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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

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Investigation of molecular aggregation mechanism of glipizide/cyclodextrin complexation by combined experimental and molecular modeling approaches

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Asian Journal of Pharmaceutical Sciences 2019年第6期14卷 609-620页

作者： Tianhe Huang Qianqian Zhao Yan Su Defang Ouyang state key laboratory of quality research in chinese medicine Institute of Chinese Medical Sciences (ICMS) University of Macao

Cyclodextrin complexation is a wise strategy to enhance aqueous solubility of waterinsoluble ***,the aggregation mechanism of drug-cyclodextrin complexes is still *** research aimed to investigate the molecular aggregation mechanism of glipizide/cyclodextrin complexation by the combination of experimental and modeling *** free energies between glipizide and cyclodextrins from modeling calculations were higher than those by the phase solubility diagram *** experimental and modeling results showed that methylated-β-cyclodextrin exhibited the best solubilizing capability to ***-measurement results confirmed the aggregation between glipizide and all four cyclodextrins in high ***/γ-cyclodextrin and glipizide/β-cyclodextrin complexes showed stronger aggregation trend than HP-β-cyclodextrin and methylated-β-*** substituted groups in the rim of HP-β-cyclodextrin and methylated-β-cyclodextrin lead to weak *** research provided us a clear molecular mechanism of glipizide/cyclodextrin complexation and *** research will also benefit the formulation development of cyclodextrin solubilization.

关键词： Glipizide Cyclodextrin Molecular modeling Aggregation Molecular mechanism

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Predicting oral disintegrating tablet formulations by neural network techniques

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Asian Journal of Pharmaceutical Sciences 2018年第4期13卷 336-342页

作者： Run Han Yilong Yang Xiaoshan Li Defang Ouyang state key laboratory of quality research in chinese medicine Institute of Chinese Medical Sciences(ICMS)University of Macao state key laboratory of quality research in chinese medicine Institute of Chinese Medical Sciences (ICMS)University of Macao Department of Computer and Information Science Faculty of Science and TechnologyUniversity of Macao

Oral disintegrating tablets(ODTs) are a novel dosage form that can be dissolved on thetongue within 3 min or less especially for geriatric and pediatric patients. Current ODT for-mulation studies usually rely on the personal experience of pharmaceutical experts andtrial-and-error in the laboratory, which is inefficient and time-consuming. The aim of cur-rent research was to establish the prediction model of ODT formulations with direct com-pression process by artificial neural network(ANN) and deep neural network(DNN) tech-niques. 145 formulation data were extracted from Web of Science. All datasets were dividedinto three parts: training set(105 data), validation set(20) and testing set(20). ANN andDNN were compared for the prediction of the disintegrating time. The accuracy of the ANNmodel have reached 85.60%, 80.00% and 75.00% on the training set, validation set and testingset respectively, whereas that of the DNN model were 85.60%, 85.00% and 80.00%, respec-tively. Compared with the ANN, DNN showed the better prediction for ODT *** is the first time that deep neural network with the improved dataset selection algorithmis applied to formulation prediction on small data. The proposed predictive approach couldevaluate the critical parameters about quality control of formulation, and guide researchand process development. The implementation of this prediction model could effectivelyreduce drug product development timeline and material usage, and proactively facilitatethe development of a robust drug product.

关键词： Oral disintegrating tablets Formulation prediction Artificial neural network Deep neural network Deep-learning

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Non-apoptotic cell death-based cancer therapy:Molecular mechanism,pharmacological modulators,and nanomedicine

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Acta Pharmaceutica Sinica B 2022年第9期12卷 3567-3593页

作者： Xuan Wang Peng Hua Chengwei He Meiwan Chen state key laboratory of quality research in chinese medicine Institute of Chinese Medical SciencesUniversity of MacaoMacaoSAR 999078China

As an emerging cancer therapeutic target,non-apoptotic cell death such as ferroptosis,necroptosis and pyroptosis,etc.,has revealed significant potential in cancer treatment for bypassing apoptosis to enhance the undermined therapeutic efficacy triggered by apoptosis resistance.A variety of anticancer drugs,synthesized compounds and natural products have been proven recently to induce non-apoptotic cell death and exhibit excellent anti-tumor ***,the convergence of nanotechnology with functional materials and biomedicine science has provided tremendous opportunities to construct non-apoptotic cell death-based nanomedicine for innovative cancer *** are not only employed in targeted delivery of non-apoptotic inducers,but also used as therapeutic components to induce non-apoptotic cell death to achieve efficient tumor *** review first introduces the main characteristics,the mechanism and various pharmacological modulators of different non-apoptotic cell death forms,including ferroptosis,necroptosis,pyroptosis,autophagy,paraptosis,lysosomal-dependent cell death,and ***,we comprehensively review the latest progresses of nanomedicine that induces various forms of non-apoptotic cell death and focus on the nanomedicine targeting different pathways and ***,the combination therapies of non-apoptotic cell death with photothermal therapy,photodynamic therapy,immunotherapy and other modalities are ***,the challenges and future perspectives in this regard are also discussed.

关键词： Non-apoptotic cell death Ferroptosis Necroptosis Pyroptosis Autophagy Nanomedicine Combination therapies Anticancer

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Click chemistry-based enrichment strategy for tracing cellular fatty acid metabolism by LC-MS/MS

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Journal of Pharmaceutical Analysis 2023年第10期13卷 1221-1231页

作者： Ru-Jie Yang Jian Zou Jia-Yue Liu Jiang-Kun Dai Jian-Bo Wan state key laboratory of quality research in chinese medicine Institute of Chinese Medical SciencesUniversity of MacaoMacao SAR999078China

Fatty acids(FAs),which were initially recognized as energy sources and essential building blocks of biomembranes,serve as the precursors of important signaling *** FA metabolism is essential to understanding the biochemical activity and role of FAs in physiological and pathological *** by the advances in click chemistry for protein enrichment,we herein established a click chemistry-based enrichment(CCBE)strategy for tracing the cellular metabolism of eicosapentaenoic acid(EPA,20:5 n-3)in neural *** alkyne-labeled EPA(EPAA)used as a surrogate was incubated with N2a,mouse neuroblastoma cells,and alkyne-labeled metabolites(ALMs)were selectively captured by an azide-modified resin via a Cu(I)-catalyzed azide-alkyne cycloaddition reaction for *** removing unlabeled metabolites,ALMs containing a triazole moiety were cleaved from solid-phase resins and subjected to liquid chromatography mass spectrometry(LC-MS)*** proposed CCBE strategy is highly selective for capturing and enriching alkyne-labeled metabolites from the complicated *** addition,this method can overcome current detection limits by enhancing MS sensitivity of targets,improving the chromatographic separation of sn-position glycerophospholipid regioisomers,facilitating structural characterization of ALMs by a specific MS/MS fragmentation signature,and providing versatile fluorescence detection of ALMs for cellular *** CCBE strategy might be expanded to trace the metabolism of other FAs,small molecules,or drugs.

关键词： Click chemistry-based enrichment EPA metabolism Terminal alkyne-labeled EPA Azide-modified resin LC-MS/MS

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Advanced Studies on Rhizoma Dioscoreae Collettii

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chinese Journal of Integrative medicine 2020年第3期26卷 235-240页

作者： LI Lai-lai MENG Xiao-wei FAN Ke-tao WANG Yan-yan XIAO Yang WANG Yi Institute of Traditional chinese medicine research Tianjin State Key Laboratory of Modern Chinese Medicine Tianjin University of Traditional Chinese Medicine

Rhizoma Dioscoreae Collettii,is known as Huang Dioscorea collettii,Rhizoma Coptidis Brevisepalae or yellow *** is neutral in nature and bitter in taste which is described to Gan(Liver)meridian,Wei(Stomach)meridian and Pangguang(Bladder)*** was often used in the treatment of chyloid stranguria,gonorrhea,leucorrhagia,rheumatism arthralgia pain,joints disable,and lumbar knee pain syndrome in clinical.

关键词： Rhizoma Dioscoreae Collettii identification chemical constituents pharmacology clinical application

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Dietary therapy may be sufficient for type 1 diabetes treatment

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Cellular & Molecular Immunology 2018年第2期15卷 85-87页

作者： Shuoyang Liu Xin Chen state key laboratory of quality research in chinese medicine Institute of Chinese Medical SciencesUniversity of MacaoMacao999078China

There is compelling evidence that the gastrointestinal commensal microbiota is instrumental in shaping the functions of the immune system.1 The short-chain fatty acids(SCFAs),mainly acetate,propionate and butyrate,which are the end products of dietary fibers after bacterial metabolism,act as an interface between the microbiota and immune cells.2 In a recent article in Nature Immunology,Mariño et al.3 reported that the levels of acetate and butyrate in the blood and feces of non-obese diabetic(NOD)mice,a mouse model of human type 1 diabetes(T1D),are inversely correlated with the *** NOD mice were completely protected from the development of diabetes by the administration of a combination of the acetate-and butyrate-yielding *** SCFAs inhibited pathogenic effector T cells and induced CD4+Foxp3+regulatory T cells(Tregs),thereby contributing to the unprecedented therapeutic effect.3 The findings of this study may open a new avenue to prevent and treat patients with T1D with medicinal food or nutraceuticals rather than conventional pharmaceutics.

关键词： metabolism inhibited treatment

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Optimization of microwave-assisted extraction of bioactive alkaloids from lotus plumule using response surface methodology

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Journal of Pharmaceutical Analysis 2016年第6期6卷 382-388页

作者： Wei Xiong Xianqiang Chen Guangping Lv Dejun Hu Jing Zhao Shaoping Li state key laboratory of quality research in chinese medicine Institute of Chinese Medical SciencesUniversity of MacaoMacao SAR

In this work,a fast and efficient microwave-assisted extraction(MAE) method was developed to extract main bioactive alkaloids from lotus *** optimize MAE conditions,three main factors were selected using univariate approach experiments,and then central composite design(CCD).The optimal extraction conditions were as follows:methanol concentration of 65%,microwave power of 200 W,and extraction time of 260 s.A high performance liquid chromatography–diode array detector(HPLC–DAD) method was established to quantitatively analyze these phytochemicals in different lotus plumule samples and in different part of *** separation was carried out on an Agilent Zorbax Extend-C_(18) column(4.6 mm×150 mm,3.5 μm).Gradient elution was applied with the mobile phase constituted with 0.1% triethylamine in water(A)and acetonitrile(B):40%-70% B at 0-8 min,70%-100% B at 8–9 min,100% B for 2 min,and then equilibrated with 40% B for 2 min.

关键词： Lotus plumule Functional food Microwave-assisted extraction Alkaloids

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A four-component combination derived from Huang-Qin Decoction significantly enhances anticancer activity of irinotecan

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chinese Journal of Natural medicines 2021年第5期19卷 364-375页

作者： XU Dou-Dou HOU Xiao-Ying WANG Ou WANG Di LI Dan-Ting QIN Si-Yuan LV Bo DAI Xiao-Min ZHANG Zun-Jian WAN Jian-Bo XU Feng-Guo key laboratory of Drug quality Control and Pharmacovigilance(Ministry of Education) State Key Laboratory of Natural MedicineChina Pharmaceutical UniversityNanjing 210009China state key laboratory of quality research in chinese medicine Institute of Chinese Medical SciencesUniversity of MacaoMacaoChina

Huang-Qin Decoction(HQD)is a classic prescription for diarrhea in chinese medicine *** studies have demonstrated that HQD and its modified formulation PHY906 could ameliorate irinotecan(CPT-11)induced gastrointestinal(GI)toxicity and enhance its anticancer therapeutic ***,which constituents in HQD are effective is still unclear so *** study aims to screen out the key bioactive components combination from HQD that could enhance the anticancer effect of ***,the potential bioactive constituents were obtained through system pharmacology *** the bioactivity of each constituent was investigated synthetically from the aspects of NCM460 cell migration,TNF-αrelease of THP-1-derived macrophage and MTT assay in HCT116 *** contribution of each constituent in HQD was evaluated using the bioactive index Ei,which taken the content and bioactivity into comprehensive *** then,the most contributing constituents were selected out to form a keycomponent *** last,the bioefficacy of the key-component combination was validated in vitro and in *** a result,a key-component combination(HB4)consisting of four compounds baicalin,baicalein,glycyrrhizic acid and wogonin was screened *** vitro assessment indicated that HB4 could enhance the effect of CPT-11 on inhibiting cell proliferation and inducing apoptosis in ***,the in vivo study confirmed that HB4 and HQD have similar pharmacological activity and could both enhance the antitumor effect of CPT-11 in HCT116 xenograft ***,HB4 could also reduce the CPT-11 induced GI toxicity.

关键词： Active components Bioactivity contribution Huang-Qin Decoction Irinotecan Toxicity attenuating and efficacy enhancing

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Comprehensive chemical study on different organs of cultivated and wild Sarcandra glabra using ultra-high performance liquid chromatography time-of-flight mass spectrometry(UHPLC-TOF-MS)

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chinese Journal of Natural medicines 2021年第5期19卷 391-400页

作者： WANG Cai-Yun LU Jing-Guang CHEN Da-Xin WANG Jing-Rong CHE Kai-Si ZHONG Ming ZHANG Wei JIANG Zhi-Hong state key laboratory of quality research in chinese medicines Macao Institute for Applied Research in Medicine and HealthMacao University of Science and TechnologyTaipaMacaoChina Fujian key laboratory of Integrative medicine on Geriatric Academy of Integrative MedicineFujian University of Traditional Chinese MedicineFuzhou 350122China Guangxi key laboratory of Traditional chinese medicine quality Standards Guangxi Institute of Chinese Medicine and Pharmaceutical ScienceNanning 530022China

To illuminate the similarities and differences between wild and cultivated Sarcandra glabra(***),we performed a comprehensively study on 26 batches of cultivated *** and 2 batches of wild *** constituents and distribution characteristics of roots,stems and leaves in both wild and cultivated *** were investigated through UHPLC-TOF-MS *** result revealed that there were significant differences between roots,stems and leaves in *** the chemical contents in the root part were less or even absence than those in leaf and stem,which suggested the root organ could be excluded as ***,the chemical contents of stems and leaves in cultivated *** was sightly higher than that of wild ***,cultivated *** may have a high potential for substitution of wild *** without affecting its pharmaceutical *** summary,our study could provide important information to the molecular basis for quality control of ***.

关键词： S.glabra UHPLC-TOF-MS Root Stem Leaf

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