce ion heating and fragmentation, primarily affecting labile polar metabolites (<500 Da), requiring individual adjustment of instrument settings. Because of component redesigns, parameters of previous systems cannot be directly transferred to the Synapt XS; this tutorial provides an overview of modifiable settings. We focus on the application of Synapt XS HRMS for untargeted metabolomics of polar and non-polar metabolites across diverse biological matrices. However, the procedures described for sample preparation, chromatographic separation, and data analysis are largely transferable to other high-performance devices. The tutorial includes step-by-step protocols for sample preparation, chromatographic separation of polar and non-polar compounds, adjustment of TWIMS parameters for labile metabolites, and the use of Progenesis QI, including creation of in-house spectral libraries and integration of existing fragment databases. Additionally, strategies for data acquisition modes and initial quality control and preprocessing are presented and discussed. Together, these methods provide a framework for highly sensitive, reproducible metabolomics analyses and, apart from MS-specific parameters, are broadly applicable to modern mass spectrometers from various manufacturers with comparable performance.
Quantification of 3,5-di-tert-butyl-4-hydroxystyrene migrating from organic materials in contact with drinking water: True occurrence or analytical artefact?
Kalweit C, Berger S, Rapp T
J Chromatogr A · 2026 Jul · PMID 41999694 · Publisher ↗
The occurrence of 3,5-di‑tert‑butyl‑4-hydroxystyrene (S.I) diffusing from cross-linked polyethylene (PE-X) pipes has been a topic of debate among industries, regulatory authorities, and scientists due to inconsistent fin...
The occurrence of 3,5-di‑tert‑butyl‑4-hydroxystyrene (S.I) diffusing from cross-linked polyethylene (PE-X) pipes has been a topic of debate among industries, regulatory authorities, and scientists due to inconsistent findings. This study aimed to clarify the origin of S.I in migration waters and provide analytical recommendations for the certification process of pipe materials. First, it was demonstrated that analysing migration waters by liquid-liquid extraction (LLE) followed by gas chromatography-mass spectrometry (GC/MS), according to EN 15,768 with an injector temperature of 250 °C, significantly biases the measured S.I concentrations, which are due to thermal degradation of 7,9-di‑tert‑butyl‑1-oxaspiro[4,5]deca-6,9-diene-2,8‑dione (S.II). Under these conditions, artificially high concentrations of S.I are obtained. Reducing the injector temperature to 150 °C improves S.I. accuracy, however, a reliable solid-phase microextraction (SPME) method was developed to quantify S.I. independently of S.II. Second, four types of PE-X pipes were evaluated using LLE with injector temperatures of 250 °C and 150 °C, as well as SPME. LLE significantly increases the likelihood of detecting S.I concentrations in the migration waters well above the 0.1 µg/L limit stipulated by the European Commission Implementing Decision. Although the fraction of S.I formed from S.II is small (0.7-2% with LLE), the concentration of S.II itself can reach up to 100 µg/L (legal limit), leading to substantially biased S.I values that exceed 0.1 µg/L. Consequently, materials could fail European certification despite being compliant, which would have significant commercial implications. Therefore, the use of SPME is recommended as an alternative method for analysing S.I in this context.
Synthesis of quaternized PAMAM-grafted magnetic carbon nanotubes as anion exchange adsorbent for highly efficient and rapid extraction of non-steroidal anti-inflammatory drugs from environmental waters.
Hussain I, Muhammad N, Shijiang L … +5 more , Subhani Q, Chengzhu N, Arif U, Yanhong Z, Yan Z
J Chromatogr A · 2026 Jun · PMID 41996944 · Publisher ↗
Extensive prescription and consumption of non-steroidal anti-inflammatory drugs (NSAIDs) in humans and livestock medicines lead to their constant discharge into the natural waters posing deleterious ecological and health...
Extensive prescription and consumption of non-steroidal anti-inflammatory drugs (NSAIDs) in humans and livestock medicines lead to their constant discharge into the natural waters posing deleterious ecological and health concerns. Considering their existence in water as anions, a new adsorbent containing a large proportion of quaternary ammonium groups for anion-exchange micro-magnetic solid phase extraction (AE-µ-MSPE) was designed and synthesized by grafting G of the poly(amidoamine) dendrimers (GPAMAM) onto the magnetic carbon nanotubes (MCNTs) followed by quaternization with glycidol. After successful characterization by NMR, FT-IR, XPS, SEM, TEM, EDX, XRD, VSM, and TGA, the synthesized adsorbent QPAMAM@MCNTs in combination with HPLC-UV was applied for the preconcentration and determination of four NSAIDs in environmental waters. Extraction parameters were optimized using Box-Behnken design (BBD), while desorption conditions were refined via a univariate approach. This anion-exchange adsorbent exhibited high extraction recoveries (86.2-96.5 %) through synergistic hydrogen bonding, π-π stacking, hydrophobic, and anion-exchange/electrostatic interactions. The developed method demonstrated excellent analytical performance, with limits of detection ranging from 0.06 to 0.13 µgL⁻¹, linearity between 0.5-50 µgL⁻¹ (R² = 0.9992-0.9997), enrichment factors of 172-195, and intra-/inter-day RSDs below 7.7 %. Overall, the proposed method offers a rapid, simple, and sensitive approach that can be opted for the selective enrichment and determination of acidic/anionic contaminants including pharmaceuticals and pesticides in environmental waters and potentially other complex matrices such as drug formulations, food, and biological samples.
A copper substitution approach for the selective analysis of chlorophyll-derived porphyrins in modern geological and environmental samples.
Yang R, Xia X, Chen J … +4 more , He C, Zhang Y, Wu J, Shi Q
J Chromatogr A · 2026 Jun · PMID 41990553 · Publisher ↗
The input of chlorophyll provides key information for reconstructing paleoproductivity and tracing diagenesis in geological matrices. However, accurate analysis is hampered as chlorophyll readily suffers from demetallati...
The input of chlorophyll provides key information for reconstructing paleoproductivity and tracing diagenesis in geological matrices. However, accurate analysis is hampered as chlorophyll readily suffers from demetallation and carbon-chain cleavage, leading to a complex mixture of modified Mg(II) porphyrins and porphins. Here, we developed a copper substitution pretreatment that selectively converts native chlorophyll, its derived Mg(II) porphyrins and porphins (chlorophyll-derived porphyrins) into stable Cu(II) porphyrins, thus enabling a comprehensive qualitative and quantitative analysis of the chlorophyll-derived pool. The method was evaluated using model compounds and ultra-performance liquid chromatography coupled with ultra-high-resolution mass spectrometry (UPLCOrbitrap MS). It demonstrated >95% conversion of chlorophyll a with CuCl and 89% for porphin with Cu sheets, whereas non-target Ni(II), V(IV), and Fe(III) porphyrins remained unaffected. Applied to lake sediments, the pretreatment enabled specific analysis of chlorophyll-derived porphyrins against complex geological matrix. This strategy unifies chlorophyll-derived porphyrins into a single detectable form, offering a selective approach for the accurate reconstruction of initial chlorophyll input and composition in geological samples.
Optimization of Zanthoxylum bungeanum essential oil extraction based on response surface methodology and machine learning with activity evaluation.
He J, Zhu Z, Pan X … +3 more , Xie J, Li P, Zhong H
J Chromatogr A · 2026 Jun · PMID 41985368 · Publisher ↗
This study extracted Zanthoxylum bungeanum essential oil via steam distillation, with the extraction process optimized using Response Surface Methodology (RSM) and machine learning techniques. The results indicated that...
This study extracted Zanthoxylum bungeanum essential oil via steam distillation, with the extraction process optimized using Response Surface Methodology (RSM) and machine learning techniques. The results indicated that the optimal conditions predicted by RSM were a distillation time of 92 min, an ultrasonic time of 25 min, and a liquid-solid ratio of 11.6 mL/g, yielding a predicted extraction rate of 2.77 % and an actual rate of 2.92 %. The Artificial Neural Network (ANN) model predicted optimal conditions as a distillation time of 117 min, an ultrasonic time of 30 min, and a liquid-solid ratio of 1:8, giving a predicted yield of 3.01 % and an actual yield of 3.06 %. The Random Forest model suggested conditions of 75 min, 30 min, and a ratio of 1:10, corresponding to a predicted yield of 2.99 % and an actual yield of 2.74 %. The chemical composition of the essential oil obtained under the optimal process was analyzed by GC-MS, identifying γ-terpinene (14.7294 %), 3-carene (14.1696 %), and linalool (13.574 %) as the major components. Antimicrobial assays demonstrated that the essential oil exhibited significant inhibitory effects against S.aureus and E.coli, indicating its potential as a natural antibacterial agent. Furthermore, antioxidant activity tests showed that at a concentration of 40 mg/mL, the ABTS⁺ radical scavenging rate reached 92.81 %. At 80 mg/mL, the scavenging rates for DPPH and hydroxyl radicals were 94.57 % and 68.33 %, respectively, demonstrating strong radical scavenging capacity. The essential oil also displayed considerable ferric ion reducing power.
A chromatographic approach to avoid the matrix effect caused by sodium acetate clusters in the liquid chromatography coupled with electrospray ionization mass spectrometry analysis of free fatty acids in human plasma.
Fukushima Y, Yamamoto K, Machida K … +2 more , Kotani A, Hakamata H
J Chromatogr A · 2026 Jun · PMID 41985367 · Publisher ↗
Liquid chromatography coupled with electrospray ionization mass spectrometry (LC-ESI-MS) is widely used for the analysis of biological samples in pharmacokinetic studies, clinical diagnostics, and therapeutic drug monito...
Liquid chromatography coupled with electrospray ionization mass spectrometry (LC-ESI-MS) is widely used for the analysis of biological samples in pharmacokinetic studies, clinical diagnostics, and therapeutic drug monitoring. However, matrix effects caused by coexisting substances in samples often compromise analytical sensitivity and accuracy. Our study showed that sodium acetate clusters, formed from sodium ions in human plasma and acetate ions in mobile phase, interfered with the detection of free fatty acids (FFAs) in a reversed-phase (RP) LC-ESI-MS analysis. To address this issue, we employed a trimodal column (reversed-phase/weak anion-exchange/weak cation-exchange), which effectively separates the sodium ions from FFAs and successfully reduces the matrix effects. Owing to its high compatibility with conventional octadecylsilyl (ODS) bonded column, enabling easy implementation into existing ODS-based methods, the trimodal column offers a promising new chromatographic strategy for mitigating matrix effect caused by sodium acetate clusters in RPLC-ESI-MS bioanalysis.
(Deep) eutectic solvents in chromatographic and electromigration techniques.
Zhang Q, Meng H, Xue S … +4 more , Tang S, Liu S, Huang Z, Wu Q
J Chromatogr A · 2026 Jun · PMID 41980487 · Publisher ↗
(Deep) eutectic solvents ((D)ESs) have been recognized as a promising class of designer solvents for separation science, offering unique physicochemical properties and structural versatility beyond those of conventional...
(Deep) eutectic solvents ((D)ESs) have been recognized as a promising class of designer solvents for separation science, offering unique physicochemical properties and structural versatility beyond those of conventional solvents. Their integration into chromatographic and electromigration techniques (i.e., capillary electrophoresis and capillary electrochromatography) has created new opportunities for enhancing separation performance while promoting greener analytical practices. This review provides a systematic summary of (D)ES applications in these fields, with particular attention to their diverse functional roles across different separation platforms. We critically examine the physicochemical properties of (D)ESs that drive separation efficiency, elucidate the associated mechanisms, and discuss persistent challenges and debates in the field. The discussion is structured around the specific roles (D)ESs serve within diverse separation systems, aiming to provide a clear and organized perspective on current research progress.
Rapid separation and enrichment of emodin and rhein in Sanhuang Xiexin Decoction by molecularly imprinted nanoparticles and evaluation of DPP-4 inhibitory activity.
Cao C, Li Y, Qi J … +7 more , Liu D, Feng X, Zong Y, Wang Y, Wu X, Wu G, Duan W
J Chromatogr A · 2026 Jun · PMID 41980486 · Publisher ↗
To achieve efficient separation of emodin and rhein, a double-template Fe₃O₄-imprinted polymer (DT-MIP@Fe₃O₄) was successfully synthesized. The characterization (FT-IR, XRD, TGA, SEM, TEM, VSM) demonstrated that the synt...
To achieve efficient separation of emodin and rhein, a double-template Fe₃O₄-imprinted polymer (DT-MIP@Fe₃O₄) was successfully synthesized. The characterization (FT-IR, XRD, TGA, SEM, TEM, VSM) demonstrated that the synthesized DT-MIP@Fe₃O₄ exhibited a core-shell architecture, exhibiting thermal stability up to 270 °C and superparamagnetic characteristics, facilitating separation in 8 s. This material exhibited significant adsorption capacities (31.7823 mg/g and 15.8942 mg/g) and quick adsorption kinetics (equilibrium achieved within 35 min), coupled with the benefits of facile separation, high selectivity, and exceptional reusability. DT-MIP@Fe₃O₄ was utilized as an adsorbent for magnetic solid-phase extraction (MSPE) in conjunction with high-performance liquid chromatography (HPLC) for the simultaneous separation and detection of emodin and rhein in the Chinese herbal medicine SXD. The optimization of parameters influencing MSPE-HPLC was conducted, such as adsorbent dosage, type and volume of desorbent, desorption time, and salt effect. The established method demonstrated exceptional linearity (R² > 0.9999) across the 0.1-100 mg/L, exhibiting high sensitivity and stability. The limits of detection (LOD) and the limits of quantification (LOQ) were established at 0.0092-0.02 mg/L and 0.0307-0.0668 mg/L, respectively. Moreover, the separated fractions demonstrated remarkable hypoglycemic efficacy by DPP-4 inhibition. These findings confirmed the effectiveness of the strategy and indicated that it has considerable prospects in the rapid separation of rhein and emodin from complex Chinese herbal compound, providing a method for the search of natural DPP-4 inhibitors.
A novel solid-phase extraction approach based on π-conjugated polymer-functionalized mesoporous silica nanoparticles for isoquinoline alkaloid purification from Cinnamomum camphora seed kernels.
Yang Y, Yu P, Zeng Z … +7 more , Gao X, Gao Y, Cheng D, Zeng C, Wen X, Gong D, Yan X
J Chromatogr A · 2026 Jun · PMID 41980485 · Publisher ↗
A new class of π-conjugated polymer-functionalized porous silica adsorbents, including a non-carbonized material (SiO@π-CP) and its carbonized derivative (SiO@C-π-CP), was developed through a simple, low-cost synthetic s...
A new class of π-conjugated polymer-functionalized porous silica adsorbents, including a non-carbonized material (SiO@π-CP) and its carbonized derivative (SiO@C-π-CP), was developed through a simple, low-cost synthetic strategy. For the first time, these materials were applied as solid-phase extraction (SPE) sorbents for selective purification of four isoquinoline alkaloids, magnoflorine, laurifoline, lindoldhamine and N-methyldomesticinium, from Cinnamomum camphora seed kernels (CCSK). The integration of π-conjugated polymers with porous silica created abundant adsorption sites, enabling synergistic π-π, electrostatic and hydrogen-bonding interactions, and thus significantly enhancing CCSK alkaloid affinity. Comprehensive characterization confirmed successful functionalization and structural stability. Under optimized static conditions, SiO@π-CP and SiO@C-π-CP exhibited high adsorption capacities of 68.57 and 97.83 mg g⁻¹, respectively, for total CCSK alkaloids, with adsorption behavior well described by pseudo-second-order kinetic and the Freundlich isotherm. Notably, carbonization significantly improved adsorption performance, chemical robustness, and reusability, with both materials maintaining high efficiency after eight adsorption-desorption cycles. Furthermore, SiO@C-π-CP was successfully implemented as a dynamic SPE sorbent, with column adsorption behavior accurately predicted by Adams-Bohart, Thomas, Yoon-Nelson, and BDST models, providing a practical basis for scale-up. Following SPE purification, the purity of CCSK alkaloid increased from 32.97% to 61.59%, with a yield of 73.54%. This work introduces a novel π-conjugated polymer-based SPE platform that combines high selectivity, robustness and scalability, offering a promising strategy for efficient plant alkaloids purification.
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