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Structural Characterization of Anhydroicaritin Glycosides Using ESI-FT-ICR mass spectrometry

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Chinese Chemical Letters 2002年第11期13卷 1103-1106页

作者： Shao Xiang XIONG Dan PU Bin XIN Guang Hui WANG Beijing mass spectrometry center Center for Molecular ScienceChinese Academy of SciencesBeijing 100080

Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) was used to determine the structures of anhydroicaritin glycosides by the MS/MS experiments of anhydroicaritin glycosides and their methylated derivatives. With high accuracy FT-ICR-MS provides much information about the structures of compounds, FT-ICR-MS shows the great potential application in the structural characterization of unknown compounds.

关键词： mass characterization anhydroicaritin glycosides FT-ICR-MS.

Quantitative analysis of urinary endogenous markers for the treatment effect of Radix Scutellariae on type 2 diabetes rats

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Chinese Chemical Letters 2017年第6期28卷 1214-1219页

作者： Guang-Yue Hou Li-Hui Men Lu Wang Zhong Zheng Zhi-Qiang Liu Feng-Rui Song Zhong-Ying Liu National center for mass spectrometry in Changchun & Jilin Province Key Laboratory of Chinese Medicine Chemistry and mass spectrometry Changchun Institute of Applied ChemistryChinese Academy of Sciences School of Pharmaceutical Sciences Jilin University

The effect of Radix Scutellariae treated on type 2 diabetic rats has been investigated by a liquid chromatography coupled with tandem mass spectrometry（LC-MS/MS） based urinary quantitative *** this research,multiple reactions monitoring mode of MS/MS in LC-MS/MS analysis was used to quantitatively analyze the concentrations of 7 endogenous compounds in urine of normal control group,type 2 diabetic model group and Radix Scutellariae-treated group,and multivariate statistical analysis was utilized for MS data *** above-mentioned three groups can be distinguished via pattern *** obtained results indicated that Radix Scutellariae affect the urinary metabolic profiling of type 2 diabetic rats on the polyol pathway,protein glycation reaction and amino acids metabolism *** to these results,Radix Scutellariae should have the pharmacological effect on preventing or delaying the onset and progression of diabetes and its complications.

关键词： LC-MS/MS Endogenous markers Multivariate statistical analysis Type 2 diabetic complications Radix Scutellariae

Screening the anti-gout traditional herbs from TCM using an in vitro method

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Chinese Chemical Letters 2016年第11期27卷 1701-1707页

作者： Wei-Jia Chen Yi Wu Xin Zhao Shu Liu Feng-Rui Song Zhong-Ying Liu Zhi-Qiang Liu School of Pharmaceutical Sciences Jilin University National center of mass spectrometry in Changchun & Jilin Province Key Laboratory of Chinese Medicine Chemistry and mass spectrometry Changchun Institute of Applied ChemistryChinese Academy of Sciences

The aim of this work was to evaluate the ability of 33 herbal extracts in inhibiting the acute inflammation and xanthine oxidase （XOD） activity. The anti-inflammation effects of the herbal extracts were detected by an in vitro cell model, which was established by stimulating human umbilical vein endothelial cells （HUVEC） using sodium urate （MSU）. In this model, the intercellular adhesion molecule-1 （ICAM-1） and interleukin-1 beta （IL-1β） were expressed, and the anti-inflammation effects of herbal extracts were evaluated by detecting the content changes of ICAM-1 and IL-1β in cell lysates and cell culture supernates using an enzyme-linked immunosorbent assay （ELISA）. Moreover, an ultrahigh performance liquid chromatography and tandem mass spectrometry （UPLC-MS/MS） method was used for the detection of XOD activity and the screening of XOD inhibitors in this research. The amount of uric acid from each analyte was directly detected using the multiple reaction monitoring mode and the uric acid level could be reduced via the addition of an inhibitor. Results indicated that Salviae Miltiorrhizae Radix et Rhizome, Rhei Radix et Rhizoma, Polygoni Cuspidati Rhizoma et Radix, Selaginellae Herba, Paeoniae Radix Rubra, especially Ginkgo Folium seemed to be more effective in anti-inflammation and inhibiting XOD activity. The anti-inflammation and enzyme inhibitory activities of the herbal extracts may be correlated with their bioactive components. And the differences between the herbal extracts were correlated with the amount of flavonoid and anthraquinone components. In our study, we have investigated the potential anti-inflammation bioactivity of 33 herbal extracts in vitro, which could provide a reference for further in vivo research in the orevention and treatment of gout.

关键词： Gout Inflammation Human umbilical vein endothelial cells Xanthine oxidase UPLC-MS/MS

A novel sample preparation method of matrix-assisted laser desorption/ionization time of flight mass spectrometry for polystyrene

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Chinese Chemical Letters 2007年第6期18卷 718-721页

作者： Shu Zhang[a] Zhen Wen Zhao[a] Lei Xiong[a] Bin Xin[a] Wei Hua Hu[a] Shao Xiang Xiong[a]&Email:mscbj@*** [a]Beijing mass spectrometry center Institute of Chemistry Chinese Academy of Sciences Beijing 100080 China

A novel sample preparation method of matrix-assisted laser desorption/ionization mass spectrometry for polystyrene was reported. Compared to the conventional dried-droplet method, the efficiency of ionization and sign... 详细信息

关键词： Polystyrene Matrix-assisted laser desorption/ionization time of flight mass spectrometry Three-layer method

α-Glucosidase immobilization on functionalized Fe_3O_4 magnetic nanoparticles for screening of enzyme inhibitors

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Chinese Chemical Letters 2019年第3期30卷 656-659页

作者： Guorong Cheng Junpeng Xing Zifeng Pi Shu Liu Zhiqiang Liu Fengrui Song National center of mass spectrometry in Changchun &Jilin Province Key Laboratory of Chinese Medicine Chemistry and mass spectrometry Changchun Institute of Applied Chemistry Chinese Academy of Sciences University of Science and Technology of China

Magnetic nanoparticles(MNPs) are widely used for the immobilization of enzyme owing to the unique properties such as good biocompatibility and rapid separation. Herein, we used Fe_3O_4 magnetic nanoparticles(Fe_3O_4 MNPs) as the carrier core with(3-aminopropyl)triethoxysilane(APTES)modification by our approach, in which a-glucosidase was stereoscopically immobilized on the surface of Fe_3O_4 MNPs via covalent binding. The result of immobilization was characterized by scanning electron microscope(SEM) and fourier transform-infrared spectroscopy(FT-IR). Then we optimized some key parameters of the immobilization reaction, including the ratio of MNPs to enzyme, GA concentration,crosslinking time and immobilization time. Moreover, under the optimal conditions, pH tolerance,thermo stability and reusability of the immobilized enzyme were investigated and compared with the free one. In order to evaluate the change of the affinity of the enzyme to its specific substrate after immobilization, the Michaelis-Menten constant(K_m) was also studied. Finally, the immobilized α-glucosidase combining with high performance liquid chromatography-tandem mass spectrometry technique(HPLC-MS/MS) was applied to screen and identify eight inhibitors from Polygonum cuspidatum extract. These results indicated that the established method had the broad prospects for biotechnological applications.

关键词： Magnetic nanoparticles(MNPs) α-Glucosidase Immobilization HPLC-MS/MS Inhibitor screening Polygonum cuspidatum

Study of the Transient Reactive Pd(Ⅳ) Intermediate in the Pd(OAc)2-Catalyzed Oxidative Coupling Reaction System by Electrospray Ionization Tandem mass spectrometry

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Chinese Journal of Chemistry 2013年第3期31卷 371-376页

作者： Wei Zhu Haoyang Wang Haihui Peng Guosheng Liu Yinlong Guo Shanghai mass spectrometry center Shanghai Institute of Organic Chemistry Chinese Academy of Sciences Shanghai 200032 China

Pd-catalyzed oxidative coupling reaction was of great importance in the aromatic C--H activation and the for-mation of new C-O and C--C bonds. Sanford has pioneered practical, directed C-H activation reactions em-ploying Pd（OAc）2 as catalyst since 2004. However, until now, the speculated reactive Pd（Ⅳ） transient intermedi-ates in these reactions have not been isolated or directly detected from reaction solution. Electrospray ionization tandem mass spectrometry （ESI-MS/MS） was used to intercept and characterize the reactive Pd（Ⅳ） transient inter-mediates in the solutions of Pd（OAc）2-catalyzed oxidative coupling reactions. In this study, the Pd（IV） transient in-termediates were detected from the solution of Pd（OAc）2-catalyzed oxidative coupling reactions by ESI-MS and the MS/MS of the intercepted Pd（IV） transient intermediate in reaction system was the same with the synthesized au-thentic Pd（Ⅳ） complex. Our ESI-MS（/MS） studies confirmed the presence of Pd（Ⅳ） reaction transient intermedi-ates. Most interestingly, the MS/MS of Pd（Ⅳ） transient intermediates showed the reductive elimination reactivity to Pd（Ⅱ） complexes with new C-O bond formation into product in gas phase, which was consistent with the proposed reactivity of the Pd（Ⅳ） transient intermediates in solution.

关键词： electrospray ionization tandem mass spectrometry (ESI-MS/MS) Pd(IV) transient intermediate oxi^dative coupling reaction

Identifying the dynamic behaviors in complete reconstruction of Co-based complex precatalysts during electrocatalytic oxygen evolution

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Journal of Energy Chemistry 2025年第1期100卷 226-233页

作者： Jingfang Zhang Danyang Wu Linke Cai Youluan Lu Fanpeng Cheng Lijuan Shi Qun Yi Yao Liu Yi Huang Key Laboratory of Green Chemical Engineering Process of Ministry of Education Engineering Research Center of Phosphorus Resources Development and Utilization of Ministry of Education Hubei Key Laboratory of Novel Reactor and Green Chemical Technology School of Chemical Engineering & Pharmacy Wuhan Institute of Technology Key Laboratory of Pesticide & Chemical Biology of Ministry of Education Engineering Research Center of Photoenergy Utilization for Pollution Control and Carbon Reduction of Ministry of Education College of Chemistry Central China Normal University College of Materials Science and Engineering Fuzhou University

Transition metal-based nanomaterials have emerged as promising electrocatalysts for oxygen evolution reaction（OER）. Considerable research efforts have shown that self-reconstruction occurs on these nanomaterials under operating conditions of OER process. However, most of them undergo incomplete reconstruction with limited thickness of reconstruction layer, leading to low component utilization and arduous exploration of real catalytic mechanism. Herein, we identify the dynamic behaviors in complete reconstruction of Co-based complexes during OER. The hollow phytic acid（PA） cross-linked CoFe-based complex nanoboxes with porous nanowalls are designed because of their good electrolyte penetration and mass transport ability, in favor of the fast and complete reconstruction. A series of experiment characterizations demonstrate that the reconstruction process includes the fast substitution of PA by OH-to form Co（Fe）(OH)xand subsequent potential-driven oxidation to Co（Fe）OOH. The obtained CoFeOOH delivers a low overpotential of 290 mV at a current density of 10 mA cm-2and a long-term *** experiment results together with theory calculations reveal that the Fe incorporation can result in the electron rearrangement of reconstructed CoFeOOH and optimization of their electronic structure,accounting for the enhanced OER activity. The work provides new insights into complete reconstruction of metal-based complexes during OER and offers guidelines for rational design of high-performance electrocatalysts.

关键词： Complete reconstruction Co-based complex Precatalysts Oxygen evolution reaction

Effects of the ambient fine particulate matter(PM2.5) exposure on urinary metabolic profiles in rats using UPLC-Q-TOF-MS

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Chinese Chemical Letters 2019年第1期30卷 90-94页

作者： Lin Zhang Tengfei Xu Zifeng Pi Meizhu Zheng Fengrui Song Zhiqiang Liu Changchun Institute of Applied Chemistry Chinese Academy of Science Changchun Center of Mass Spectrometry Key Laboratory of Chinese Medicine Chemistry and Mass Spectrometry School of Pharmaceutical Sciences Jilin University The Central Laboratory Changchun Normal University

In order to study the damage of ambient fine particulate matter(PM2.5) to organism in the environment,the method of urinary metabolomics was used to detect the potential endogenous metabolites and their related metabolic pathways to clarify the toxicity mechanisms. Particles of PM2.5 collected from the fibrous membrane were extracted ultrasonically and dissolved in physiological saline to prepare PM2.5 suspension. The solution of saline and fine particular matter was injected into the trachea of rats respectively. The rats were injected two times a week for four weeks. Samples of 24-h urine were collected at the 14 th day after the end of exposure, and the ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS) was used for the metabolomics detection. Principal component analysis(PCA) was used to investigate the global metabolomic alterations and a clear separation in the scatter diagram were observed. 17 potential endogenous metablites were identified from urinary samples in rats by UPLC-Q-TOF-MS. The primary metabolism pathways involved pentose and glucuronate interconversions, starch and sucrose metabolism, tryptophan metabolism, tyrosine metabolism, phenylalanine metabolism, purine metabolism, acetaminophen metabolism pathway, retinol metabolism and valproic acid metabolism *** results are helpful to understand the toxicological mechanisms of PM2.5 and screened out potential biomarkers of rats which exposure to PM2.5.

关键词： Ambient fine particulate matter UPLC -Q-TOF-MS Metabolomics Urine

Effect of type 2 diabetes mellitus on flavonoid pharmacokinetics and tissue distribution after oral administration of Radix Scutellaria extract in rats

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Chinese Journal of Natural Medicines 2018年第6期16卷 418-427页

作者： ZHANG Xue-Ju LIU Shu XING Jun-Peng LIU Zhi-Qiang SONG Feng-Rui National center of mass spectrometry in Changchun Jilin Province Key Laboratory of Chinese Medicine Chemistry and Mass SpectrometryChangchun Institute of Applied ChemistryChinese Academy of SciencesChangchun 130022China University of Chinese Academy of Sciences Beijing 100039China

Radix Scutellaria is widely applied to the treatment of diabetes mellitus in China. Its main bioactive constituents contain baicalin, wogonoside, oroxyloside, and their aglycones. To investigate the effect of type 2 diabetes mellitus on both pharmacokinetics and tissue distribution of these flavonoid compounds, the six flavonoids in plasma and tissues from the normal and type 2 diabetic rats after oral administration of Radix Scutellaria extract were simultaneously measured by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method. The results showed that baicalin, wogonoside, and oroxyloside had higher Cmax and AUC values(P < 0.05) in type 2 diabetic rats than that in normal rats and the tissue-distribution behaviors of the six flavonoid compounds in hearts, livers, spleens, lungs, kidneys, brains, pancreas, fat and muscle of the type 2 diabetic rats showed obviously differences from the normal rats(P < 0.05). In conclusion, the differences in the pharmacokinetics of oroxyloside and tissue distribution of the six flavanoids in Radix Scutellaria extract between diabetic and normal rats were found for the first time. The results from the present study provided a crucial basis for a better understanding of in vivo anti-diabetic mechanism of action of the six flavonoids from Radix Scutellaria.

关键词： Radix Scutellaria Diabetes mellitus Flavonoid Pharmacokinetics Tissue distribution