ANALYTICAL LETTERS
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2023
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IF 2
Zhengyu Wang,Yufeng Hu,Zhiduo Ding,Hao Zhou,Jianye Zhang,Jingjing Zhan,Minghuo Wu
For the identification of trace-level organic nitrogen compounds (NCs) in gasoline, a method consisting of water-assisted dispersive solid-phase extraction (DSPE) and high-performance liquid chromatography-high resolution mass spectrometry was developed in which mixed-mode cation exchange was used as the adsorbent. To increase the DSPE efficiency, water was dispersed into the gasoline to increase the pronation of NCs and enhance the ionic interaction with the adsorbent. After systematic optimization of DSPE conditions, including the adsorbent mass, sample volume, water to gasoline ratio, sample loading time, washing and elution solvents, sensitive determination of NCs (detection limits from 0.1 to 5 ng/L for the 14 analytes) was achieved by this method with a 100-fold enrichment. A number of unknown NC isomers were observed from the extracted ion chromatograms based on the accurate determination of mass-to-charge ratio (m/z), from which two sets of isomers at theoretical m/z of 122.09643 and 136.11208 were selected for identification. By careful elucidation of the product ion spectra of the selected ions, 16 NCs were putatively identified, in which six non-aniline homologs were reported for the first time.
研究领域:
分析化学
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环境科学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2019
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IF 2.813
Shengdong Pan,Jiabin Zhang,Qian He,Xiaohong Chen,Micong Jin
In this study, novel benzenesulfonic acid groups modified magnetic microspheres (Fe 3 O 4 @SiO 2 @poly(4-VB)) were synthesized and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectrometry (FTIR), and vibrating sample magnetometer (VSM). The as-prepared Fe 3 O 4 @SiO 2 @poly(4-VB) was employed as a magnetic-phase extraction (MSPE) adsorbent for rapid determination of paraquat (PQ) and diquat (DQ) in human urine samples coupled with ultra-high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). Moreover, this paper had expounded systematically the mass spectrum cracking mechanisms of PQ and DQ. And a zwitterionic functionalized SIELC Obelisc R column was employed for separation and retention of the above two polar herbicides using 50 mmol/L ammonium formate (pH = 3.7)-acetonitrile as the mobile phase. Besides, the adsorption and desorption conditions of Fe 3 O 4 @SiO 2 @poly(4-VB) toward PQ and DQ were optimized in spiking urine samples to obtain the best adsorption and desorption efficiencies. And the adsorption mechanisms of Fe 3 O 4 @SiO 2 @poly(4-VB) toward PQ and DQ referred to synergetic effect of electrostatic attraction and π-π interaction. Under the optimal conditions, the inter-day and intra-day spiking recoveries of the proposed method were in the range of 86.7–109.9% with RSDs less than 10%. The limits of detection (LODs) were obtained by spiking in blank urine samples at a series of low concentrations and were found to be 0.12 μg/L and 0.14 μg/L for PQ and DQ, respectively, which were lower than the comparing literatures. The developed analytical method was proven to be simple, rapid, sensitive, and accurate for clinical poisoning analysis.
研究领域:
分析化学
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毒理学
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临床医学
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DOI
PubMed
高影响因子
Analytical Methods
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2023
·Vol. 15
·期 26
·3206-3224
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IF 3.1
Yunxi Liu,Tianyu Dong,Kuan Yan,Zhanliang Wang,Genye He,Yufeng Zhang,Congcong Ma,Lu Liu,Wei Chang,Lisi Zhang
Since the World Anti-Doping Agency's (WADA) Prohibited List is updated on an annual basis, screening methods must be continually adapted to align with these changes. In accordance with Technical Document-MRPL 2022, a newly combined, comprehensive, rapid and high-throughput doping control screening method has been developed for the analysis of 350 substances with different polarities in human urine using ultra-high performance liquid chromatography coupled with Q Exactive Plus Hybrid Quadrupole-Orbitrap mass spectrometer (UPLC-QE Plus-HRMS) and ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometer (UPLC-QQQ-MS). The limits of detection were in the range of 0.12–50 ng mL−1 for beta-2 agonists, hormone and metabolic modulators, narcotics, cannabinoids and glucocorticoids, 0.1–14 ng mL−1 for the manipulation of blood and blood components, beta blockers, anabolic agents and hypoxia-inducible factor (HIF) activating agents, and 2.5–100 000 ng mL−1 for substances of Appendix A, diuretics & masking agents and stimulants. The sample preparation consisted of two parts: one is the dilute & shoot part analyzed in UPLC-QQQ-MS, another is a mixture of the dilute & shoot part and a liquid–liquid extraction part of hydrolyzed human urine analyzed in UPLC-QE Plus-HRMS in full scan mode with polarity switching and parallel reaction monitoring (PRM) mode. The method has been fully validated for doping control purposes. All the substances were compliant with WADA's required 1/2 minimum requirement performance level (MRPL) or minimum reporting level (MRL), and this method was successfully used in the 2022 Beijing Winter Olympic Games and Winter Paralympic Games for anti-doping purpose.
研究领域:
分析化学
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运动科学
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药理学
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法医学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2024
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IF 3.1
Jiayue Wang,Feixu Qin,Hongjin Wang,Lu Wang,Caihong Li,Lixin Sun
Senecio scandens Buch.-Ham., a traditional Chinese medicine commonly used clinically, exhibits various pharmacological properties, including anti-inflammatory, anti-tumor, antiviral, and antibacterial activities. However, its water extracts' chemical components and metabolites are inadequately understood, limiting further research. In this study, the chemical components and metabolism processes of Senecio scandens, both in vivo (plasma, feces, urine, and bile) and in vitro (gut microbiota and liver microsomes), were characterized based on ultra-high performance liquid chromatography coupled with hybrid quadrupole-orbitrap high-resolution mass spectrometry. Additionally, metabolites detectable in fecal samples and intestinal microbiota incubated but absent in liver microsomes were identified as characteristic metabolites of intestinal microbiota. The targets of the characteristic metabolites of intestinal microbiota were collected, followed by exploration of potential pathways through KEGG enrichment analysis. As a result, a total of 133 chemical components were preliminarily identified, including 35 organic acids, 21 alkaloids, 19 flavonoids and their glycosides, 17 phenylpropanoids, 10 jacaranda ketones, and 31 other compounds. Notably, 12 of these were potentially novel compounds. In addition, 39 prototype components in rats and 109 metabolites were identified and characterized, including 102 in vivo and 52 metabolites in vitro (51 in rat gut microbiota and 24 in rat liver microsomes). The main metabolic pathways include oxidation, reduction, hydrolysis, methylation, glucuronidation, sulfonation, and acetylation reactions. Furthermore, KEGG enrichment analysis revealed that the characteristic metabolites of intestinal microbiota may be related to the ErbB, FoxO, mTOR, and MAPK signaling pathways, exhibiting anti-inflammatory and anti-tumor effects. In summary, the chemical components and metabolites of Senecio scandens were comprehensively identified using a rapid and accurate method, providing a scientific basis for the in-depth study of the material basis and its clinical application of Senecio scandens .
研究领域:
药理学
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代谢组学
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生物信息学
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中药学
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化学生物学
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微生物学
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DOI
PubMed
高影响因子
FOOD RESEARCH INTERNATIONAL
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2026
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IF 8.8
Kangyan Zhang,Siyu Wang,Huiru Zhang,Jing Ming,Wanjun Long,Haiyan Fu
Artemisiae Argyi Folium (AAF) is a medicinal and edible herb whose quality is dependent on its geographical origin and aging years. This study employed untargeted metabolomics based on GC–MS and UHPLC-HRMS to identify its geographical origin and aging years. First, we employed our proprietary AntDAS platform to fully analyze the mass spectrometry data and screen for key differential metabolites. Analysis identified 58 geographical origin-related metabolites (35 non-volatile and 23 volatile). Notably, the chemical profiles of the two Dao-di production regions differed markedly. Samples from Nanyang (Henan) were characterized by high abundances of endo -borneol, terpinen-4-ol, eucalyptol, 3,4-dicaffeoylquinic acid, phellopterin, and quercetin, whereas these compounds were found in low abundance in samples from the other Dao-di production region, Qichun (Hubei). Furthermore, 27 metabolites with aging-year differences were identified, comprising 18 non-volatile and 9 volatile compounds, and the aged AAF compared to fresh AAF showed significantly enriched chemical components. Regarding the aging effect, the contents of eucalyptol and 5-methyl-decane were highest in the 5-year samples. Endo -borneol showed higher levels in both 1-year and 5-year samples, with its content in 3-year samples being intermediate. In contrast, n-hexadecanoic acid and phytol were more abundant in samples aged for over 5 years. Finally, using these differential metabolites, OPLS-DA models achieved 100.0% accuracy in geographical origin classification and over 94.4% accuracy for aging year discrimination. This study provides a chemical basis for the geographical origin traceability and aging year identification of food-drug homologous products.
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2019
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IF 3.858
Enming Miao,Nazhen Zhang,Shiwei Lu,Yufeng Hu,Lin Fu,Hao Zhou,Jingjing Zhan,Minghuo Wu
A simple magnetization method was developed for the preparation of magnetic materials from conventional solid phase packing though coprecipitation and solvothermal approaches. And the prepared magnetic materials were used for magnetic solid phase extraction (MSPE) of biogenic amines (BAs) from beers. Furthermore, to improve the analytical throughput, a solid phase “on-situ” quadraplex isotope dimethyl labeling method was developed for the quantification of BAs by liquid chromatography-high resolution mass spectrometry (LC HRMS). Compared to conventional in-solution labeling, the “on-situ” labeling could simplify the sample preparation procedure and efficiently remove the residuals such as inorganic salts and excessive labeling reagents. The quadraplex labeling, which enabled three real samples and one internal standard sample to be analyzed simultaneously in a single LC HRMS run. For the tested 8 BAs (cadaverine, phenethylamine, spermine, spermidine, tyramine, histamine, putrescine and tryptamine), LODs of 0.02–0.05 μg/L and LOQs of 0.05–0.1 μg/L were achieved at good reproducibility (RSD of 0.5–4.6% and 2.2–7.0% for intra- and inter-day reproducibility, respectively). With this method, six beer samples were analyzed, and these 8 BAs were all detected in the range of low μg/L to 2.9 mg/L, which were lower than maximal residual level (MRL) required in the regulations of China and EU.
研究领域:
分析化学
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食品科学
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质谱分析
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DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
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2023
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IF 8.2
Qiuyang Huang,Xiaoling Zang,Zhiwei Zhang,Hang Yu,Baoyan Ding,Zhuangzhuang Li,Simin Cheng,Xin Zhang,Mustafa R.K. Ali,Xue Qiu,Zhihua Lv
The discovery of new anti-cancer drugs targeting the PD-1/PD-L1 pathway has been a research hotspot in recent years. In this study, biological affinity ultrafiltration (BAU), UPLC-HRMS, molecular dynamic (MD) simulations and molecular docking methods were applied to search for endogenous active compounds that can inhibit the binding of PD-L1 to PD-1. We screened dozens of potential cancer related endogenous compounds. Surprisingly, cyclic adenosine monophosphate (cAMP) was found to have a direct inhibitory effect on the PD-1/PD-L1 binding with an in vitro IC 50 value of about 36.4 ± 9.3 μM determined by homogeneous time-resolved fluorescence (HTRF) assay. cAMP could recover the proliferation of Jurkat T cells co-cultured with DU-145 cells and may suppress PD-L1 expression of DU-145 cells. cAMP was demonstrated to bind and induce PD-L1 dimerization by FRET assay, and also predicted by MD simulations and molecular docking. The finding of cAMP as a potential inhibitor directly targeting the PD-1/PD-L1 interaction could advance our understanding of the activity of endogenous compounds regulating PD-L1.
研究领域:
肿瘤学
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药理学
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分子生物学
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细胞生物学
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DOI
PubMed
高影响因子
SCIENCE OF THE TOTAL ENVIRONMENT
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2020
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IF 6.551
Yanping Xian,Ming Liang,Yuluan Wu,Bin Wang,Xiangchang Hou,Hao Dong,Liya Wang
Most of the reported magnetic adsorbents are difficult to absorb multi-class of per - and polyfluoroalkyl substances (PFASs), especially the short-chain PFASs. In this work, a novel fluorine and nitrogen functionalized magnetic graphene (G-NH-FBC/Fe 2 O 3 ) was first synthesized and characterized by scanning electron microscope (SEM), Fourier Transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). The as-prepared G-NH-FBC/Fe 2 O 3 was utilized as adsorbents for the magnetic solid-phase extraction (MSPE) of 19 PFASs from water and functional beverages and showed excellent adsorption capacity probably due to the hydrophobic interaction. Under the optimal pretreatment and instrumental conditions, a selective and sensitive high performance liquid chromatography Orbitrap high resolution mass spectrometry (HPLC-Orbitrap HRMS) method was developed for the determination of PFASs. Results indicated that the proposed method had favorable linearity (R 2 ≥ 0.994) within a wide range of concentrations. Limit of detection (LOD) and limit of quantification (LOQ) for the developed method ranged from 3 ng/L to 15 ng/L and 10 ng/L to 49 ng/L, respectively. Finally, the method was successfully applied to determine PFASs in drinking water , river water, tap water , factory drainage and functional beverages with recoveries ranging from 71.9% to 117.6% and relative standard deviation of <10%. The prepared G-NH-FBC/Fe 2 O 3 was easy to recycle and could be reused for five times without significant decrease in extraction recoveries of PFASs. These results demonstrated that this novel magnetic G-NH-FBC/Fe 2 O 3 could efficiently enrich PFASs and the proposed method is reliable and robust for the determination of PFASs in water and beverage samples.
研究领域:
环境科学
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分析化学
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DOI
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2026
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IF 4.1
Liu Feng,Yu Decong,He Kun,Song Yanan,Li Yichao,Gao Haoxuan,Wu Bing,Li Xiaoyu,Zhao Ji,Xu Fei,Yang Huifang
The widespread use of neonicotinoids has raised growing concerns about their potential health risks. In this study, we developed a robust and high-throughput analytical method based on liquid-liquid extraction (LLE) and dispersive solid-phase extraction (dSPE), followed by high-performance liquid chromatography-quadrupole-Orbitrap high-resolution mass spectrometry (HPLC-Q-Orbitrap HRMS) for the simultaneous determination of 11 neonicotinoids and their 6 metabolites in human urine. After pretreatment of LLE and dSPE, qualitative and confirmatory analysis was achieved using tMS 2 acquisition of HPLC-Q-Orbitrap HRMS, and quantitative analysis was performed using isotope-labeled internal standards and matrix-matched calibration curves. The method was validated with good linearity ( R 2 > 0.9975), recoveries of 75.8%~118.9% (RSDs < 15%), and detection limits of 0.001~0.06 μg/L. The established method was successfully applied to urine samples of community-dwelling elderly population individuals ( n = 150) and to a suspected case of acute acetamiprid poisoning in Ningxia, China. The results showed that thirteen neonicotinoids and metabolites were detected in the elderly cohort, and the poisoning incident was confirmed to be caused by acetamiprid and its metabolite N-desmethyl-acetamiprid. Meanwhile, Spearman correlation analysis indicated significant positive correlations between parent compounds and their metabolites for all analytes except acetamiprid, and a strong correlation between clothianidin and thiamethoxam, suggesting shared exposure sources or common metabolic pathways. The established method is sensitive, accurate, and high-throughput, and has proven reliable for human biomonitoring and health risk assessment of neonicotinoid exposure. Graphical
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高影响因子
INDUSTRIAL CROPS AND PRODUCTS
·
2023
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IF 5.9
Jia-Ni Zhang,Meng-Han Ma,Xing-Ling Ma,Feng-Lian Ma,Qing-Yu Du,Jia-Nan Liu,Xing-Cai Wang,Qi-Peng Zhao,Yong-Jie Yu,Yuanbin She
The effect of drying methods on the variations of volatile, semi-volatile, and involatile compounds in Elaeagnus angustifolia L. (E.A.) flower was comprehensively investigated by using gas chromatography-mass spectrometry (GC-MS) and ultrahigh performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) based untargeted metabolomics combined with our recently developed automatic data analysis software AntDAS for the first time. About 21 volatile compounds, 44 semi-volatile compounds, and 17 involatile compounds were identified and showed significant differences among drying methods. Chemometric methods like principal components analysis (PCA), and partial least squares-discriminant analysis (PLS-DA) were used in combination with heatmap analysis to reveal the relationship between compound compositions and drying methods. Finally, it was concluded that room-temperature drying is more conducive to preserving volatile compounds in E.A. flower, and hot air drying is better for preserving semi-volatile and involatile compounds. This work can provide guidelines for industrial processes of E.A. flower.
研究领域:
植物学
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分析化学
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药用植物研究
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DOI
高影响因子
Applications in Energy and Combustion Science
·
2025
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IF 6
Zhongyue Zhou,Haoran Liu,Xinghua Liu,Chih-Hao Chin
Coke deposition and catalyst deactivation represent significant challenges in catalytic research, yet the mechanisms underlying their formation remain inadequately understood. Herein, we employed the HZSM-5 catalyzed conversion of furfural as a model reaction and, using a newly developed online high-resolution mass spectrometry (HRMS) technique, directly detected a broad spectrum of oxygenated polycyclic aromatic hydrocarbons (OPAHs) under reaction conditions. Solid-state NMR further revealed the functional group architectures of OPAH side chains in condensed-phase coke, while density functional theory (DFT) calculations elucidated plausible formation and transformation pathways. These complementary approaches establish that highly active OPAHs serve as crucial intermediates in the coke deposition process. We propose a novel mechanism in which light OPAHs, orginating from small-molecule products, undergo rapid polymerization at the active sites to yield larger polycyclic aromatic hydrocarbons, traditionally classified as coke. This newly identified mechanism highlights the unexpectedly rapid coking during the catalytic pyrolysis of biomass, and underscores the significant role of OPAHs in catalyst deactivation. By providing molecular-level insights into coke growth, this study lays a foundation for strategies to suppress coke formation, thereby improving the efficiency and sustainability of catalytic conversion technologies for biomass utilization.
研究领域:
催化化学
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生物质能源
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石油化学
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分析化学
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理论化学
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产品关联
DOI
高影响因子
Frontiers in Microbiology
·
2024
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IF 4
Xu Chong,Pan Danyang,Zhang Dexiang,Lin Lin,Chen Yiti,Liang Shuangcheng,He Jingyu
Introduction: Microorganisms as a component of scalp ecosystem play a vital role in human scalp health. Soapberry pericarp is employed in improving scalp health, and its content of active ingredients could be enhanced resulted in fermentation. This study aims to investigate the effect of the fermentation filtrate from soapberry pericarp on the diversity of scalp microorganisms.Methods: The components in fermentation filtrate from soapberry pericarp were analyzed by HPLC-Q-Orbitrap HRMS, and 16S and ITS sequences of 198 samples from three different used stages (Day 0, Day 7, Day 28) were sequenced using the Illumina Novaseq platform. Microbial diversity was assessed using alpha diversity (Chao1 and Shannon indexes) and beta diversity (weighted unifrac and unweighted unifrac). Principal coordinate analysis (PCoA) and linear discriminant analysis (LDA) effect size analysis (LEfSe) were used to visualize microbial variation among different stages.Results: There were 22 components were identified in the fermentation filtrate from soapberry pericarp by HPLC-Q-Orbitrap HRMS. The alpha-diversity and beta-diversity analyses showed that scalp microbial diversity and composition were influenced by the fermentation filtrate of soapberry pericarp. Based on functional analysis, this study found an enrichment of healthy scalp-related bacterial pathways, such as amino acid, nucleoside, and nucleotide biosynthesis, while a decrease in fungal pathogenesis pathways, specifically saprotroph and symbiotroph pathways, was observed.Discussion: The study described about the complex community dynamics of human scalp microorganisms during the stages of using the fermentation filtrate from soapberry pericarp. This result will help rationally utilize the fermentation filtrate from soapberry pericarp to keep or improve human scalp health.
研究领域:
微生物学
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药学
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生物技术
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皮肤科
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DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）