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PHYTOCHEMICAL ANALYSIS · 2022 ·Vol. 34 ·期 1 ·67-75 · IF 3.024

Ligand fishing of monoamine oxidase B inhibitors from Platycodon grandiflorus (Jacq.) A.DC. roots by the enzyme functionalised magnetic nanoparticles

Hao Yuan,Xiao-Lin Bai,Yi-Kao Hu,Wen-Qin Fan,Emmanuel Ayodeji Ayeni,Xun Liao

Introduction As a famous traditional Chinese medicine, roots of Platycodon grandiflorus (Jacq.) A.DC. have shown multiple effects against neurodegenerative diseases. To investigate the components against Parkinson's disease (PD), the roots of P. grandiflora were selected as the research subject. Objective Screening and identifying of monoamine oxidase B (MAO-B) inhibitors from the roots of P. grandiflorum via enzyme functionalised magnetic nanoparticles (MNPs)-based ligand fishing combined with high-performance liquid chromatography–mass spectrometry (HPLC–MS) analysis. Method MAO-B functionalised MNPs have been synthesised for screening MAO-B inhibitors from the roots of P. grandiflorum . The ligands were identified by HPLC–MS and nuclear magnetic resonance (NMR) analysis, and their anti-PD activity was evaluated via MAO-B inhibition assay and cell viability assay in vitro . Results Two MAO-B inhibitors were fished out and identified by HPLC–MS as protocatechuic aldehyde ( 1 ) and coumarin ( 2 ), with the half maximal inhibitory concentrations of 28.54 ± 0.39 and 25.39 ± 0.29 μM, respectively. Among them, 1 could also significantly increase the viability of 6-hydroxydopamine-damaged PC12 cells. Conclusion The results are helpful to elucidate the anti-PD activity of the plant, and the ligand fishing method has shown good potential in discovery of MAO-B inhibitors.

CAS / MDL: 25952-53-8 6066-82-6
研究领域: 药理学 · 神经科学 · 中药化学
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PHYTOCHEMICAL ANALYSIS · 2023 ·Vol. 34 ·期 5 ·560-570 · IF 3.3

Determination of 44 major components and chemical profiling of saccharide in Chinese medicinal formula Lanqin Oral Liquid

Heng-Li Zhao,Run-Zhou Liu,Meng Ding,Ya-Liu Fan,Bin-Bin Lin,Hong-Wei Lu,Xiao-Dong Wen,Ping Li,Hua Yang

Introduction Lanqin Oral Liquid (LQL) is a traditional Chinese medicine preparation (TCMP) containing five herbal medicines and has been commonly used for the treatment of pharyngitis and hand-foot-and-mouth disease in clinic. The material basis of LQL has been reported in our previous study, but the contents of the major components and the features of saccharide in LQL are still unclear. Objectives This study aimed to establish accurate and rapid methods for the quantification of the major components and profiling of saccharide in LQL. The quantitative results combined with similarity evaluation were applied to improve the quality control of LQL. Methodology An ultra-high performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (UPLC-QQQ-MS) method was utilised to determine 44 major components. Cosine similarity was used to evaluate the similarities among 20 batches of LQL based on the quantitative results of 44 major components. The physicochemical properties, structure, composition, and contents of saccharide in LQL were detected by a combination of chemical and instrumental analysis. Results A total of 44 compounds, including flavonoids, iridoid glycosides, alkaloids, and nucleosides, were accurately determined. The 20 batches of LQL were remarkably similar (> 0.95). In addition, d -glucose, galactose, d -glucuronic acid, arabinose, and d -mannose were detected in saccharide of LQL. The contents of saccharide in LQL were 13.52–21.09 mg/ml. Conclusions The established methods can be applied for the comprehensive quality control of LQL, including characterisation of saccharide and quantification of representative components. Our study will provide a robust chemical foundation for disclosing the quality markers of its therapeutic effect.

CAS / MDL: 108-95-2
研究领域: 药理学 · 分析化学 · 中医药
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYTOCHEMICAL ANALYSIS · 2017 ·Vol. 28 ·期 5 ·424-432 · IF 2.292

Statistical Model Based HPLC Analytical Method Adjustment Strategy to Adapt to Different Sets of Analytes in Complicated Samples

Binjun Yan,Xue Bai,Yunjie Sheng,Fanzhu Li

Introduction On account of the complicated compositions of the products like traditional Chinese medicines (TCMs) and functional foods, it is a common practice to determine different sets of analytes in the same product for different purposes. Objective To efficiently develop the corresponding HPLC methods, a statistical model based analytical method adjustment (SMB-AMA) strategy was proposed. Methods In this strategy, the HPLC data acquired with design of experiments methodology were efficiently utilised to build the retention models for all the analytes and interferences shown in the chromatograms with multivariate statistical modelling methods. According to the set of analytes under research, Monte-Carlo simulations were conducted based on these retention models to estimate the probability of achieving adequate separations between all the analytes and their interferences. Then the analytical parameters were mathematically optimised to the point giving a high value of this probability to compose a robust HPLC method. Radix Angelica Sinensis (RAS) and its TCM formula with Folium Epimedii (FE) were taken as the complicated samples for case studies. Results The retention models for the compounds in RAS and FE were built independently with correlation coefficients all above 0.9799. The analytical parameters were tactfully adjusted to adapt to six cases of different sets of analytes and different sample matrices. In the validation experiments using the adjusted analytical parameters, satisfactory separations were acquired. Conclusion The results demonstrated that the SMB-AMA strategy was able to develop HPLC methods rationally and rapidly in the adaption of different sets of analytes. Copyright © 2017 John Wiley & Sons, Ltd.

CAS / MDL: 64-18-6
研究领域: 分析化学 · 中药学
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PHYTOCHEMICAL ANALYSIS · 2017 ·Vol. 28 ·期 6 ·505-511 · IF 2.292

One-Step Extraction and Hydrolysis of Flavonoid Glycosides in Rape Bee Pollen Based on Soxhlet-Assisted Matrix Solid Phase Dispersion

Xijuan Tu,Shuangqin Ma,Zhaosheng Gao,Jing Wang,Shaokang Huang,Wenbin Chen

Introduction Flavonoids are frequently found as glycosylated derivatives in plant materials. To determine contents of flavonoid aglycones in these matrices, procedures for the extraction and hydrolysis of flavonoid glycosides are required. The current sample preparation method is both labour and time consuming. Objective Develop a modified matrix solid phase dispersion (MSPD) procedure as an alternative methodology for the one-step extraction and hydrolysis of flavonoid glycosides. Method HPLC-DAD was applied for demonstrating the one-step extraction and hydrolysis of flavonoids in rape bee pollen. The obtained contents of flavonoid aglycones (quercetin, kaempferol, isorhamnetin) were used for the optimisation and validation of the method. Results The extraction and hydrolysis were accomplished in one step. The procedure completes in 2 h with silica gel as dispersant, a 1:2 ratio of sample to dispersant, and 60% aqueous ethanol with 0.3 M hydrochloric acid as the extraction solution. The relative standard deviations (RSDs) of repeatability were less than 5%, and the recoveries at two fortified levels were between 88.3 and 104.8%. Conclusion The proposed methodology is simple and highly efficient, with good repeatability and recovery. Compared with currently available methods, the present work has advantages of using less time and labour, higher extraction efficiency, and less consumption of the acid catalyst. This method may have applications for the one-step extraction and hydrolysis of bioactive compounds from plant materials. Copyright © 2017 John Wiley & Sons, Ltd.

研究领域: 植物化学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYTOCHEMICAL ANALYSIS · 2024 · IF 3

A strategy to distinguish similar traditional Chinese medicines by liquid chromatography–mass spectrometry, electronic senses, and gas chromatography–ion mobility spectrometry: Marsdeniae tenacissimae Caulis and Paederiae scandens Caulis as examples

Jia-Wei Wang,Zhi-Dong Pei,Yue-Hua Chen,Si-Yu Li,Tian-Min Wang,Ting-Guo Kang,Na Li,Ya-Mei Song,Hui-Peng Song,Hui Zhang

Introduction Marsdeniae tenacissimae Caulis (MTC), a popular traditional Chinese medicine, has been widely used in the treatment of tumor diseases. Paederiae scandens Caulis (PSC), which is similar in appearance to MTC, is a common counterfeit product. It is difficult for traditional methods to effectively distinguish between MTC and PSC. Therefore, there is an urgent need for a rapid and accurate method to identify MTC and PSC. Objectives The aim is to distinguish between MTC and PSC by analyzing the differences in nonvolatile organic compounds (NVOCs), taste, odor, and volatile organic compounds (VOCs). Methods Liquid chromatography–mass spectrometry (LC-MS) was utilized to analyze the NVOCs of MTC and PSC. Electronic tongue (E-tongue) and electronic nose (E-nose) were used to analyze their taste and odor respectively. Gas chromatography–ion mobility spectrometry (GC-IMS) was applied to analyze VOCs. Finally, multivariate statistical analyses were conducted to further investigate the differences between MTC and PSC, including principal component analysis, orthogonal partial least squares discriminant analysis, discriminant factor analysis, and soft independent modeling of class analysis. Results The results of this study indicate that the integrated strategy of LC-MS, E-tongue, E-nose, GC-IMS, and multivariate statistical analysis can be effectively applied to distinguish between MTC and PSC. Using LC-MS, 25 NVOCs were identified in MTC, while 18 NVOCs were identified in PSC. The major compounds in MTC are steroids, while the major compounds in PSC are iridoid glycosides. Similarly, the distinct taste difference between MTC and PSC was precisely revealed by the E-tongue. Specifically, the pronounced bitterness in PSC was proven to stem from iridoid glycosides, whereas the bitterness evident in MTC was intimately tied to steroids. The E-nose detected eight odor components in MTC and six in PSC, respectively. The subsequent statistical analysis uncovered notable differences in their odor profiles. GC-IMS provided a visual representation of the differences in VOCs between MTC and PSC. The results indicated a relatively high relative content of 82 VOCs in MTC, contrasted with 32 VOCs exhibiting a similarly high relative content in PSC. Conclusion In this study, for the first time, the combined use of LC-MS, E-tongue, E-nose, GC-IMS, and multivariate statistical analysis has proven to be an effective method for distinguishing between MTC and PSC from multiple perspectives. This approach provides a valuable reference for the identification of other visually similar traditional Chinese medicines.

研究领域: 中药学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYTOCHEMICAL ANALYSIS · 2024 · IF 3

A step-by-step progressive strategy exploring whole metabolic profiles in vivo for Polygalae Radix with/without licorice

Tiantian Zhao,Ningning Zhao,Junpeng Xing,Zhong Zheng,Zhiqiang Liu,Shu Liu

Introduction Polygalae Radix (PR) is known to relieve toxicity and increase efficiency in various diseases after processing. However, there were few studies for aromatic carboxylic acids (ACAs) due to the limited detection, especially for the metabolites within m/z 100–2000. Objectives This study aims to elucidate the whole metabolism of PR with/without licorice (LP), focusing on metabolites within m/z 100–2000 and pharmacodynamics in vivo. Material and methods This study was established by the combination of multidimensional ultra-high performance liquid chromatography coupled with a mass spectrometer (UPLC–MS) technology with protein sedimentation method to analyze metabolites in plasma, brain, colon, and stomach contents. Quantitative monitoring ACAs was enhanced with our novel stable isotope derivatization (SILD) technique. And then the pharmacokinetics (PK) study of relatively large metabolites was carried out. A targeted network pharmacology approach was established to avoid false positive results, mapping interactions relevant to Alzheimer's disease (AD), and other conditions. Results The 85 polygala metabolites were qualitatively analyzed in plasma, brain, colon, and stomach contents. The 11 types of relatively large metabolites and 8 types of ACAs were quantitatively monitored. Among them, nine types of relatively large metabolites were assessed through PK studies. In targeted network pharmacology, it highlighted the significance of small molecular metabolites, including ACAs et al, which were frequently overlooked. LP may play a more key role mainly through neural active ligand-receptor interaction, AD, and pertussis pathways. These findings have outlined a step-by-step strategy for in-depth research in vivo, laying a foundation for further verification of biological function.

研究领域: 中药学 · 代谢组学 · 药理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYTOCHEMICAL ANALYSIS · 2021 ·Vol. 33 ·期 3 ·441-451 · IF 3.373

Development of an immunochromatographic test strip for the rapid detection of aristolochic acid A in herbal medicinal materials

Xianrui Chen,Ting Huang,Zhibing Huang,Quanbin Han

Introduction Plants containing aristolochic acid and its derivatives are nephrotoxic, mutagenic, and carcinogenic to humans; chronic diet poisoning caused by the aristolochic acid is the cause of endemic (Balkan) nephropathy and related cancers. Objective To develop a colloidal gold immunochromatographic test strip (ICS) based on the competitive format for the rapid detection of aristolochic acid A (AA-A) in herbal medicinal materials. Materials and methods For the ICS based on gold nanoparticles (AuNPs), the antigen [AA-A–bovine serum albumin (BSA)], and goat anti-mouse IgG were drawn on the nitrocellulose membrane as the test line (T line) and the control line (C line), respectively. Monoclonal antibody (MAb)–AuNP conjugates were sprayed onto the conjugate pad. The sensitivity of the ICS was 6 ng/mL, and the test was completed in 10 min. The analysis of AA-A in traditional Chinese medicine samples showed that the ICS results were in good agreement with those obtained by high-performance liquid chromatography methods. Conclusion These results demonstrated that the ICS test could be used as a reliable, rapid, cost-effective, and convenient qualitative tool for on-site screening techniques to detect AA-A in herbal medicinal materials without any special instrumentation.

研究领域: 药理学 · 分析化学 · 毒理学 · 医学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYTOCHEMICAL ANALYSIS · 2020 ·Vol. 31 ·期 3 ·366-374 · IF 2.772

Assessment of ATR-NIR and ATR-MIR spectroscopy as an analytical tool for the quantification of the total polyphenols in Dendrobium huoshanense

Jing-Wen Hao,Yue Chen,Nai-Dong Chen

In this study, the potentiality of applying attenuated total reflectance near-infrared (ATR-NIR) and attenuated total reflectance mid-infrared (ATR-MIR) techniques combined with a partial least squares (PLS) regression technology to quantify the total polyphenols (TPs) in Dendrobium huoshanense (DHS) was investigated and compared. The real TP contents in the DHS samples were analysed using methods of reference. The capability of the two IR spectroscopic techniques to quantify the TPs in DHS was assessed by the root-mean-square error of calibration (RMSEC) and determination coefficients ( R 2 ). The results showed that both NIR and MIR might be used as a fast and simple tool to replace traditional chemical assays for the determination of the TP contents in DHS, and the best NIR model showed slightly better prediction performance [root-mean-square error of prediction (RMSEP): 0.307, R 2 : 0.9122, ratio performance deviation (RPD): 4.43] than the best MIR model (RMSEP: 0.440, R 2 : 0.9069, RPD: 3.09). Results from this study indicated that both the NIR and MIR models could be used to quantify the TP in DHS, and ATR-NIR appeared to be the more predominant and more robust technique for the quantification of the TP in DHS.

CAS / MDL: 149-91-7
研究领域: 植物化学 · 分析化学 · 药用植物学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYTOCHEMICAL ANALYSIS · 2022 ·Vol. 33 ·期 4 ·599-611 · IF 3.024

Colour, chemical compounds, and antioxidant capacity of Astragali Radix based on untargeted metabolomics and targeted quantification

Mei Yang,Minzhen Yin,Shanshan Chu,Yujiao Zhao,Qingying Fang,Ming'en Cheng,Huasheng Peng,Luqi Huang

Introduction Astragali Radix has been used for over 2000 years in traditional Chinese medicine. Its secondary xylem “Jinjing” and secondary phloem “Yulan” are important for evaluating the quality of the Daodi medicinal material in China. However, its systematic characterisation has not been conducted. Objective This study aims to investigate the colour, chemical compounds, and antioxidant capacity of the secondary xylem and phloem of Astragali Radix on the basis of untargeted metabolomics, broadening the application scope of Astragali Radix in food and pharmaceutical industries. Methods The L* , a* , and b* of the secondary xylem and phloem were measured by colorimetry, and the chemical compounds were identified and quantified by ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and high-performance liquid chromatography-diode array detector-evaporative light scattering detection. 2,2-Diphenyl-1-picrylhydrazyl (DPPH) and 2-azino-bis-(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) assays were conducted to evaluate their antioxidant capacity. Results Thirty-one compounds were identified by UPLC-Q-TOF-MS. The secondary xylem exhibited high parameter b* , flavonoid content, and antioxidant capacity, while the secondary phloem was rich in astragalosides. The colour parameters of well-defined type A significantly varied from those of the other types. Well-defined type A also exhibited the highest antioxidant activity and flavonoid content, followed by middle type A-like, middle type B-like, and yellow shading type B. Conclusion The colour parameters, chemical compounds, and antioxidant capacity among the different transverse sections of secondary xylem and phloem varied. The yellow colour of secondary xylem was correlated to high flavonoid content and antioxidant activity, and well-defined type A of Astragali Radix had better quality than other types.

CAS / MDL: 64-18-6
研究领域: 药用植物学 · 药学 · 食品科学 · 代谢组学 · 传统中药
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYTOCHEMICAL ANALYSIS · 2022 ·Vol. 33 ·期 6 ·895-905 · IF 3.024

Rapid profiling of potential antitumor polymethoxylated flavonoids in natural products by integrating cell biospecific extraction with neutral loss/diagnostic ion filtering-based high-performance liquid chromatography–quadrupole time-of-flight tandem mass spectrometry

Li Cheng,Fang Wang,Yuanxin Cao,Chaoying Tong,Qisheng Wei,Shuyun Shi,Ying Guo

Introduction Citri Reticulatae Pericarpium Viride (CRPV, Qing Pi in Chinese) has been widely used in traditional Chinese medicine. Polymethoxylated flavonoids (PMFs), which are a special group of flavonoids with strong antitumor activity, are broadly distributed in citrus peels. However, systematic investigation of antitumor PMFs in CRPV has received little attention to date. Objectives An MCF-7 cell biospecific extraction method integrated with neutral loss/diagnostic ion filtering-based HPLC-QTOF-MS/MS strategy was developed for rapid and specific profiling of antitumor PMFs and systematic identification of PMFs in CRPV. Methodology By incubating MCF-7 cells with CRPV extract, potential antitumor PMFs specifically bound to cells and were isolated. Then, by systematic investigation of fragmentation pathways, neutral loss and diagnostic ion filtering strategies were proposed to comprehensively and accurately identify PMFs. Results Sixteen antitumor PMFs were unambiguously or tentatively identified. Among them, minor compound 15 (5-hydroxy-6,7,8,3′,4′-pentamethoxyflavone with a free hydroxyl group at C-5) exhibited excellent antitumor activity, with an IC 50 value of 2.81 ± 0.76 μg/mL, which is lower than that of 5-fluorouracil (IC 50 , 4.92 ± 0.83 μg/mL). Nobiletin ( 12 ) and tangeretin ( 16 ), two major PMFs, presented moderate antitumor activities with IC 50 values of 13.06 ± 1.85 and 17.07 ± 1.18 μg/mL, respectively, and their contents were sensitively and precisely determined. Conclusions To the best of our knowledge, this is the first report on the systematic investigation of antitumor PMFs in CRPV. The study will lay a foundation for the quality control and clinical application of CRPV.

CAS / MDL: 67-68-5 51-21-8 298-93-1
研究领域: 中药学 · 分析化学 · 肿瘤学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYTOCHEMICAL ANALYSIS · 2022 ·Vol. 34 ·期 2 ·198-208 · IF 3.024

Quality consistency evaluation of commercial Prunellae Spica by integrating determination of secondary metabolites and saccharides

Xin-Yu Lin,Jing Zhou,Cai-Feng Hao,He Zhu,Shan-Shan Zhou,Jin-Di Xu,Qian Mao,Song-Lin Li,Ming Kong

Introduction Prunellae Spica (PS) is a commonly used medicinal herb in China. Secondary metabolites and saccharides are major bioactive components of PS. However, holistic quality consistency of commercial PS is ambiguous due to lack of comprehensive evaluation methods and reliable quality control markers. Objectives Integrating multiple chromatographic and chemometric methods to comprehensively evaluate the holistic quality of PS. Material and methods Ultrahigh-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (UPLC-TQ-MS/MS) was applied to quantify 12 secondary metabolites of PS. High-performance liquid chromatography coupled with photodiode array/evaporative light scattering detection (HPLC-PDA/ELSD) and high-performance gel permeation chromatography (HPGPC) methods were used to characterise the saccharides. Multivariate statistical analysis was adopted to evaluate the quality consistency of commercial PS and explore the potential quality control markers. Results The contents of secondary metabolites and saccharides were significantly different among commercial PS. All samples could be classified into three groups with ferulic acid, protocatechualdehyde, gallic acid, ursolic acid/oleanolic acid, sucrose, p -coumaric acid, chlorogenic acid as the major contributing components responsible for the difference. The content of rosmarinic acid was correlated with that of betulinic acid, hyperposide, chlorogenic acid, rutin, caffeic acid, p -coumaric acid and glucose, whereas polysaccharides, ferulic acid, protocatechualdehyde and ursolic acid/oleanolic acid, quercetin, sucrose and majority monosaccharides were not. Conclusion The holistic quality of commercial PS was inconsistent. Together with rosmarinic acid, ferulic acid, protocatechualdehyde, ursolic acid/oleanolic acid, polysaccharides and sucrose might be recommended as potential quality control markers for the holistic quality control of PS.

CAS / MDL: 64-19-7 76-05-1
研究领域: 中药学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYTOCHEMICAL ANALYSIS · 2023 ·Vol. 34 ·期 3 ·347-362 · IF 3.3

Rapid identification of chemical components in vitro and in vivo of Menispermi Rhizoma by integrating UPLC-Q-TOF-MS with data post-processing strategy

Jinxia Wei,Yuanyuan Wang,Yue Zhang,Yanxue Zheng,Jia Shao,Wenbo Cheng,Yubo Li

Introduction Menispermi Rhizoma (MR), the dried rhizome of Menispermum dauricum DC. (Menispermaceae), has been used to treat sore throat, enteritis, dysentery, and rheumatic arthralgia. Despite extensive research on its pharmacological effects, the chemical components in vitro and in vivo have not been thoroughly studied. Objective To establish an efficient method for rapid classification and identification of alkaloids in MR and its preparations, as well as metabolites in vivo after oral administration of MR. Methods Rapid identification of alkaloids and absorbed components of MR was performed using ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) coupled with UNIFI software. Moreover, the characteristic fragmentations and neutral losses of different types of alkaloids in MR were summarised to realise the rapid classification of alkaloids. Results A total of 55 components were unambiguously or tentatively identified in MR. Among them, 37 and 31 components were found in MR capsules and tablets, respectively. Meanwhile, 109 compounds were tentatively identified in rat plasma, urine and faeces, including 55 prototypes and 54 metabolites. Hydrogenation, hydroxylation, methylation, glucuronic acid and sulphate conjugations were the dominating metabolic fates of alkaloids. Conclusion The data post-processing strategy established could greatly enhance the structural identification efficiency. The results obtained might lay the foundation for further interpretation of clinical effects, mechanism of action and quality control of MR.

CAS / MDL: 64-17-5
研究领域: 药理学 · 分析化学 · 植物化学 · 代谢组学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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