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1.
Int J Mol Sci ; 21(5)2020 Mar 04.
Artigo em Inglês | MEDLINE | ID: mdl-32143538

RESUMO

Uncaria alkaloids are the major bioactive chemicals found in the Uncaria genus, which have a long history of clinical application in treating cardiovascular and mental diseases in traditional Chinese medicine (TCM). However, there are gaps in understanding the multiple targets, pathways, and biological activities of Uncaria alkaloids. By constructing the interactions among drug-targets-diseases, network pharmacology provides a systemic methodology and a novel perspective to present the intricate connections among drugs, potential targets, and related pathways. It is a valuable tool for studying TCM drugs with multiple indications, and how these multi-indication drugs are affected by complex interactions in the biological system. To better understand the mechanisms and targets of Uncaria alkaloids, we built an integrated analytical platform based on network pharmacology, including target prediction, protein-protein interaction (PPI) network, topology analysis, gene enrichment analysis, and molecular docking. Using this platform, we revealed the underlying mechanisms of Uncaria alkaloids' anti-hypertensive effects and explored the possible application of Uncaria alkaloids in preventing Alzheimer's disease. These results were further evaluated and refined using biological experiments. Our study provides a novel strategy for understanding the holistic pharmacology of TCM, as well as for exploring the multi-indication properties of TCM beyond its traditional applications.

2.
Phytochem Anal ; 2020 Mar 04.
Artigo em Inglês | MEDLINE | ID: mdl-32130754

RESUMO

INTRODUCTION: Liuwei Dihuang Pills (concentrated pills, simplified as LWDHP), one of the most famous classic Chinese Patent Medicine (CPM), is produced by hundreds of pharmaceutical manufacturers with billions of Chinese yuan (CNY) in annual sales. However, current quality identification of LWDHP mainly relies on a thin-layer chromatography (TLC) method that is complicated and deficient. OBJECTIVE: The goal of this study is to simplify the identification process and provide a more comprehensive quality assessment method of LWDHP by developing an integrated strategy based on liquid chromatography coupled with mass spectrometry (LC-MS) and multivariate statistical analysis. METHOD: Ultra-high-performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UHPLC/QTOF-MS) was employed to perform qualitative analyses of a home-made LWDHP and to establish a stably characteristic compound library by analysis of batches of its component herbs. Then selective ion monitoring (SIM) of single MS was utilised to develop a rapid identification method based on the UHPLC/QTOF-MS analysis result. Multivariate statistical analysis was subsequently used for the quality assessment of different commercial samples. RESULTS: Seventy-eight characteristic compounds were characterised, and 68 of them were recorded to establish a stably characteristic compound library. Thirty-one compounds were selected from the library for the establishment of SIM identification method. Good specificity, capability, and feasibility had been respectively verified by the analysis of blank sample, negative control (NC) preparation samples, home-made LWDHP sample, and commercial sample. Multivariate statistical analysis of 20 batches of commercial LWDHP samples revealed the quality consistency of the same vendor's product and quality difference between diverse vendors' products. CONCLUSION: The SIM identification method by a single analysis could significantly simplify the identification process of LWDHP, and it was performed in a holistic mode for no less than two compounds of each component herb monitored. Moreover, it could also be combined with multivariate statistical analysis to conduct quality assessments of batches of samples. The integrated strategy used in the study of LWDHP could be applied for the identification of other CPM as well.

3.
J Pharm Biomed Anal ; 177: 112813, 2020 Jan 05.
Artigo em Inglês | MEDLINE | ID: mdl-31472326

RESUMO

Differentiated composition in precursor ions for different subclasses of ginsenosides in the negative electrospray-ionization mode has been reported, which lays a foundation for the sorted and untargeted identification of ginsenosides. Carboxyl-free ginsenosides simultaneously from Panax ginseng, P. quinquefolius, and P. notoginseng, were comprehensively characterized and statistically compared. A neutral loss/product ion scan (NL-PIS) incorporated untargeted profiling approach, coupled to ultra-high performance liquid chromatography, was developed on a linear ion-trap/Orbitrap mass spectrometer for characterizing carboxyl-free ginsenosides. It incorporated in-source fragmentation (ISF) full scan-MS1, mass tag-MS2, and product ion scan-MS3. Sixty batches of ginseng samples were analyzed by metabolomics workflows for the discovery of ginsenoside markers. Using formic acid (FA) as the additive, carboxyl-free ginsenosides (protopanaxadiol-type, protopanaxatriol-type, and octillol-type) gave predominant FA-adducts, while rich deprotonated molecules were observed for carboxyl-containing ginsenosides (oleanolic acid-type and malonylated) when source-induced dissociation (SID) was set at 0 V. Based on the NL transition [M+FA‒H]- > [M-H]- and the characteristic sapogenin product ions, a NL-PIS approach was established. It took advantage of the efficient full-information acquisition of ISF-MS1 (SID: 50 V), the high specificity of mass tag (NL: 46.0055 Da)-induced MS2 fragmentation, and the substructure fragmentation of product ion scan-MS3. We could characterize 216 carboxyl-free ginsenosides, and 21 thereof were potentially diagnostic for the species differentiation. Conclusively, sorted and untargeted characterization of the carboxyl-free ginsenosides was achieved by the established NL-PIS approach. In contrast to the conventional NL or PIS-based survey scan strategies, the high-accuracy MSn data obtained can enable more reliable identification of ginsenosides.


Assuntos
Ginsenosídeos/análise , Espectrometria de Massas/métodos , Panax/química , Cromatografia Líquida de Alta Pressão/métodos , Íons/análise , Panax/classificação
4.
Acta Pharm Sin B ; 9(4): 809-818, 2019 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-31384540

RESUMO

Twenty-one protostane-type triterpenoids with diverse structures, including nine new compounds (1-9), were isolated from the of Alisma plantago-aquatica Linn. Structurally, alisolides A‒F (1-6), composed of an oxole group coupled to a five-membered ring, represent unusual C-17 spirost protostane-type triterpenoids. Alisolide H (8) is a novel triterpenoid with an unreported endoperoxide bridge. Alisolide I (9) represents the first example of 23,24-acetal triterpenoid. Their structures were elucidated based on spectroscopic analysis, wherein the absolute configurations of 4‒6, 8 were further confirmed by the Mo2(OAc)4-induced ECD method. Furthermore, all isolates were evaluated for their inhibitory effects on LPS-induced NO production in Caco-2 cells, and all the compounds showed remarkable inhibitory activities, with IC50 values in the range of 0.76-38.20 µmol/L.

5.
Front Pharmacol ; 10: 845, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31417403

RESUMO

The sourcing of plants from multiple botanical origins is a common phenomenon in traditional Chinese medicines. Uncaria Stem with Hooks (UHs) are approved for using five botanical origins in the Chinese Pharmacopoeia (2015 Edition). All five UHs are commonly used for treating hypertension even though the plants have different chromatographic fingerprints based on our previous study. However, their hypotensive effects and metabolic phenotypes have not been fully studied. In the present study, spontaneously hypertensive rats (SHRs) were orally administered five aqueous extracts (4 g crude drug/kg) prepared from the different UHs over a 6-week period. Systolic blood pressure (SBP) was measured every week, and urine was collected after SBP measurement. Untargeted metabonomics was performed using ultra performance liquid chromatography (UPLC) coupled with an LTQ-Orbitrap mass spectrometer. Bidirectional orthogonal projection to latent structures discriminant analysis (O2PLS-DA), Student's t test, and correlation analysis were used for pattern recognition and the selection of significant metabolites. A similar and prolonged reduction in SBP was observed in each of the groups given the five different UHs, while the metabolic profiles were perturbed slightly compared with that of SHR. Further analysis has shown that only a few common, different components were observed within the five groups, which showed the similar antihypertensive effect in spite of the distinct metabolic pathways due to their different alkaloid composition. These results help in understanding the mechanisms of the phenomenon "different species, same effect" of UHs.

6.
Molecules ; 24(13)2019 Jul 02.
Artigo em Inglês | MEDLINE | ID: mdl-31269719

RESUMO

Gastrodia elata Blume (G. elata) is a valuable Traditional Chinese Medicine (TCM) with a wide range of clinical applications. G. elata polysaccharides, as one of the main active ingredients of G. elata, have interesting extraction, purification, qualitative analysis, quantitative analysis, derivatization, and pharmacological activity aspects, yet a review of G. elata polysaccharides has not yet been published. Based on this, this article summarizes the progress of G. elata polysaccharides in terms of the above aspects to provide a basis for their further research and development.


Assuntos
Gastrodia/química , Polissacarídeos/análise , Polissacarídeos/farmacologia , Antineoplásicos/farmacologia , Peso Molecular , Fármacos Neuroprotetores/farmacologia , Polissacarídeos/isolamento & purificação
7.
J Chromatogr A ; 1603: 179-189, 2019 Oct 11.
Artigo em Inglês | MEDLINE | ID: mdl-31255247

RESUMO

Comprehensive analysis and identification of chemical components are very important to evaluate the efficacy and safety of traditional Chinese medicine (TCM). Meanwhile, the discovery of new natural compounds is of great significance for drug exploitation and development. Although two-dimensional liquid chromatography (2D LC) systems expand the peak capacity and improve selectivity and resolution, interpreting the post-processing data is tedious and time-consuming. In this study, an off-line two-dimensional liquid chromatography/ultra-high performance supercritical fluid chromatography tandem quadrupole time-of-flight mass spectrometry (2D LC/UHPSFC-Q-TOF/MS) system was established for systematic chromatographic separation and identification of bufadienolides. Subsequently, the Global Natural Product Social Molecular Networking (GNPS) was applied for dereplication of chemical components of adjacent fractions with high efficiency and accuracy. The key parameters which affected separation and detection with respect to chromatographic conditions and mass spectrometry conditions were optimized. The extract of Venenum Bufonis was fractionated into forty fractions by first-dimensional reversed phase high-performance liquid chromatography (HPLC), which were further analyzed by the second-dimensional UHPSFC-Q-TOF/MS in positive ion mode. The data of forty fractions was imported into GNPS and processed automatically within about five hours. Furthermore, the chemical components with similar featured fragments were classified into the same cluster, which was helpful for components identification. A total of 229 bufadienolides were characterized and two subclasses of compounds (bufogenins conjugated with carboxylic acid and N-heterocyclic bufogenins) were found in Venenum Bufonis for the first time. In addition, UHPSFC exhibited powerful separation ability of isomers in Venenum Bufonis. In this analysis, two new compounds were isolated and fully characterized by NMR verifying the feasibility of this combined analytical strategy. This integrated strategy can improve the efficiency in the detection of new compounds and offer greater observation of isomers from medicinal herbs and other natural sources.


Assuntos
Bufanolídeos/isolamento & purificação , Animais , Produtos Biológicos/análise , Bufanolídeos/química , Bufonidae , Cromatografia Líquida de Alta Pressão , Cromatografia de Fase Reversa , Espectroscopia de Ressonância Magnética , Espectrometria de Massas em Tandem
8.
Phytomedicine ; 60: 152971, 2019 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-31178234

RESUMO

BACKGROUND: Resibufogenin is one of the main active compounds of Venenum Bufonis and exhibits diverse pharmacological activities. It is brought into focus for its potency in heart failure and cancer therapy. PURPOSE: The purpose of this study was to establish a convenient and effective method which was used to simultaneously determine the resibufogenin and its metabolites in rat plasma for further understanding the metabolic profiles of resibufogenin in vivo and pharmacokinetic study by LC-MS/MS. METHODS: The analytes were separated on a BEH C18 column with a mobile phase of water containing 0.05% formic acid and acetonitrile under gradient elution at a flow rate of 0.4 ml/min. Resibufogenin and its eight metabolites were quantified in positive electrospray ionization and MRM mode with transitions of m/z 385.5→349.2 for resibufogenin; m/z 513.7→145.3 for IS (internal standard); m/z 401.23→365.21, m/z 417.23→285.21 and m/z 385.24→349.21 for three main metabolites (hydroxylated-resibufogenin; dihydroxylated-resibufogenin and 3-epi-resibufogenin, respectively). RESULTS: This method was successfully validated with a good linearity over the concentration ranges of 1-200 ng/ml for resibufogenin and the correlation coefficients was more than 0.990. The lower limit of quantification was 1 ng/ml and the precision and accuracy values were less than 15%. The method was applied to study the metabolic profiles of resibufogenin in rat plasma after oral administration of 20 mg/kg. The results indicated that the metabolic reactions of resibufogenin were mainly hydroxylation, dihydroxylation, dehydrogenation and isomerization. Totally eleven metabolites were identified, among which eight were successfully quantified. CONCLUSION: The results could provide further research foundation for the mechanisms study of activity and toxicity in vivo and facilitate the appropriate clinical application of resibufogenin.


Assuntos
Bufanolídeos/farmacocinética , Metaboloma , Administração Oral , Animais , Bufanolídeos/administração & dosagem , Bufanolídeos/metabolismo , Cromatografia Líquida , Estabilidade de Medicamentos , Medicamentos de Ervas Chinesas , Masculino , Ratos , Ratos Wistar , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Espectrometria de Massas em Tandem
9.
Molecules ; 24(9)2019 Apr 28.
Artigo em Inglês | MEDLINE | ID: mdl-31035327

RESUMO

Characterization and determination of metabolites to monitor metabolic pathways play a paramount role in evaluating the efficacy and safety of medicines. However, the separation and quantification of metabolites are rather difficult due to their limited contents in vivo, especially in the case of Chinese medicine, due to its complexity. In this study, an effective and convenient method was developed to simultaneously quantify bufalin and its nine metabolites (semi-quantitation) in rat plasma after an oral administration of 10 mg/kg to rats. The prototype and metabolites that were identified were subsequently quantified using positive electrospray ionization in multiple reaction monitoring (MRM) mode with transitions of m/z 387.4→369.6 and 387.4→351.3 for bufalin, m/z 513.7→145.3 for IS, and 387.4→369.6, 419.2→365.2, and 403.2→349.2 for the main metabolites (3-epi-bufalin, dihydroxylated bufalin, and hydroxylated bufalin, respectively). The method was validated over the calibration curve range of 1.00-100 ng/mL with a limit of quantitation (LOQ) of 1 ng/mL for bufalin. No obvious matrix effect was observed, and the intra- and inter-day precisions, as well as accuracy, were all within the acceptable criteria in this method. Then, this method was successfully applied in metabolic profiling and a pharmacokinetic study of bufalin after an oral administration of 10 mg/kg to rats. The method of simultaneous determination of bufalin and its nine metabolites in rat plasma could be useful for pharmacokinetic-pharmacodynamic relationship research of bufalin, providing experimental evidence for explaining the occurrence of some adverse effects of Venenum Bufonis and its related preparations.


Assuntos
Antineoplásicos/farmacocinética , Bufanolídeos/farmacocinética , Metaboloma , Metabolômica , Animais , Antineoplásicos/química , Bufanolídeos/química , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Metabolômica/métodos , Estrutura Molecular , Controle de Qualidade , Ratos , Reprodutibilidade dos Testes , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem
10.
Phytomedicine ; : 152918, 2019 Apr 03.
Artigo em Inglês | MEDLINE | ID: mdl-30979691

RESUMO

BACKGROUND: Danqi Tongmai tablet (DQTM), a combination of salvianolic acids (SA) and panax notoginsenosides (PNS), is now in phase II clinical trial developed for the treatment of cardiovascular diseases. However, the mechanisms of its protective effects through regulating endogenous metabolites remain unclear. PURPOSE: The purpose of this study was to explore the protective effects of DQTM on acute myocardial ischemia rats by comprehensive metabolomics profiling. STUDY DESIGN: The rats were divided into three groups: sham-operating, acute myocardial ischemia (AMI) and DQTM groups. The plasma and heart were collected and profiled by LC-MS based metabolomics and lipidomics. Based on the identified differential metabolites, the pathway analysis results were obtained and further validated using the network pharmacology approach. METHODS: The AMI model was induced by ligating the left anterior descending coronary artery. The metabolomics and lipidomics profiling were based on two established LC-QTOF/MS analysis methods. The raw data were processed using XCMS Online, then the differential metabolites with nonparametric t-test p value less than 0.05 were selected and identified using HMDB and METLIN. The pathway analysis was conducted using MetaboAnalyst and validated with the predicted network results obtained by BATMAN-TCM. RESULTS: The metabolomics and lipidomics profiles of plasma and heart in response to AMI and DQTM were significantly different. The AMI operation had a serious influence on metabolites in heart ischemia region, while DQTM had a greater impact on lipids in heart non-ischemia region. A total of 151 differential metabolites were identified, including mainly amino acids and fatty acids. Multiple metabolic pathways were disturbed after AMI and could be restored by DQTM, of which arachidonic acid metabolism was further validated with the predicted results of network pharmacology. CONCLUSION: The protective effects of DQTM on acute myocardial ischemia rats could be achieved through the regulation of multiple metabolic pathways.

11.
J Ethnopharmacol ; 237: 215-235, 2019 Jun 12.
Artigo em Inglês | MEDLINE | ID: mdl-30905791

RESUMO

ETHNOPHARMACOLOGICAL RELEVANCE: The animal medicine of Venenum Bufonis (VB), a product of the secretions of Bufo gargarizans Cantor or B. melanostictus Schneider, has long been used as a traditional Chinese medicine (TCM) for the treatment of sunstroke and faint, acute filthy disease - abdominal pain or vomiting and diarrhea, etc. AIM OF THE REVIEW: This review is aimed at providing the comprehensive and up-to-date information of VB as regards its ethnopharmacological uses, constituents and their metabolism, pharmacokinetics, pharmacology and toxicology, all of which could be used as fundamental data for future research as well as development of new drugs. MATERIALS AND METHODS: The information and data about the studies of VB were collected from scientific journals, material medica, historical documents, library, and electronic databases (PubMed, Google Scholar, Science Direct, Researchgate, Web of Science and CNKI). RESULTS: To date, about 142 bufadienolides and 16 indole alkaloids have been isolated from VB in total. The extract and isolated compounds showed a wide range of in vitro and in vivo pharmacologic effects, such as cardiotonic, anti-tumor, antinociceptive, anti-inflammatory, anesthetic and antimicrobial activities. Especially, bufadienolides have been extensively studied due to its powerful anti-tumor activities against various cancer cells. Furthermore, their metabolites and metabolic pathways were concluded in detail, and the main metabolic pathways of bufadienolides were hydroxylation, 3-isomerization, 3-keto, 16-hydrolyzation, 3-O-sulfate and 3-O-glucuronide. CONCLUSIONS: Although VB possesses significant anti-tumor effect against various cancer cell lines, the development of new drugs still remains to be a challenge due to its pharmacodynamic effects in vivo, druggability and toxicology. The main problem lies in its side effects in vivo, poor bioavailability, fast metabolism, cardiotoxicity and neurovirulence. Besides, studies on its metabolism and toxicology in vitro and in vivo, as well as clinical trials should be further conducted for the new drug development and the establishment of optimal dosage of consumption of its administration.


Assuntos
Bufanolídeos , Medicina Tradicional Chinesa , Animais , Bufanolídeos/química , Bufanolídeos/farmacologia , Bufanolídeos/uso terapêutico , Humanos , Compostos Fitoquímicos/análise
12.
J Pharm Biomed Anal ; 166: 52-65, 2019 Mar 20.
Artigo em Inglês | MEDLINE | ID: mdl-30609394

RESUMO

Danqi Tongmai tablet (DQTT), an innovative TCM formula under clinical trials, is composed of salvianolic acids (SA) and panax notoginsenosides (PNE) for the treatment of coronary heart disease and angina pectoris. However, the in vivo herb-herb interaction of DQTT remains unclear. In the present research, a rapid, reliable and sensitive method for quantitative analysis of multi-notoginsenoside in rat plasma based on ultra high performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-TQ/MS) was established and then applied to explore the herb-herb interaction mechanism of DQTT based on the pharmacokinetics in acute myocardial ischemia (AMI) and sham rats after oral administration of DQTT and PNE. Compared with sham rats after oral administration of PNE, the values of AUC0-t for Rf and Rb2 were significantly higher in DQTT group. Compared with AMI rats after oral PNE, AUC0-t for NR1, Rg1, Re, Rb1, Rd, Rg2, Rb2, NR2, Rh1, F1 and F2 were significantly increased after oral administration of DQTT. These results hinted that SA could improve the bioavailability of notoginsenosides in AMI rats, which provides scientific information for better understanding the herb-herb interaction mechanism and offers a reference for clinical administration of DQTT. Additionally, the presently developed methodology was simple, robust, accurate, precise, and would be useful for the pharmacokinetic studies for all kinds of notoginsenosides and other herbal saponins.


Assuntos
Medicamentos de Ervas Chinesas/farmacologia , Ginsenosídeos/farmacocinética , Interações Ervas-Drogas , Panax/metabolismo , Animais , Disponibilidade Biológica , Ginsenosídeos/sangue , Masculino , Isquemia Miocárdica/sangue , Ratos , Comprimidos
13.
Biomed Chromatogr ; 33(2): e4385, 2019 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-30242797

RESUMO

Salvia miltiorrhiza, one of the most well-known herbal medicines, is commonly used for the treatment of coronary heart diseases in China. Besides traditional decoction slices (TDS), another relatively new product of S. miltiorrhiza, ultrafine granular powder (UGP; D90 < 45 µm), is also increasingly being used. In this paper, a UHPLC-LTQ-Orbitrap MS technique was developed for a metabolite profile study after oral administration of UGP and TDS of S. miltiorrhiza. The results showed that the number of in vivo absorbed compounds from UGP was much greater than that from TDS, and different types of products from S. miltiorrhiza will have different metabolic processes in vivo. Furthermore, a UHPLC-Q-Trap MS/MS method for simultaneously determining four tanshinones (tanshinone IIA, dihydrotanshinone I, tanshinone I and cryptotanshinone) was established and applied to assess the pharmacokinetics of the two types of products. All of the analytes displayed significant higher area under the concentration-time curve and peak concentration after oral administration of UGP than after TDS, indicating that ultrafine powder product could improve the bioavailability and absorption of cryptotanshinon,tanshinone II A,dihydrotanshinonE I and tanshinone I in vivo. The present study provides scientific information for further exploration of the pharmacology of these two types of S. miltiorrhiza and offers a reference for clinical administration of S. miltiorrhiza.


Assuntos
/sangue , Medicamentos de Ervas Chinesas/análise , Medicamentos de Ervas Chinesas/farmacocinética , Salvia miltiorrhiza , /química , Administração Oral , Animais , Cromatografia Líquida de Alta Pressão , Medicamentos de Ervas Chinesas/administração & dosagem , Medicamentos de Ervas Chinesas/química , Modelos Lineares , Masculino , Espectrometria de Massas , Pós , Ratos , Ratos Wistar , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
14.
Molecules ; 23(12)2018 Dec 11.
Artigo em Inglês | MEDLINE | ID: mdl-30544925

RESUMO

By investigating of the roots of Salvia miltiorrhiza, which is one of the most widely used Chinese herbs, we used phytochemical methods successfully to obtain twelve depsides: four depsides (1⁻4) that were previously undescribed, along with eight known ones (5⁻12). Their structure characteristics were assessed by HR-ESIMS, CD, NMR (¹H, 13C, HSQC, HMBC) data analyses. These four newly isolated compounds (1⁻4), as well as the other eight compounds (5⁻12), show extraordinary protective effects on hydrogen peroxide-induced apoptosis in HS-SY5Y cells. Among them, depside 4 and depside 6 displayed more obviously protective effects than others.


Assuntos
Depsídeos/química , Depsídeos/farmacologia , Fármacos Neuroprotetores/farmacologia , Salvia miltiorrhiza/química , Linhagem Celular , Dicroísmo Circular , Depsídeos/isolamento & purificação , Avaliação Pré-Clínica de Medicamentos/métodos , Humanos , Espectroscopia de Ressonância Magnética , Estrutura Molecular , Fármacos Neuroprotetores/química , Plantas Medicinais/química
15.
Molecules ; 23(11)2018 Nov 19.
Artigo em Inglês | MEDLINE | ID: mdl-30463184

RESUMO

The mass spectrometry (MS) has been widely used for profiling chemical components of traditional Chinese medicine (TCM). However, there are few studies reporting quality control of TCM based on mass spectrometry fingerprint (MSF) due to its complicated operation and high cost. The aim of this study was to extend the application of MSF for quality evaluation of TCM. In this study, an MSF based on single quadrupole mass spectrometry method was established, and was successfully used for the quality control of Venenum bufonis (VB), a famous TCM which was used clinically for cancer treatment in China. The results showed that the superiority of MSF for more chemical information exposure and the finding of more potential chemical markers (eight versus four) compared with the traditional photo-diode array (a kind of ultra violet detector, PDA). Besides, the performance of MSF was also validated by similarity and principle component analysis (PCA) of MS data acquired on two other mass spectrometry (low-resolution, triple quadrupole, QQQ, and high-resolution, quadruple time-of-flight, Q-TOF), showing high consistency with QQQ and Q-TOF, but robustness with few parameters' settings. Based on our study, MSF could be widely applied for the quality control of TCM.


Assuntos
Bufanolídeos/análise , Medicamentos de Ervas Chinesas/análise , Espectrometria de Massas/métodos , Análise de Componente Principal/métodos , Bufanolídeos/química , Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/química , Extratos Vegetais/análise , Extratos Vegetais/química , Controle de Qualidade
16.
J Sep Sci ; 41(22): 4212-4221, 2018 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-30168286

RESUMO

Tribulus terrestris L. is a well-known medicinal plant from subtropical areas. In China Pharmacopoeia, only the fruit of T. terrestris is recorded to be the medicinal part. But some pharmaceutical preparations and food supplements made of total saponins of aerial part of T. terrestris including fruits, stems, and leaves are commercially available. However, steroidal saponins in different parts have not been studied extensively. So differentiating three parts and ensuring reasonable application of T. terrestris has been an important issue. Herein, we developed an integrated platform based on components profiling and chemometrics analysis to comparatively characterize and investigate steroidal saponins in three parts. As a result, a total of 84 steroidal saponins were characterized or tentatively identified, including 20 compounds reported for the first time. A clear separation of the three parts was achieved by partial least squares discriminant analysis based on the identified saponins, and 17 saponins were screened as biomarkers. Support vector machines model established based on 17 markers showed excellent predication accuracy of 100%. Finally, different distribution of steroidal saponins in three parts was shown obviously by heatmap visualization. These results provide promising perspectives for quality control of Chinese medicine, especially those with different medical parts.


Assuntos
Componentes Aéreos da Planta/química , Saponinas/análise , Esteroides/análise , Tribulus/química , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas , Conformação Molecular
17.
J Chromatogr A ; 1571: 213-222, 2018 Oct 12.
Artigo em Inglês | MEDLINE | ID: mdl-30146372

RESUMO

Specific analytical approaches that enable untargeted profiling of modified metabolites are in great need. An untargeted profiling strategy, by integrating in-source collision-induced dissociation (ISCID)-MS1, mass tag-MS2, and neutral loss scan-MS3, is established on a linear ion-trap/Orbitrap mass spectrometer coupled to ultra-high performance liquid chromatography. This strategy is applied to screen malonylginsenosides from three reputable Panax species (P. ginseng, P. quinquefolius, and P. notoginseng). In light of the preferred neutral elimination of CO2 and entire malonyl substituent (C3H2O3) in the negative electrospray ionization mode, a pseudo-neutral loss scan (PNL) method was established by applying ISCID energy 40 V in MS1, mass tag 43.9898 Da oriented CID-MS2 at normalized collision energy (NCE) 30%, and neutral loss 43.9898 Da-triggered high-energy C-trap dissociation-MS3 at NCE 70%. The PNL approach achieved a high coverage of targeted malonylginsenosides but introduced less false positives. It displayed comparable performance to a precursor ions list-driven targeted approach we have reported in the profiling and characterization of malonylginsenosides, but could avoid complex data processing. Totally 178 malonylginsenosides were characterized from the roots, leaves, and flower buds of P. ginseng, P. quinquefolius, and P. notoginseng, and most of them possess potentially new structures. The compositions of malonylginsenosides identified from these three Panax species are similar, and only malonylginsenoside Rb2 and some minor may have potential chemotaxonomic significance. In conclusion, we provide a potent analytical strategy for the direct and efficient screening of modified metabolites, which may have broad applications in the fields of metabolomics, drug metabolism, and natural product research.


Assuntos
Ginsenosídeos/análise , Panax/química , Espectrometria de Massas por Ionização por Electrospray/métodos , Cromatografia Líquida de Alta Pressão , Flores/química , Flores/metabolismo , Ginsenosídeos/química , Panax/metabolismo , Folhas de Planta/química , Folhas de Planta/metabolismo , Raízes de Plantas/química , Raízes de Plantas/metabolismo
18.
Phytomedicine ; 45: 1-7, 2018 Jun 01.
Artigo em Inglês | MEDLINE | ID: mdl-29576266

RESUMO

BACKGROUND: Lipids, a group of primary metabolites, could be used as quality markers of Traditional Chinese medicine. PURPOSE: The present study was designed to develop a research method to explore lipid markers of the quality of coix seeds with different geographical origins. STUDY DESIGN: The geographical origins of coix seeds were divided into three regions based on the latitude. A central composite design (CCD test) was used to optimize the chromatographic parameters of supercritical fluid chromatography to obtain optimal lipid profile of coix seed. METHODS: An untargeted method based on ultra-performance convergence chromatography - quadrupole/time-of-flight hybrid mass spectrometry (UPC2-QTOF) was developed. Four chromatographic parameters were optimized using CCD test, and a fusion index established by Derringer function was used to evaluate. The lipid profile of 27 batches of coix seeds were acquired and processed by Progenesis QI software, and the MS/MS spectrums were obtained to identify, simultaneously. The difference lipids were explored by orthogonal partial least squares discriminant analysis (OPLS-DA). The lipids that showed differences depending on their seeds' geographical origin were selected as markers of the quality of coix seeds from the three regions. RESULTS: A Torus 2-PIC (1.7 µm, 100 mm × 3.0 mm) was selected as the optimal column of the untargeted method which the run time was only 8 minutes. From the CCD test, the interaction of chromatographic parameters between column temperature and backpressure was founded which the optimal parameters were 55 °C and 2600 psi, respectively. Thirty-two peaks in the lipid profile of coix seed were tentatively identified, of which 20 were triglyceride, and 12 were diglyceride. Nine features that could potentially be used to distinguish the coix seeds by their geographical origin were identified, most of which were diglycerides, such as OP. CONCLUSIONS: Our findings confirm that UPC2-QTOF combined with chemometrics could be used as an efficient method for exploring potential lipid markers of the quality of herbal medicine.


Assuntos
Biomarcadores/análise , Cromatografia com Fluido Supercrítico/métodos , Coix/química , Lipídeos/análise , Sementes/química , Plantas Medicinais/química , Espectrometria de Massas em Tandem/métodos
19.
J Chromatogr A ; 1548: 64-75, 2018 May 04.
Artigo em Inglês | MEDLINE | ID: mdl-29588100

RESUMO

Lipidomics currently is still confronted with challenges from chromatographic separation and lipids identification. Here we report a lipidomics platform by integrating ultrahigh performance supercritical fluid chromatography/quadrupole time-of-flight mass spectrometry (UHPSFC/QTOF-MS) and collision cross section (CCS) measurement using ion mobility spectroscopy/time-of-flight mass spectrometry (IMS/QTOF-MS), aiming to enhance the profiling performance and identification reliability of lipids. The lipidomes extracted from three congeneric Panax species (P. ginseng, P. quinquefolius, and P. notoginseng) by methyl tert-butyl ether are comprehensively profiled and compared by use of this platform. A potent UHPSFC/QTOF-MS approach was developed on a 1.7-µm particles packed Torus 2-PIC column using CH3OH (in CO2) as a modifier and CH3OH/0.2 mM ammonium acetate as the makeup liquid, enabling well resolution of six lipid subclasses by both positive and negative MSE modes. In contrast to the reversed-phase chromatography, "normal-phase" like elution order and better resolution of polar lipids and some lipid isomers were achieved by UHPSFC separation. Pattern recognition chemometric analysis of 60 batches of Ginseng samples ultimately unveiled 24 lipid markers, of which triacylglycerols were the most important. Aside from the automated MS database searching against HMDB and LIPID MAPS, the application of CCS retrieval or CCS prediction improved lipid identification by reducing the possible hits. In conclusion, this integral platform can significantly improve the chromatographic separation and the reliability of lipids identification in lipidomics studies. It is the first report that systematically compares the lipidomic difference of three reputable Panax species, providing useful information for their quality control in addition to ginsenoside analysis.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Cromatografia com Fluido Supercrítico/métodos , Metabolismo dos Lipídeos , Espectrometria de Massas/métodos , Metaboloma , Panax/metabolismo , Eletricidade , Íons , Panax/química , Reprodutibilidade dos Testes , Reologia , Soluções , Temperatura Ambiente
20.
Planta Med ; 84(6-07): 457-464, 2018 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-29388182

RESUMO

Triglycerides are the primary constituents of some seed kernels used in traditional Chinese medicine. Quality control of seed kernels containing multiple components with an environmentally friendly method is indispensable for establishing their quality standards (called monographs) in pharmacopeia. Using coix seeds (Semen Coicis) as an example, a green quantification strategy was proposed by combining C8 core-shell particles with single standard to determine multicomponent technologies to quantify seven triglycerides simultaneously. A core-shell column, namely, Halo C8 (3.0 × 100 mm, 2.7 µm), was used. Methanol was used as the mobile phase at a flow rate of 0.3 mL/min, enabling UV detection of the elutes. Seven triglycerides were well separated in 20 min, and simultaneously quantified using triolein as a single standard. The conversion factor for each standard was set as 1.0 on ELSD, while for the conversion factors at 203 nm, the values increased with the reduction of linoleate. The recovery values were all in the range of 97 - 107% (RSD < 3.0%). The RSD values of precision, including intraday and intermediate precision, were < 3.0% when the total content of triglycerides was calculated. The linearity reached r ≥ 0.9990, and the limit of quantitation reached 40 - 70 ng. Forty-nine batches of coix seeds from four different places of origins and eight batches of adulterants were evaluated and differentiated using principal component analysis. In addition, the validated method was used successfully to quantity seven triglycerides in Semen Persicae, Semen Armeniacae Amarum, and Semen Pruni.


Assuntos
Química Verde/métodos , Medicina Tradicional Chinesa , Sementes/química , Triglicerídeos/análise , Cromatografia Líquida de Alta Pressão/métodos , Coix/química , Medicina Tradicional Chinesa/métodos
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