Bioanalysis
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2025
·
IF 1.8
You-Rim Lee,Jae Guk Kim,Soo Joo Lee,Jiyeong Lee,Hee-Gyoo Kang
Aim Ischemic stroke (IS) occurs when a clot obstructs cerebral blood flow, leading to potentially irreversible damage. Metabolites, as the end products of cellular metabolism, can reflect pathological changes in the body. This study aimed to characterize serum metabolic alterations associated with acute ischemic stroke.Method Participants were divided into discovery and validation sets, each comprising healthy controls and IS patients. In the discovery set, untargeted serum metabolomic profiling was performed using liquid chromatography – tandem mass spectrometry. Metabolites showing significant intergroup differences were selected as biomarker candidates and quantitatively validated in the independent set. Diagnostic performance was assessed using receiver operating characteristic (ROC) curve analysis.Results Three metabolites – cytidine, decanoyl-L-carnitine, and 2-hydroxyestradiol – were identified as significantly altered in IS patients. Cytidine and 2-hydroxyestradiol demonstrated excellent diagnostic performance (AUCs of 0.968 and 0.929, respectively), while decanoyl-L-carnitine showed good performance (AUC = 0.808).Conclusion The three metabolites exhibit significant alterations in acute ischemic stroke patients and provide insight into disease-associated metabolic changes. Their validation lays the groundwork for future exploratory studies investigating potential biomarkers.
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ANALYTICA CHIMICA ACTA
·
2026
·
IF 6.1
Yali Yang,Hui Ding,Kaijun Quan,Hongwei Zhao,Mingxia Sun,Zhimin Yang,Xiuhui Liu,Hongdeng Qiu,Jia Chen
Background To address the limitations of traditional single-mode stationary phases in separating complex samples, mixed-mode or multi-mode chromatographic stationary phases, which can provide two or more interaction mechanisms, have attracted extensive research interest. Among them, sulfonated pyrene derivatives present a promising candidate ligand, as they synergistically retain the hydrophobicity and π-π interaction capability of the pyrene moiety along with the hydrophilicity and strong cation-exchange capacity provided by the sulfonic acid groups. This synergistic multi-mechanism design significantly enhances separation selectivity for diverse and complex components. Results A pyrene trisulfonic acid-functionalized silica stationary phase (Sil-PyTSa) was successfully prepared and evaluated. In hydrophilic interaction liquid chromatography (HILIC) mode, Sil-PyTSa could efficiently separate nucleobases and nucleosides, ginsenosides, and alkaloids. For nucleobases and nucleosides, it utilized hydrophilic, electrostatic, and π-π interactions, showing superior retention and selectivity over a control HILIC column. In reversed-phase liquid chromatography (RPLC) mode, favorable separation of PAHs was achieved via hydrophobic and π-π interactions, enabling faster analysis and lower solvent consumption than a C18 column. In ion-exchange chromatography (IEC) mode, baseline separation of 14 rare earth elements (REEs) and removal of Fe/U impurities were accomplished. The column efficiency reached 95,920 N/m for naphthalene. Additionally, Sil-PyTSa achieved effective separation for REEs and iron (Fe) in a simulated NdFeB leaching solution and detected nucleobases and nucleosides in Angelica, indicting promising potential for analyzing complex matrices. Significance and novelty This work developed a novel multi-mode chromatographic stationary phase with multiple interactions mechanisms to enable high-performance separations in HILIC, RPLC, and IEC modes. It demonstrates good separation efficiency and selectivity, low solvent consumption, and high stability. This offers a versatile and green solution for the separation of complex samples with diverse analytes.
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FOOD CHEMISTRY
·
2026
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IF 10.4
Bo Wang,Feng Zhao,Zheng Zhou,Ji Wang,Lei Qin,Xuhui Huang
Studied hazardous compound changes in the thermal processing of 7 animal foods. • Hazards: acrylamide, 5-hydroxymethylfurfural, 13 heterocyclic aromatic amines. • AA, 5-HMF, and 13 HAAs in all animal foods increased with roasting temperature. • Low moisture and high carbs promoted AA; high protein favored HAAs. • Amino acids and dipeptides had negative correlations with hazardous compounds. The thermal processing of food is often accompanied by changes in composition and the generation of hazardous compounds. However, the unclear mechanisms linking food composition to related hazardous compounds hinder the advancement of inhibition technologies for hazardous compounds formed during thermal processing. In this paper, the mechanisms of 15 kinds of associated hazardous compounds produced by 7 different animal-derived food samples during the roasting process were investigated. When the roasting temperature was 260 °C, mutton exhibited the highest acrylamide content at 0.11 μg/g, chicken had the highest HAAs (heterocyclic aromatic amines) content at 0.17 μg/g, and Antarctic krill showed the highest 5-hydroxymethylfurfural content at 0.72 μg/g. notably, the compounds closely related to the production of associated hazards during thermal processing include amino acids, small dipeptides, and certain carbohydrate compounds. The results of this study have positive significance in improving food safety and optimizing production processes. Download: Download high-res image (136KB) Download: Download full-size image
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Advanced Science
·
2023
·Vol. 10
·期 9
·2206851
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IF 15.1
Peidong Du,Yanzhe Shen,Baoli Zhang,Shan Li,Minzheng Gao,Ting Wang,Xiaokang Ding,Bingran Yu,Zhen-Gang Wang,Fu-Jian Xu
Photodynamic therapy (PDT) is a light triggered therapy by producing reactive oxygen species (ROS), but traditional PDT may suffer from the real-time illumination that reduces the compliance of treatment and cause phototoxicity. A supramolecular photoactive G-quartet based material is reported, which is self-assembled from guanosine (G) and 4-formylphenylboronic acid/1,8-diaminooctane, with incorporation of riboflavin as a photocatalyst to the G4 nanowire, for post-irradiation photodynamic antibacterial therapy. The G4-materials, which exhibit hydrogel-like properties, provide a scaffold for loading riboflavin, and the reductant guanosine for the riboflavin for phototriggered production of the therapeutic H 2 O 2 . The photocatalytic activity shows great tolerance against room temperature storage and heating/cooling treatments. The riboflavin-loaded G4 hydrogels, after photo-irradiation, are capable of killing gram-positive bacteria (e.g., Staphylococcus aureus ), gram-negative bacteria (e.g., Escherichia coli ), and multidrug resistant bacteria (methicillin-resistant Staphylococcus aureus ) with sterilization ratio over 99.999%. The post-irradiated hydrogels also exhibit great antibacterial activity in the infected wound of the rats, revealing the potential of this novel concept in the light therapy.
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Genes
·
2022
·Vol. 13
·期 5
·878
·
IF 4.141
Xiuying Lin,Qianhui Zhang,Yichao Qin,Qisheng Zhong,Daizhu Lv,Xiaopeng Wu,Pengcheng Fu,Huan Lin
Triple quadrupole mass spectrometry coupled to liquid chromatography (LC-TQ-MS) can detect and quantify modified nucleosides present in various types of RNA, and is being used increasingly in epitranscriptomics. However, due to the low resolution of TQ-MS and the structural complexity of the many naturally modified nucleosides identified to date (>160), the discrimination of isomers and mass-analogs can be problematic and is often overlooked. This study analyzes 17 nucleoside standards by LC-TQ-MS with separation on three different analytical columns and discusses, with examples, three major causes of analyte misidentification: structural isomers, mass-analogs, and isotopic crosstalk. It is hoped that this overview and practical examples will help to strengthen the accuracy of the identification of modified nucleosides by LC-TQ-MS.Keywords:nucleoside misidentification;RNA modification;epitranscriptomics;LC-MS/MS;tRNA;HILIC
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JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Yan Wu,Kaixing Luo,Yanjuan Liu,Wei Chen,Zhengwu Bai,Sheng Tang
Developing a versatile stationary phase to achieve the purpose of efficiently separating various target analytes is of great significance. In this work, ureido/dodecyl dual-functionalized silica (Sil-Ur-DD) was synthesized and employed as a new mixed-mode stationary phase for high-resolution chromatographic analysis. It was observed that multiple interactions, including hydrophobic, hydrophilic, hydrogen bonding, electrostatic and π-π interactions, contributed to the retention. Nucleosides and nucleobases could be effectively determined in hydrophilic interaction chromatography mode, and the separation performance of the Sil-Ur-DD was found to be even superior to that of the commercial XAmide column. Environmental endocrine disruptors, including alkylphenols, bisphenols, steroid hormones and phthalates, were more favorably separated in reversed-phase chromatography mode with highly aqueous mobile phases compared with the commercial C18-silica column. The experimental results indicated that the combined effect of ureido and long-chain alkyl groups obviously enhanced separation efficiency and selectivity. More significantly, the proposed method concerning the preparation of an efficient separation material with powerful separation ability is economical and environmentally friendly, which provides a proven and effective way for the recycling and utilization of the discarded chromatographic packing materials, thereby showing a good application prospect.
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SENSORS AND ACTUATORS B-CHEMICAL
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2022
·
IF 9.221
Shuzhen Dou,Zhongshun Wang,Qiye Chen,Nan Lu
The high sensitivity of surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS) analysis depends on the enhancement of the signal intensity and the reduction of the background. Here, high-density Si nanotips were prepared as SALDI-MS substrate by taking template-free reactive ion etching for sensitive detection . The high-density Si nanotips act as tiny antennas to concentrate the laser energy and generate photo-induced electrons on a small area, which promotes desorption and ionization of molecule, enhancing the signal intensity. Additionally, the high stability of Si nanotips under laser irradiation ensures low background interference. The applicability of the substrate was demonstrated by the detection of various small molecules, e.g., fatty acids, amino acids , environmental pollutants and drugs. In addition, this substrate can be successfully applied for detecting trace small molecules in complex sample, such as 10 −9 M verapamil in serum and 10 −12 M crystal violet in lake water. Moreover, the banned fungicides left on the fish skin was also detected. The substrate is compatible with imaging, and the endogenous and exogenous substances in fingerprint were visualized by MS imaging. These results demonstrate the easily prepared high-density Si nanotips SALDI-MS substrate is of high detection sensitivity and great value toward large-scale practical applications.
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JOURNAL OF CHROMATOGRAPHY A
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2022
·
IF 4.601
Shitao Feng,An Zhang,Fengshou Wu,Xiaogang Luo,Juan Zhang
This study constructed boronic acid grafted Zr-MOF (BA-Zr-MOF) by a simple pre-installation strategy through mixed organic ligands. Typically, BA-Zr-MOF was prepared by one-step hydrothermal method used for enrichment of cis -diol-containing nucleosides through pipette tip solid-phase extraction (PT-SPE) followed by detection of high-performance liquid chromatography. It is worth mentioning that BA is well assembled into MOF and cis -diol-containing compounds can be efficiently and selectively enriched by abundant boronic acid groups. Three groups of different types of compounds were used to evaluate their selectivity and the results showed the excellent selectivity to cis -diol-containing compounds of as-prepared adsorbent. The BA-Zr-MOF adsorbent possesses a high adsorption capacity, which can reach 86.40 mg g −1 for adenosine. Under the optimal extraction condition, a PT-SPE-HPLC method based on BA-Zr-MOF for analysis of nucleosides was established. The linear range of the four nucleosides is 0.01 to 50 µg mL −1 with R 2 ≥ 0.99 and the detection limits (LODs) are estimated at between 0.005-0.012 µg mL −1 . The recoveries in urine were used to test the reliability of the analytical methods, which ranged from 82.8% to 117.1%, with intra-day relative standard deviations (RSDs) ranged from 0.1% to 4.2% and the inter-day RSDs ranged from 0.2% to 6.2%. All the results show that the pre-installation strategy based on dual ligands is an alternative to fabricate MOF composite material and BA-Zr-MOF is a promising material for the analysis of cis -diol-containing biomolecules.
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JOURNAL OF CHROMATOGRAPHY A
·
2021
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IF 4.759
Chao Fan,Bei Liu,Hui Li,Kaijun Quan,Jia Chen,Hongdeng Qiu
In this work, three new mixed-mode stationary phases were prepared, based on different ratio of N-vinyl pyrrolidone (NVP) copolymerized together with undecylenic acid (UA) on silica microspheres surface without silanization, which named Sil@NVPUA series. The combination of NVP and UA rendered the Sil@NVPUA suitable for reversed-phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC), and shown excellent methyl, planar, isomers and ion selectivity. Five types of model analytes including eight polycyclic aromatic hydrocarbons, six alkylbenzenes, eight nucleosides and nucleobases, seven ginsenosides and five oxazolidinones can be well separated on this stationary phase. The preparation method of NVP and UA modified silica-based stationary phase is simple, and it also provides a new idea for the design of synthetic polymers to develop mixed-mode chromatography.
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JOURNAL OF CHROMATOGRAPHY A
·
2021
·
IF 4.759
Houmei Liu,Pian Jin,Mi Jiang,Yu Duan,Guozheng Zhu,Hui Yu,Hongdeng Qiu
In this work, for the first time five amine-ligands including mono-amine, di-amine, tri-amine, secondary and tertiary amine, were functionalized on mesoporous micro-silicas and developed as stationary phases for hydrophilic interaction liquid chromatography (HILIC). The investigations about the retention mechanisms, effects of different chromatographic conditions and stability were systematically conducted. Three kinds of polar and hydrophilic compounds (saccharides, sulfonamides, nucleosides and nucleobases) were selected as probe molecules to evaluate their separation performances. Among the five stationary phases, only aminopropyl-bonded silica has already gained wide developments and applications. Whereas, there are no related researches about the other four to be utilized as separation media. By a series of chromatographic evaluations, the results revealed the other four mesoporous micro-silica materials functionalized with di-amine, tri-amine, secondary and tertiary amine, had great potential to be explored as novel stationary phases of HILIC. Particularly, the two stationary phases functionalized with di-amine and tri-amine exhibited outstanding separation and retention abilities. This work offered some insights on the understanding of retention in HILIC mode and provided us possibility to explore other amine-based HILIC stationary phases.
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Analytical Methods
·
2020
·Vol. 12
·期 46
·5635-5641
·
IF 2.596
Dan Liu,Lili Meng,Liping Huang,Shipeng Luo,Guohua Zhang
Chitosan is a considerably versatile and promising biomaterial and can easily form a 3D hierarchical porous scaffold. In this work, a novel boronate-affinity monolithic column modified with a boronic acid–chitosan complex was prepared and characterized by different methods such as Fourier transform infrared spectroscopy, scanning electron microscopy, thermal gravimetric analysis, specific surface area analysis and pore size distribution analysis. The synthesized monolithic column was used for polymer monolithic microextraction combined with high performance liquid chromatography for the simultaneous determination of cytidine, uridine, inosine, and guanosine in milk powder samples. Several parameters affecting extraction efficiency, including the eluent proportion, eluent flow rate, sample flow rate, sample volume, and sample pH were investigated. The boronate-affinity monolithic column showed high enrichment ability due to the selective formation of cyclic borate esters between nucleosides and boronic acid groups at high pH and the release of cyclic borates at low pH values. Under the optimum operating conditions, the linear range was 0.1–50 μg mL−1, and the correlation coefficients were in the range of 0.9993–0.9994. The LOD and LOQ were in the range of 0.0027–0.0034 and 0.0090–0.011 μg mL−1, respectively. In addition, the results of recovery and relative standard deviation were satisfactory.
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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2020
·
IF 0.992
Shiyun Tang,Yuanxing Duan,Feng Chang,Wei Jiang,Fengmei Zhang,Zhihua Liu,Yuting Yang,Chunbo Liu,Yingzhuang Chen
The porous layer open-tube (PLOT) columns, which were characterized by their considerable specific surface area and high permeability, have attracted a growing attention from researchers in liquid chromatography. In this work, a hydrophilic PLOT column rich in carboxylic acid functional groups was successfully synthesized in capillary with an inner diameter of 200 µm by thermally initiated aqueous two-phase polymerization. Methacrylic acid (MAA) areas monomers that responsible for the introduction of polar functional groups, and poly(ethylene glycol) diacrylate (PEGDA) are as cross-linker. The optimized PLOT column has a uniform, moderately thick porous layer, which is tightly bonded to the inner wall without any detachment. The hollow structure gives the PLOT column good permeability, which facilitates fast mass transfer. The systematical evaluations of the resulting PLOT columns were performed by using polar analytes including nucleosides, bases, amides, phenols and carboxylic acids. Those results demonstrated excellent separation performance for the small polar molecules. Compared to the poly(PEGDA) PLOT column, the hydrophilic retention of analytes on poly(PEGDA-co-MAA) porous layer open-tube column is significantly improved by the introduction of carboxylic acids. Furthermore, with modified nucleosides and chlorophenols being disease markers and the persistent pollutant of wide concern, respectively, the separation was optimized and the linear range of the quantitative analysis was examined for both targets. which indicates the potential application of such PLOT column for analysis of real samples.
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