scholarly journals Rapid Identification of the Chemical Components of Ilex rotunda Thunb Using UPLC-Q-TOF-MS/MS

2021 ◽  
Vol 2021 ◽  
pp. 1-16
Author(s):  
Xinxin Chen ◽  
Junmao Li ◽  
Renyikun Yuan ◽  
Youqiong Zhuo ◽  
Yangling Chen ◽  
...  

Ilicis Rotundae Cortex (IRC) consists of the bark of Ilex rotunda Thunb, and its chemical constituents mainly include flavonoid glycosides, phenols, and triterpenoid saponins. In this study, a preliminary analysis was performed to identify and obtain the chemical components from IRC to better control the quality of the medicinal materials and provide a chemical basis for the study of the efficacy of the active components. Simple and efficient sample pretreatment and ultrasonic-assisted extraction methods were used to analyze the mass spectrum fragments and fracture modes in the anion mode by UPLC-Q-TOF-MS/MS. Using a two-step strategy, the neutral loss, diagnostic ions, and characteristic fragments were studied to screen diverse skeletons and substitutions, and the possible compounds were identified by comparison with databases. The representative compounds were compared with the standard, and the mass spectrogram was found to match perfectly. Thus, our findings reveal that this method is feasible and reliable and can be used to analyze the chemical components of IRC. We identified 105 compounds, including 22 triterpenoid saponins, 15 chlorogenic acids, 33 phenylpropanoids and phenylpropanosides, 3 iridoids, 1 flavonoid, 10 lignans, 12 glycosides, and 9 other compounds. This method lays the foundation for further elucidating the pharmacodynamics of IRC and provides a practical method for the identification of IRC.

2018 ◽  
Vol 2018 ◽  
pp. 1-11 ◽  
Author(s):  
Xin Shao ◽  
Jie Zhao ◽  
Xu Wang ◽  
Yi Tao

Qing-Hua-Yu-Re-Formula (QHYRF), a new herbal preparation, has been extensively used for treating diabetic cardiomyopathy. However, the chemical constituents of QHYRF remain uninvestigated. In the present study, rapid ultrahigh-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UHPLC-Q-TOF/MS) was used to qualitatively analyze the components of QHYRF. Qualitative detection was performed on a Kromasil C18 column through the gradient elution mode, using acetonitrile-water containing 0.1% formic acid. Twenty-seven compounds were identified or tentatively characterized, including 12 phenolic acids, nine monoterpene glycosides, two flavonoids, three iridoids, and one unknown compound. Among these, six compounds were confirmed by comparing with standards. A high-performance liquid chromatography (HPLC) method was developed to simultaneously determine the following six active components in QHYRF: danshensu, paeoniflorin, acteoside, lithospermic acid, salvianolic acid B, and salvianolic acid C. These HPLC chromatograms were monitored at 254, 280, and 320 nm. The method was well validated with respect to specificity, linearity, limit of detection, limit of quantification, precision, stability, and recovery. The HPLC-UV method was successfully applied to 10 batches of QHYRF.


2011 ◽  
Vol 6 (1) ◽  
pp. 1934578X1100600 ◽  
Author(s):  
Jasmina Petreska ◽  
Gjose Stefkov ◽  
Svetlana Kulevanova ◽  
Kalina Alipieva ◽  
Vassya Bankova ◽  
...  

Twenty-one samples of Sideritis species ( S. scardica, S. raeseri, S. taurica, S. syriaca and S. perfoliata) from various locations on the Balkan Peninsula were evaluated for their chemical constituents. Chemical analyses were focused on secondary metabolites, particularly phenolic compounds, which have several roles in the plant physiological processes and have demonstrated significant health beneficial effects. The occurrence of hydroxycinnamic acids, phenylethanoid glycosides and flavonoids has been investigated in taxonomically related taxa of the genus Sideritis. A systematic method for phenolic compounds identification was developed using tandem mass spectrometry coupled to high performance liquid chromatography with diode array detection. Scanning for precursor ions of commonly found phenolics in Sideritis species using LC/MSn with an ion trap instrument permitted the specific determination of hydroxycinnamic acid derivatives, and phenylethanoid and flavonoid glycosides. Further characterization of each phenolic compound was performed using MS/MS production analysis and common–neutral-loss analysis. This online technique allowed identification of three hydroxycinnamic acid derivatives, eight phenylethanoid glycosides, and twenty-four flavonoid glycosides. All the taxa analysed produced very similar phenolic patterns characterized by the presence of 5-caffeoylquinic acid, lavandulifolioside, verbascoside, hypolaetin 7- O-[6′”- O-acetyl]-allosyl(1→2)glucoside, apigenin 7-(4″- p-coumaroylglucoside), 4′- O-methylisoscutellarein 7- O-[6′”- O-acetyl]-allosyl(1→2)glucoside, and minor amounts of isoverbascoside, apigenin 7- O-allosyl(1→2)glucoside, isoscutellarein 7- O-allosyl-(1→2)-[6′- O-acetyl]-glucoside, hypolaetin 7- O-allosyl-(1→2)-[6″- O-acetyl]-glucoside and 4′- O-methylhypolaetin 7- O-[6′”- O-acetyl]-allosyl-(1→2)-[6′- O-acetyl]-glucoside. These results show that the investigated species are systematically very closely related. Phenylethanoid glycosides and flavonoid acetylglycosides are dominant and constitute 90% of the total phenolic compounds compared with hydroxycinnamic acid and flavonoid 7- O-glycosides. Principal component analysis (PCA) was performed for the nature and content of the different compounds to be correlated to the particular Sideritis species and also to the locations.


Molecules ◽  
2019 ◽  
Vol 24 (16) ◽  
pp. 2948 ◽  
Author(s):  
Wang ◽  
Mei ◽  
Liu ◽  
Li ◽  
Zhang ◽  
...  

Astragli Radix (AR) is one of the most popular traditional Chinese medicines with chemical constituents including flavonoids and saponins. As recently evidenced, some fungi or their fermentation liquid may have the potential to affect the bioactive constituents and different pharmacological effects of AR. Thus, the composition of fermented AR (FAR) produced by Paecilomyces cicadae (Miquel) Samson in liquid-state fermentation was investigated using a UHPLC-LTQ-Orbitrap mass spectrometer in both positive and negative ion modes. Firstly, the MSn data sets were obtained based on a data-dependent acquisition method and a full scan–parent ions list–dynamic exclusion (FS-PIL-DE) strategy. Then, diagnostic product ions (DPIs) and neutral loss fragments (NLFs) were proposed for better constituent detection and structural characterization. Consequently, 107 constituents in total, particularly microconstituents in FAR and AR, were characterized and compared in parallel on the same LTQ–Orbitrap instrument. Our results indicated that AR fermentation with Paecilomyces significantly influenced the production of saponins and flavonoids, especially increasing the content of astragaloside IV. In conclusion, this research was not only the first to show changes in the chemical components of unfermented AR and FAR, but it also provides a foundation for further studies on the chemical interaction between microbiota and AR.


2021 ◽  
Author(s):  
wei wei ◽  
Siwei Li ◽  
Linyou Cheng ◽  
Erwei Hao ◽  
Xiaotao Hou ◽  
...  

Abstract Background: Yiganmingmu oral liquid (YGMM), a well known over-the-counter (OTC) drug in China, is composed of 12 types of valuable herbal medicines and has been widely used in clinical for the treatment of soreness and weakness of waist and knees, dizziness, memory loss, and fatigue. However, the chemical compositions of YGMM and its absorbed compounds in plasma remain unclear. Methods: Since chemical investigation is the first important step to reveal effects and action mechanisms of traditional Chinese medicine (TCM), in this study, based on the self built components database, systematic characterization of the chemical profile of YGMM in vivo was carried out by using a reliable UPLC-Q-TOF-MS method. Moreover, to obtain better understanding of the absorbed prototypes in plasma, serum pharmacochemistry analysis of YGMM after oral administration was conducted by using cynomolgus monkeys as animal model. Results: A total of 667 constituents from the 12 single herbal medicines were collected in the self built components database by searching the reported literatures, and 415 of them were initially screened as candidate compounds in YGMM by comparison of their experimental accurate mass measurements with those theoretical values. After that, 117 compounds including 17 phenolic acids, 25 flavonoids, 4 alkaloids, 10 phthalides, 5 monoterpenes, 8 triterpenoid saponins, 9 anthraquinones, and 39 other compounds, were unambiguously identified or tentatively characterized by analysing their MS/MS fragmentation patterns, and also by comparison with reference standards and those data reported in the literatures. 61 prototypes absorbed in plasma of cynomolgus monkey, including 13 phenolic acids, 21 flavonoids, 8 phthalides, 3 monoterpenes, 4 triterpenoid saponins, and 12 other compounds were tentatively assigned by serum pharmacochemistry analysis after oral administration. Conclusion: It was the first comprehensive analysis of chemical constituents of YGMM and prototypes in plasma, and the data analysis strategy developed in this study showed high efficiency in the structural elucidations. The results might provide scientific evidence for further research on material basis of YGMM.


Molecules ◽  
2018 ◽  
Vol 23 (12) ◽  
pp. 3258 ◽  
Author(s):  
Haixing Wang ◽  
Yuanyuan Li ◽  
Yeqing Huang ◽  
Chunyan Zhao ◽  
Hon-Yeung Cheung

Lobelia chinensis is a kind of herbal medicine widely distributed and used in Asia. The chemical components of this herb, however, have not been well studied until now. Lobeline, as an essential and famous bioactive compound in Lobelia genus, has been assumed to be present in L. chinensis. In order to ascertain its presence and, more importantly, proper use of this herb, chemical profiling this herb with highly sensitive and high-resolution analytical mass spectrometry was applied. In this study, high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC/Q-TOF MS) method was employed to systematically profile the chemical constituents of L. chinensis for the first time. Comparative chemical profiling study of L. chinensis and Lobelia inflata was also conducted to provide evidence whether lobeline is present or not. Piperidine alkaloids except for lobeline, alkaloid-lignan hybrids, flavonoids, polyacetylenes, nonanedioic acid, and some new phytochemicals were successfully identified in L. chinensis simultaneously. Comparing to the chemical profiles of L. inflata, lobeline was found to be absent in L. chinensis. All of the secondary metabolites in L. chinensis were determined with the HPLC/Q-TOF MS method. The absence of lobeline in L. chinensis was confirmed after this extensive study.


2021 ◽  
Vol 16 (1) ◽  
Author(s):  
Wei Wei ◽  
Siwei Li ◽  
Linyou Cheng ◽  
Erwei Hao ◽  
Xiaotao Hou ◽  
...  

Abstract Background Yiganmingmu oral liquid (YGMM), a well known over-the-counter (OTC) drug in China, is composed of 12 types of valuable herbal medicines and has been widely used in clinical for the treatment of soreness and weakness of waist and knees, dizziness, memory loss, and fatigue. However, the chemical compositions of YGMM and its absorbed compounds in plasma remain unclear. Methods Since chemical investigation is the first important step to reveal effects and action mechanisms of traditional Chinese medicine (TCM), in this study, based on the self built components database, systematic characterization of the chemical profile of YGMM in vitro was carried out by using a reliable UPLC-Q-TOF-MS method. Moreover, to obtain better understanding of the absorbed prototypes in plasma, serum pharmacochemistry analysis of YGMM after oral administration was conducted by using cynomolgus monkeys as animal model. Results A total of 667 constituents from the 12 single herbal medicines were collected in the self built components database by searching the reported literatures, and 415 of them were initially screened as candidate compounds in YGMM by comparison of their experimental accurate mass measurements with those theoretical values. After that, 117 compounds including 17 phenolic acids, 25 flavonoids, 4 alkaloids, 10 phthalides, 5 monoterpenes, 8 triterpenoid saponins, 9 anthraquinones, and 39 other compounds, were unambiguously identified or tentatively characterized by analysing their MS/MS fragmentation patterns, and also by comparison with reference standards and those data reported in the literatures. 61 prototypes absorbed in plasma of cynomolgus monkey, including 13 phenolic acids, 21 flavonoids, 8 phthalides, 3 monoterpenes, 4 triterpenoid saponins, and 12 other compounds were tentatively assigned by serum pharmacochemistry analysis after oral administration. Conclusion It was the first comprehensive analysis of chemical constituents of YGMM and prototypes in plasma, and the data analysis strategy developed in this study showed high efficiency in the structural elucidations. The results might provide scientific evidence for further research on material basis of YGMM.


2021 ◽  
Vol 2021 ◽  
pp. 1-27
Author(s):  
Hengyu Li ◽  
Hongwei Zhao ◽  
Yong Yang ◽  
Dongmei Qi ◽  
Xiaorui Cheng ◽  
...  

Qi-Fu-Yin, a traditional Chinese medicine formula, has been used to treat Alzheimer’s disease (AD, a neurodegenerative disorder) in clinical setting. In this study, the chemical components of Qi-Fu-Yin and its prototype components and metabolites in rat plasma and cerebrospinal fluid, after oral administration, were preliminarily characterized via ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS). A total of 180 compounds, including saponins, flavonoids, organic acids, sucrose esters, oligosaccharide esters, phthalides, phenylethanoid glycosides, alkaloids, xanthones, terpene lactones, ionones, and iridoid glycoside, were tentatively characterized. For the first time, 51 prototypical components and 26 metabolites, including saponins, phthalides, flavonoids, sucrose esters, organic acids, alkaloids, ionones, terpene lactones, iridoid glycoside, and their derivatives, have been tentatively identified in the plasma. Furthermore, 10 prototypical components (including butylidenephthalide, butylphthalide, 20(S)-ginsenoside Rh1, 20(R)-ginsenoside Rh1, and zingibroside R1) and 6 metabolites were preliminarily characterized in cerebrospinal fluid. These results were beneficial to the discovery of the active components of Qi-Fu-Yin anti-AD.


2021 ◽  
Vol 12 ◽  
Author(s):  
Ruixia Wu ◽  
Yan Liang ◽  
Min Xu ◽  
Ke Fu ◽  
Yangliu Zhang ◽  
...  

Dengzhanxixin (DZXX), the dried whole plant of Erigeron breviscapus (Vaniot) Hand.-Mazz., belonging to Compositae and first published in Materia Medica of South Yunnan by Lan Mao in the Ming Dynasty (1368 AD–1644 AD), is included in Medicinal Materials and Decoction Pieces of the 2020 edition of the Pharmacopeia of the People’s Republic of China. Its main chemical components are flavonoids that mainly include flavonoid, flavonols, dihydroflavones, flavonol glycosides, flavonoid glycosides, coffee acyl compounds, and other substances, such as volatile oil compounds, coumarins, aromatic acids, pentacyclic terpenoids, phytosterols, and xanthones. Among them, scutellarin and 1,5-dicoffeoylquininic acid are the main active components of DZXX. DZXX has pharmacological effects, such as improving cerebral and cerebrovascular ischemia, increasing blood flow, inhibiting platelet aggregation, promoting antithrombotic formation, improving microcirculation, reducing blood viscosity, protecting optic nerves, exhibiting anti-inflammatory properties, scavenging free radicals, and eliciting antioxidant activities. It is widely used in the treatment of cardiovascular and cerebrovascular ischemic diseases, kidney diseases, liver diseases, diabetic complications, and glaucoma. Pharmacokinetic studies have shown that the active components of DZXX have a low bioavailability and a high elimination rate in vivo. Nevertheless, its utilization can be improved through liposome preparation and combination with other drugs. Acute and subacute toxicity studies have shown that DZXX is a safe medicinal material widely used in clinical settings. However, its target and drug action mechanism are unclear because of the complexity of its composition. In this paper, the clinical application and pharmacological toxicology of DZXX are reviewed to provide a reference for further studying its active components and action mechanism.


2020 ◽  
Vol 11 ◽  
Author(s):  
Huijun Wang ◽  
Ruoming Wu ◽  
Dong Xie ◽  
Liqin Ding ◽  
Xing Lv ◽  
...  

Wei-Fu-Chun (WFC) tablet is a commercial medicinal product approved by China Food and Drug Administration, which is made of Panax ginseng C.A.Mey., Citrus aurantium L., and Isodon amethystoides (Benth.). WFC has been popularly used for the treatment of precancerous lesions of gastric cancer (PLGC) in clinical practice. In this study, a UHPLC-ESI-Q-TOF/MS method in both positive and negative ion mode was employed to rapidly survey the major constituents of WFC. 178 compounds including diterpenoids, triterpenes, sesquiterpenes, flavonoids, saponins, phenylpropanoids, lignans, coumarins, organic acids, fatty acids, quinones, and sterols, were identified by comparing their retention times, accurate mass within 5 ppm error, and MS fragmentation ions. In addition, 77 absorbed parent molecules and nine metabolites in rat serum were rapidly characterized by UHPLC-ESI-Q-TOF/MS. The network pharmacology method was used to predict the active components, corresponding therapeutic targets, and related pathways of WFC in the treatment of PLGC. Based on the main compounds in WFC and their metabolites in rat plasma and existing databases, 13 active components, 48 therapeutic targets, and 61 pathways were found to treat PLGC. The results of PLGC experiment in rats showed that WFC could improve the weight of PLGC rats and the histopathological changes of gastric mucosa partly by inhibiting Mitogen-activated protein kinase (MAPK) signaling pathway to increase pepsin secretion. This study offers an applicable approach to identify chemical components, absorbed compounds, and metabolic compounds in WFC, and provides a method to explore bioactive ingredients and action mechanisms of WFC.


Molecules ◽  
2021 ◽  
Vol 26 (21) ◽  
pp. 6634
Author(s):  
Hanze Wang ◽  
Xiaomeng Hou ◽  
Bingqi Li ◽  
Yang Yang ◽  
Qiang Li ◽  
...  

Neural stem cells (NSCs) exist in the central nervous system of adult animals and capable of self-replication. NSCs have two basic functions, namely the proliferation ability and the potential for multi-directional differentiation. In this study, based on the bioassay-guided fractionation, we aim to screen active components in Cuscuta chinensis to promote the proliferation of NSCs. CCK-8 assays were used as an active detection method to track the active components. On the basis of isolating active fraction and monomer compounds, the structures of these were identified by LC-MS and (1H, 13C) NMR. Moreover, active components were verified by pharmacodynamics and network pharmacology. The system solvent extraction method combined with the traditional isolation method were used to ensure that the fraction TSZE-EA-G6 of Cuscuta chinensis exhibited the highest activity. Seven chemical components were identified from the TSZE-EA-G6 fraction by UPLC-QE-Orbitrap-MS technology, which were 4-O-p-coumarinic acid, chlorogenic acid, 5-O-p-coumarinic acid, hyperoside, astragalin, isochlorogenic acid C, and quercetin-3-O-galactose-7-O-glucoside. Using different chromatographic techniques, five compounds were isolated in TSZE-EA-G6 and identified as kaempferol, kaempferol-3-O-glucoside (astragalin), quercetin-3-O-galactoside (hyperoside), chlorogenic acid, and sucrose. The activity study of these five compounds showed that the proliferation rate of kaempferol had the highest effects; at a certain concentration (25 μg/mL, 3.12 μg/mL), the proliferation rate could reach 87.44% and 59.59%, respectively. Furthermore, research results using network pharmacology techniques verified that kaempferol had an activity of promoting NSCs proliferation and the activity of flavonoid aglycones might be greater than that of flavonoid glycosides. In conclusion, this research shows that kaempferol is the active component in Cuscuta chinensis to promote the proliferation of NSCs.


Sign in / Sign up

Export Citation Format

Share Document