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Authentic compound-free strategy for simultaneous determination of primary coumarins in Peucedani Radix using offline high performance liquid chromatography–nuclear magnetic resonance spectroscopy–tandem mass spectrometry

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Acta Pharmaceutica Sinica B 2018年第4期8卷 645-654页

作者： Yao Liu Qingqing Song Wenjing Liu Peng Li Jun Li Yunfang Zhao Liang Zhang Pengfei Tu Yitao Wang Yuelin Song Modern research Center for Traditional chinese Medicine School of Chinese Materia MedicaBeijing University of Chinese Medicine state key laboratory of quality research in chinese Medicine Institute of Chinese Medical SciencesUniversity of Macao state key laboratory of Tea Plant Biology and Utilization Anhui Agricultural University

Herein, a strategy is proposed for the simultaneous determination of primary coumarins in Peucedani Radix(chinese name: Qianhu). The methodology consists of three consecutive steps: 1) Semi-preparative LC in combination with a home-made automated fraction collection module to fragment the universal metabolome standard into ten fractions(Frs. I–X); 2) LC–accurate MS/MS and quantitative1 H NMR spectroscopy conducted in parallel to acquire the qualitative and quantitative data of each fraction; 3) Robust identification and quantification of components by use of LC coupled to multiple reaction monitoring. In this final step, the most significant fractions(Frs. III–X) were pooled to serve as the pseudo-mixed standard solution. Meticulous online parameter optimization was performed to obtain the optimal parameters, including ion transitions and collision energies. Concerns were particularly paid onto pursuing the parameters being capable of monitoring regiospecific isomers, notably praeruptorin E vs. 3′-isovaleryl-4′-angeloylkhellactone. The quantitative performance of the method was validated according to diverse assays. Eleven primary coumarins(1–11) were unambiguously identified and absolutely quantified, even though no external reference compound was used. Above all, the integrated strategy not only provides a feasible pipeline for the quality assessment of Peucedani Radix, but more importantly, shows the potential for authentic compound-free quantitative evaluation of traditional chinese medicines.

关键词： Authentic compoundindependent quantitation Offline LC–NMR–MS/MS Automated fraction collection module Quantitative1H NMR Peucedani Radix Regio-specific monitoring

Macrocyclic Nonapeptides Incorporating Uncharacterized Amino Acids with Inhibitory Effects on Th17 Differentiation

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CCS Chemistry 2021年第2期3卷 844-858页

作者： Kai-Long Ji Yao-Yue Fan Hio-Ha Kuok Qun-Fang Liu Ting Li Jian-Min Yue state key laboratory of Drug research Shanghai Institute of Materia MedicaChinese Academy of SciencesShanghai 201203 state key laboratory of quality research in chinese medicines Macao Institute for Applied Research in Medicine and HealthMacao University of Science and TechnologyMacao 999078

Four unprecedented macrocyclic nonapeptides,orberryamides A–D(1–4),were isolated from Glycosmis pentaphylla(orangeberry)and structurally characterized by obtaining solid data from numerous analytical *** 1 incorporated a new amino acid residue,named orangeberrine(Orgb),compounds 2 and 3 integrated the rare,nonproteinogenic amino acid residues(Kyn and Dioia,respectively),and compound 4 existed as two major conformational isomers in solution at ambient *** biosynthetic pathways proposed for compounds 1–4 are of considerable biological significance for the modification and metabolism of tryptophan(Trp)and/or Trp containing proteins in ***,compounds 1–4 suppressed Th17 differentiation significantly,and the effects of 1–3 was achieved through targeting the ligand-binding domain(LBD)of the retinoic acid-related orphan receptor gamma t(RORγt).

关键词： natural products Glycosmis pentaphylla,cyclopeptides Th17 differentiation inhibitors RORγt LBD blockers

Identification of anti-cancer compounds from natural products

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chinese Journal of Natural medicines 2020年第7期18卷 481-482页

作者： LU Jin-Jian WANG Yi-Tao state key laboratory of quality research in chinese Medicine Institute of Chinese Medical SciencesUniversity of MacaoMacao 999078China

Natural products serve as abundant resources with diversity of chemical structures,which has been widely explored for the pharmacological researches and drug discovery[1,2].They are generally isolated from microorgani... 详细信息

关键词： cancer abundant compounds

A novel 12,23-epoxy dammarane saponin from Panax notoginseng

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chinese Journal of Natural medicines 2015年第4期13卷 303-306页

作者： YUAN Cen XU Fa-Xiang HUANG Xiao-Jun LI Shao-Ping ZHANG Qing-Wen state key laboratory of quality research in chinese Medicine Institute of Chinese Medical SciencesUniversity of Macao Institute of Traditional chinese Medicine and Natural Products Jinan University

The present study investigated the chemical constituents of the roots and rhizomes of Panax *** were isolated by various column chromatographic methods,and their structures were elucidated by the extensive analysis of spectroscopic data and chemical evidences.A novel 12,23-epoxy dammarane-type saponin,named epoxynotoginsenoside A(1),together with four known compounds(2-5),was isolated and characterized.

关键词： Panax notoginseng Dammarane saponin Epoxynotoginsenoside A

quality analysis of commercial samples of Ziziphi spinosae semen(suanzaoren) by means of chromatographic fingerprinting assisted by principal component analysis

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Journal of Pharmaceutical Analysis 2014年第3期4卷 217-222页

作者： Shuai Sun Hailing Liu Shunjun Xu Yuzhen Yan Peishan Xie Faculty of chinese Medicine Macao University of Science and Technology state key laboratory for quality research in chinese Medicine Macao Institute for Applied Research in Medicine and HealthMacao University of Science and Technology state key laboratory of Natural medicines China Pharmaceutical University

Due to the scarcity of resources of Ziziphi spinosae semen （ZSS）, many inferior goods and even adulterants are generally found in medicine markets. To strengthen the quality control, HPLC fingerprint common pattern established in this paper showed three main bioactive compounds in one chromatogram simultaneously. Principal component analysis based on DAD signals could discriminate adulterants and inferiorities. Principal component analysis indicated that all samples could be mainly regrouped into two main clusters according to the first principal component （PC1, redefined as Vicenin II） and the second principal component （PC2, redefined as zizyphusine）. PC1 and PC2 could explain 91.42%of the variance. Content of zizyphusine fluctuated more greatly than that of spinosin, and this result was also confirmed by the HPTLC result. Samples with low content of jujubosides and two common adulterants could not be used equivalently with authenticated ones in clinic, while one reference standard extract could substitute the crude drug in pharmaceutical production. Giving special consideration to the well-known bioactive saponins but with low response by end absorption, a fast and cheap HPTLC method for quality control of ZSS was developed and the result obtained was commensurate well with that of HPLC analysis. Samples having similar fingerprints to HPTLC common pattern targeting at saponins could be regarded as authenticated ones. This work provided a faster and cheaper way for quality control of ZSS and laid foundation for establishing a more effective quality control method for ZSS.

关键词： Adulterant Common pattern Principal component analysis quality control Ziziphi spinosae semen

Quantitation of camellianin A in HepG2 cells using a high performance liquid chromatography-electrospray ionization tandem mass spectrometric method

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chinese Journal of Natural medicines 2017年第3期15卷 234-240页

作者： CHEN Qian-Qian XI Hai-Ling WANG Cai-Yun XU Feng-Guo ZHANG Wei state key laboratory of quality research in chinese Medicine Macao University of Science and Technology School of Public Health Baotou Medical College key laboratory of Drug quality Control and Pharmacovigilance(Ministry of Education) China Pharmaceutical University

The present study was designed to develop a sensitive and selective high performance liquid chromatography-tandem mass spectrometric method for the determination of Camellianin A in HepG2 *** extraction of Camellianin A was achieved using 15% trichloroacetic acid and then separated on a C_(18) column interfaced with a triple quadrupole tandem mass spectrometer in multiple reaction monitoring *** mobile phase was consisted of methanol-water(0.1% formic acid)(55:45,V/V).The total run time was 5.0 *** method was linear in the concentration range of 0.25-250.0 ng·mL^(-1).The lower limit of quantification was 0.25 ng·mL^(-1).The intra-and inter-day relative standard deviations of entire concentration range were less than 9.3%.The proposed HPLC-MS/MS method was successfully applied to detect the intracellular concentration of Camellianin A in HepG2 cells.

关键词： Camellianin A HepG2 cells HPLC-MS/MS

Chemical Diversity Investigation of Hepatotoxic Pyrrolizidine Alkaloids in Qianliguang(Senecio scandens)and Related Species by UHPLC-QTOF-MS

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World Journal of Traditional chinese Medicine 2015年第2期1卷 1-11页

作者： Lin Zhu Na Li Jian-Qing Ruan Peter P.Fu Zhong-Zhen Zhao Ge Lin School of Biomedical Sciences Faculty of Medicine The Chinese University of Hong Kong state key lab for quality research in chinese medicines Macao Institute for Applied Research in Medicine and Health Macao University of Science and Technology National Center for Toxicological research School of chinese Medicine Hong Kong Baptist University

Objective: Qianliguang(Senecio scandens) is a common chinese medicinal herb. Qianliguang-containing herbal proprietary products are registered as over-the-counter remedies in China and exported to Western countries. The presence of hepatotoxic pyrrolizidine alkaloids(PAs)has raised concerns about the safety of using Qianliguang and its products. The present study aims at investigation of different types of PAs present in Qianliguang collected from representative locations in ***: In this study, a simple but specific UHPLC-QTOF-MS method for the determination of toxic PAs was developed, based on the characteristic fragment ions specific to different types of PAs. It was successfully applied for the identification and distinguishing of PAs present in Qianliguang and related Senecio species growing in different locations of ***: Significant diversity of the PA types and quantities were revealed among the samples tested. The estimated total amounts of toxic PAs in three of the samples exceed the toxic limits of PA intake restricted by WHO, demonstrating the timely and highly demand for regulating both types and quantities of PAs present in ***: This study provides the methodology for simultaneous identification and quantification of PAs present in herbs without requiring corresponding standards, which could be further used for more systematic investigations of the PA distribution in Qianliguang and other PA-containing herbs.

关键词： Qianliguang(Senecio scandens) Pyrrolizidine alkaloids UHPLC-QTOF-MS Qualitation Quantification

Lobelia chinensis: chemical constituents and anticancer activity perspective

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chinese Journal of Natural medicines 2014年第2期12卷 103-107页

作者： CHEN Mei-Wan CHEN Wen-Rong ZHANG Jin-Ming LONG Xiao-Ying WANG Yi-Tao state key laboratory of quality research in chinese Medicine Institute of Chinese Medical Sciences University of Macao School of Traditional chinese Medicine Guangdong Pharmaceutical University

research has demonstrated that many chemical constituents dominated by piperidine alkaloids and flavonoids, such as lobelanidine, lobeline, and lobelanine, have been obtained from Lobelia chinensis Lour. Experimental studies and clinical applications have also indicated that L. chinensis possesses a number of pharmacological activities(e.g., diuretic, choleretic, breathing excitement, anti-venom, anti-bacterial, and anticancer). This paper focuses on the properties, chemical constituents, and anticancer activity of L. chinensis to clarify the connection among them, and identify the active anticancer compounds. This work serves as the foundation for further research and development of L. chinensis.

关键词： Lobelia chinensis Chemical constituents Anticancer activity

Optimization of post-classification processing of high-resolution satellite image:A case study

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Science China(Technological Sciences) 2006年第Z1期49卷 98-107页

作者： DONG Rencai DONG Jiajia WU Gang DENG Hongbing state key lab of Systems Ecology Research Center for Eco-Environmental Sciences Chinese Academy of Sciences Beijing 100085 China State Key Lab of Systems Ecology Research Center for Eco-Environmental Sciences Chinese Academy of Sciences Beijing 100085 China State Key Lab of Systems Ecology Research Center for Eco-Environmental Sciences Chinese Academy of Sciences Beijing 100085 China State Key Lab of Systems Ecology Research Center for Eco-Environmental Sciences Chinese Academy of Sciences Beijing 100085 China

The application of remote sensing monitoring techniques plays a crucial role in evaluating and governing the vast amount of ecological construction projects in China. However, extracting information of ecological engineering target through high-resolution satellite image is arduous due to the unique topography and complicated spatial pattern on the Loess Plateau of China. As a result, enhancing classification accuracy is a huge challenge to high-resolution image processing techniques. Image processing techniques have a definitive effect on image properties and the selection of different parameters may change the final classification accuracy during post-classification processing. The common method of eliminating noise and smoothing image is majority filtering. However, the filter function may modify the original classified image and the final accuracy. The aim of this study is to develop an efficient and accurate post-processing technique for acquiring information of soil and water conservation engineering, on the Loess Plateau of China, using SPOT image with 2.5 rn resolution. We argue that it is vital to optimize satellite image filtering parameters for special areas and purposes, which focus on monitoring ecological construction projects. We want to know how image filtering influences final classified results and which filtering kernel is optimum. The study design used a series of window sizes to filter the original classified image, and then assess the accuracy of each output map and image quality. We measured the relationship between filtering window size and classification accuracy, and optimized the post-processing techniques of SPOT5satellite images. We conclude that (1) smoothing with the majority filter is sensitive to the information accuracy of soil and water conservation engineering, and (2) for SPOT5 2.5 m image, the 5×5 pixel majority filter is most suitable kernel for extracting information of ecological construction sites in the Loess Plateau of Chi

关键词： ecological construction, soil and water conservation measure, high spatial resolution satellite image,image post-processing, majority filter.