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1.
J Pharm Biomed Anal ; 185: 113215, 2020 Mar 02.
Artigo em Inglês | MEDLINE | ID: mdl-32199327

RESUMO

Herbal medicine (HM) has been playing a pivotal role in maintaining human health since ancient times, and its therapeutic theory and clinical experience are the precious traditional medical knowledge reserves. As HM occupies an important position in its own right in global healthcare systems, robust quality assessment and control over its complex chemical composition was of great significance to assure its efficacy and safety. Over the past decades, the concept of HM chemical fingerprints aiming to obtain a comprehensive characterization of complex chemical matrices has become one of the most convincing tools for the quality assessment of HM. This review summarizes the recent analytical techniques used to generate HM chemical fingerprints, including chromatography, vibrational spectroscopy, nuclear magnetic resonance spectroscopy, and mass spectrometry. The advantages, drawbacks, and the application scope of each technology have been scrutinized in an attempt to better understand the data analysis. Furthermore, HM fingerprints together with multivariate and multiway chemometrics methods used for different application domains, such as similarity, exploratory, classification, and regression analysis, have also been discussed and illustrated with a few typical studies. The article provides a general picture and workflow of fingerprinting analyses that have been used for the quality assessment of HM.

2.
Molecules ; 25(5)2020 Mar 09.
Artigo em Inglês | MEDLINE | ID: mdl-32182812

RESUMO

Gentianae Radix et Rhizome (Longdan in Chinese, GRR) in Chinese Pharmacopoeia is derived from the dried roots and rhizomes of Gentiana scabra and G. rigescens, that have long been used for heat-clearing and damp-drying in the medicinal history of China. However, the characterization of the chemical components of two species and the screening of chemical markers still remain unsolved. In current research, the identification and characterization of chemical components of two species was performed using ultra-high-performance liquid chromatography (UHPLC) coupled with linear ion trap-Orbitrap (LTQ-Orbitrap) mass spectrometry. Subsequently, the chemical markers of two species were screened based on metabolomics and multivariate statistical analysis. In total, 87 chemical constituents were characterized in G. scabra (65 chemical constituents) and G. rigescens (51 chemical constituents), with 29 common chemical constituents being discovered. Thereafter, 11 differential characteristic components which could differentiate the two species were designated with orthogonal partial least squares discriminant analysis (OPLS-DA) and random forest (RF) iterative modeling. Finally, seven characteristic components identified as (+)-syringaresinol, lutonarin, trifloroside, 4-O-ß-d-glu-trifloroside, 4″-O-ß-d-glucopyranosy1-6'-O-(4-O-ß-d-glucaffeoyl)-linearroside, macrophylloside a and scabraside were selected as the chemical markers for the recognition of two Gentiana species. It was implied that the results could distinguish the GRR derived from different botanical sources, and also be beneficial in the rational clinical use of GRR.

3.
J Chromatogr A ; : 460850, 2020 Jan 03.
Artigo em Inglês | MEDLINE | ID: mdl-31983414

RESUMO

In-source fragmentation of ginsenosides in the positive ESI mode (pISF-G) frequently occurs, which results in little fragment information useful for the structural elucidation. We are aimed to unveil the genesic mechanism and explore its potential significance in quality control of Ginseng and the related compound formulae. By applying six high-resolution mass spectrometers from Agilent, Waters, and Thermo Fisher, we could primarily demonstrate the susceptibility of pISF-G. The ion clusters in the positive full-scan MS1 spectra were generated from the protonated sapogenins by successive elimination of H2O, and showed specificity for ginsenoside classification. Selective ion monitoring (SIM) of the sapogenin product ions could delineate group-target ginsenoside profiles from Ginseng. A high-selectivity characteristic chromatogram (CC) was elaborated for Ginseng, on the Vion™ IMS-QTOF mass spectrometer by IM (ion mobility) separation and quadrupole filtering of four sapogenin fragments (m/z 407.37/CCS 206.24 Å2; m/z 423.36/CCS 211.26 Å2; m/z 439.36/CCS 209.60 Å2; m/z 457.37/CCS 217.81 Å2). Chemometric analysis, based on the CC data of seven Ginseng drugs (P. ginseng, P. quinquefolius, P. notoginseng, Red ginseng, leaf of P. ginseng, P. japonicus, and P. japonicus var. major), disclosed 35 marker compounds. We could readily discriminate among P. ginseng, P. quinquefolius, and P. notoginseng, in 15 different compound formulae by identifying these marker compounds on both the Vion IMS-QTOF and QTrap 4500 mass spectrometers. Conclusively, SIM of the pISF-G sapogenin product ions renders a new concept of CC enabling the group-target profiling of ginsenosides and authentication of Ginseng and the related compound formulae.

4.
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
5.
J Ethnopharmacol ; 251: 112490, 2019 Dec 27.
Artigo em Inglês | MEDLINE | ID: mdl-31884035

RESUMO

ETHNOPHARMACOLOGICAL RELEVANCE: Venenum Bufonis, a product of the secretions of Bufo gargarizans Cantor or B. melanostictus Schneider, possessed an array of pharmacological activities, such as cardiotonic, anti-tumor, antinociceptive, anti-inflammatory, anesthetic and antimicrobial activities. However, there were few efficient methods for quality evaluation of Venenum Bufonis medicinal materials and its related Chinese patent medicines. AIM OF THE STUDY: To establish an effective method for quality assessment of crude drugs and Chinese proprietary medicines of Venenum Bufonis, and explore the relationship of primary compounds - target - pathway - disease through a series of network databases. MATERIALS AND METHODS: An ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-QqQ-MS/MS) method was developed and validated to simultaneously determine 14 bufadienolides for quantitative analysis of 71 batches of crude drugs and 20 kinds of Chinese patent medicines of Venenum Bufonis. Multiple reaction monitoring with good specificity and accuracy was applied to monitor the 14 bufadienolides in positive mode. RESULTS: The methodology was validated with good specificity, precision, stability, repeatability and recovery. The low limits of quantification were in the range of 0.1-2.7 ng/mL. The relative standard deviation values for intra- and inter-day precisions ranged from 0.98% to 6.3% and from 2.39% to 6.76%, respectively. The recovery was varied from 87.78% to 110.57% for crude drugs and 88.32%-100.96% for Chinese proprietary medicine (Shexiang Baoxin Pill). The contents of 14 analytes in 71 batches of crude drugs and 20 sorts of Chinese proprietary medicines were procured, the results showed that the contents of crude drugs collected from the market exhibited great variations. Furthermore, 13 batches of crude drugs were identified as counterfeit with no bufadienolides detected. In addition, the total contents of bufadienolides in the same drug showed great difference among products from various manufacturers or brands. Subsequently, 9 bufadienolides with the higher contents were applied to screen the anti-tumor effect by network pharmacology, and 8 pathways which had prior correlation with bufadienolides were disclosed. CONCLUSION: This method could be used for quality assessment of crude drugs and Chinese patent medicines of Venenum Bufonis, and the data could be served as the fundamental basis for drug research and development of Venenum Bufonis.

6.
Chin J Nat Med ; 17(8): 631-640, 2019 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-31472901

RESUMO

Characterization of aqueous extract in traditional Chinese medicine (TCM) is challenging due to the poor retention of the analytes on conventional C18 columns. This study presents a systematic characterization method based on a rapid chromatographic separation (8 min) on a polar-modified C18 (Waters Cortecs T3) column of aqueous extract of Cordyceps sinensis. UHPLC-HRMS method was used to profile components in both untargeted and targeted manners by full MS/PIL/dd-MS2 acquisition approach. The components were identified or tentatively identified by reference standards comparison, fragmentation rules elucidation and available databases search. A total of 91 components, including 10 nucleobases, 20 nucleosides, 39 dipeptides, 18 amino acids and derivatives and 4 other components, were characterized from the aqueous extract of C. sinensis. And this was the first time to systematically report the presence of nucleosides and dipeptides in C. sinensis, especially for modified nucleosides. The chemical basis inquiry of this work would be beneficial to mechanism exploration and quality control of C. sinensis and related products. Meanwhile, this work also provided an effective solution for characterization of aqueous extract in TCM.


Assuntos
Cromatografia Líquida de Alta Pressão , Cordyceps/química , Espectrometria de Massas em Tandem , Aminoácidos/química , Cromatografia Líquida de Alta Pressão/normas , Dipeptídeos/química , Medicina Tradicional Chinesa , Estrutura Molecular , Nucleosídeos/química , Extratos Vegetais/química , Controle de Qualidade , Padrões de Referência , Riboflavina/química , Espectrometria de Massas em Tandem/normas
7.
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.

8.
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
9.
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
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 Chromatogr A ; 1584: 87-96, 2019 Jan 11.
Artigo em Inglês | MEDLINE | ID: mdl-30473109

RESUMO

Large-scale targeted and untargeted metabolites characterization can be achieved by feat of different liquid chromatography/mass spectrometry (LC-MS) platforms by multiple MS experiments or using data-independent acquisition followed by precursor-product ions matching based on certain algorithms. The resulting insufficiency in efficiency and availability greatly restricts the applicability of these strategies in large-scale profiling and identification of various metabolites. A strategy simultaneously enabling both the targeted and untargeted metabolites characterization is established on a Q Exactive hybrid quadrupole-Orbitrap mass spectrometer, by integrating precursor ions list-triggered data-dependent MS2 acquisition (PIL/dd-MS2) of the targeted components and using the "If idle-pick others" (IIPO) function to induce untargeted metabolites fragmentation. A compounds-specific mass defect filter (MDF) algorithm is proposed as a method to generate the PIL. As a proof of concept, this strategy coupled with offline two-dimensional liquid chromatography (2D-LC) was applied to identify the multicomponents of a traditional Chinese medicine formula Erzhi Pill (EZP). A rigid MDF vehicle was elaborated by orthogonal screening of the integer mass and integer mass-dependent dynamic mass defects considering a variation of 20 ppm. The Full MS/dd-MS2 method enabling PIL and IIPO exhibited better performance than Full MS/dd-MS2 and Targeted SIM/dd-MS2 (selected ion monitoring) in respect of the sensitivity in identifying the targeted components and the ability to characterize more untargeted ones. As a consequence, 270 components were separated from EZP, and 146 thereof were selectively characterized. In conclusion, it is a practical, multifaced strategy facilitating the in-depth metabolites profiling and characterization of complex herbal and biological samples.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/análise , Medicamentos de Ervas Chinesas/química , Espectrometria de Massas em Tandem/métodos
13.
Chin J Nat Med ; 16(10): 791-800, 2018 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-30322613

RESUMO

Shenshao Tablet (SST), prepared from Paeoniae Radix Alba (PRA) and total ginsenoside of Ginseng Stems and Leaves (GSL), is a traditional Chinese medicine (TCM) preparation prescribed to treat coronary heart disease. However, its chemical composition and the components that can migrate into blood potentially exerting the therapeutic effects have rarely been elucidated. We developed an HPLC/DAD/ESI-MSn approach aiming to comprehensively profile and identify both the chemical components of SST and its absorbed ingredients (and metabolites) in rat plasma and urine. Chromatographic separation was performed on an Agilent Eclipse XDB C18 column using acetonitrile/0.1% formic acid as the mobile phase. MS detection was conducted in both negative and positive ESI modes to yield more structure information. Comparison with reference compounds (tR, MSn), interpretation of the fragmentation pathways, and searching of in-house database, were utilized for more reliable structure elucidation. A total of 82 components, including 21 monoterpene glycosides, four galloyl glucoses, two phenols from PRA, and 55 ginsenosides from GSL, were identified or tentatively characterized from the 70% ethanolic extract of SST. Amongst them, seven and 24 prototype compounds could be detectable in the plasma and urine samples, respectively, after oral administration of an SST extract (4 g·kg-1) in rats. No metabolites were observed in the rat samples. The findings of this work first unveiled the chemical complexity of SST and its absorbed components, which would be beneficial to understanding the therapeutic basis and quality control of SST.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/farmacocinética , Espectrometria de Massas por Ionização por Electrospray/métodos , Animais , Masculino , Ratos , Ratos Sprague-Dawley , Comprimidos/química
14.
Phytomedicine ; 44: 85-86, 2018 05 15.
Artigo em Inglês | MEDLINE | ID: mdl-29895496
15.
Phytomedicine ; 44: 247-257, 2018 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-29631807

RESUMO

BACKGROUND: Due to a variety of factors to affect the herb quality, the existing quality management model is unable to evaluate the process control. The development of the concept of "quality marker" (Q-marker) lays basis for establishing an independent process quality control system for herbal products. HYPOTHESIS/PURPOSE: To ensure the highest degree of safety, effectiveness and quality process control of herbal products, it is aimed to establish a quality transitivity and traceability system of quality and process control from raw materials to finished herbal products. STUDY DESIGN: Based on the key issues and challenges of quality assessment, the current status of quality and process controls from raw materials to herbal medicinal products listed in Pharmacopoeia were analyzed and the research models including discovery and identification of Q-markers, analysis and quality management of risk evaluation were designed. METHODS: Authors introduced a few new technologies and methodologies, such as DNA barcoding, chromatographic technologies, fingerprint analysis, chemical markers, bio-responses, risk management and solution for quality process control. RESULTS: The quality and process control models for herbal medicinal products were proposed and the transitivity and traceability system from raw materials to the finished products was constructed to improve the herbal quality from the entire supply and production chain. CONCLUSION: The transitivity and traceability system has been established based on quality markers, especially on how to control the production process under Good Engineering Practices, as well as to implement the risk management for quality and process control in herbal medicine production.


Assuntos
Biomarcadores/análise , Medicina Herbária/normas , Controle de Qualidade , Código de Barras de DNA Taxonômico , Humanos , Medicina Tradicional Chinesa/normas , Fitoterapia/normas , Plantas Medicinais
16.
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
17.
Chin J Nat Med ; 16(2): 139-142, 2018 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-29455729

RESUMO

The present study was designed to determine the chemical constituents of the stem tuber of Pinellia pedatisecta. The chemical constituents were isolated and purified by various chromatographic techniques, and their structures were elucidated on the basis of physicochemical properties and spectral data. Three new alkaloids (compounds 1, 2, and 3) were obtained and identified as 9-((5-methoxypyridin-2-yl)methyl)-9H-purin-6-amine (1), 4-(2-(2, 5-dioxopyrrolidin-1-yl)ethyl)phenyl acetate (2), and N-(9-((5-methoxypyridin-2-yl)methyl)-9H-purin-6-yl)acetamide (3). These compounds were evaluated for their cytotoxicity against human cervical cancer HeLa cells. Compounds 1 and 3 significantly inhibited the proliferation of HeLa cells with IC50 values being 3.02 ± 0.54 and 7.16 ± 0.62 µmol·L-1, respectively.


Assuntos
Alcaloides/química , Pinellia/química , Extratos Vegetais/química , Alcaloides/isolamento & purificação , Alcaloides/farmacologia , Proliferação de Células/efeitos dos fármacos , Células HeLa , Humanos , Extratos Vegetais/isolamento & purificação , Extratos Vegetais/farmacologia , Caules de Planta/química , Tubérculos/química
18.
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
19.
J Chromatogr A ; 1538: 34-44, 2018 Feb 23.
Artigo em Inglês | MEDLINE | ID: mdl-29395157

RESUMO

Liquid chromatography-mass spectrometry (LC-MS) guided isolation is a favored strategy to quickly and efficiently explore the chemical diversity of herbal medicines. In this study, two methods were adopted to improve the performance of the strategy, including offline two-dimensional (2D) LC to extend the peak capacities and predicted metabolites screening (PMS) to automatically screen the targets with expanded databases. Ginsenosides in the leaves of Panax notoginseng (PNL) were taken as a case. An offline 2D LC system was constructed with an orthogonality of 0.69 and peak capacity of 8925. Quadrupole time-of-flight mass spectrometry-fast data directed analysis (QTOF-Fast DDA) was employed for detection of the ginsenosides in the fractioned samples. Four modified groups, including glucose, xylose, rhamnose and malonyl, were adopted and markedly extended the screening coverage. The combined strategy showed about 7.5 times improvement in the screening capability. PMS is conveniently and automatically implemented in UNIFI. Using this strategy, 945 ginsenosides were discovered from PNL, including 662 potentially novel ginsenosides. Furthermore, two new ginsenosides were purified, and unambiguously identified by NMR analysis, partially demonstrating the LC-MS guided isolation. The combined strategy can also be applied in characterizing and discovering new bioactive constituents from other herbal medicines.


Assuntos
Ginsenosídeos/química , Medicina Herbária/métodos , Panax notoginseng/química , Folhas de Planta/química , Cromatografia Líquida , Ginsenosídeos/análise , Espectroscopia de Ressonância Magnética , Plantas Medicinais/química , Espectrometria de Massas em Tandem
20.
J Sep Sci ; 41(8): 1888-1895, 2018 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-29333638

RESUMO

Phenolic acids are the major water-soluble components in Salvia miltiorrhiza (>5%). According to previous studies, many of them contribute to the cardiovascular effects and antioxidant effects of S. miltiorrhiza. Polymeric phenolic acids can be considered as the tanshinol derived metabolites, e.g., dimmers, trimers, and tetramers. A strategy combined with tanshinol-based expected compounds prediction, total ion chromatogram filtering, fragment ion searching, and parent list-based multistage mass spectrometry acquisition by linear trap quadropole-orbitrap Velos mass spectrometry was proposed to rapid profile polymeric phenolic acids in S. miltiorrhiza. More than 480 potential polymeric phenolic acids could be screened out by this strategy. Based on the fragment information obtained by parent list-activated data dependent multistage mass spectrometry acquisition, 190 polymeric phenolic acids were characterized by comparing their mass information with literature data, and 18 of them were firstly detected from S. miltiorrhiza. Seven potential compounds were tentatively characterized as new polymeric phenolic acids from S. miltiorrhiza. This strategy facilitates identification of polymeric phenolic acids in complex matrix with both selectivity and sensitivity, which could be expanded for rapid discovery and identification of compounds from complex matrix.


Assuntos
Hidroxibenzoatos/análise , Polímeros/análise , Salvia miltiorrhiza/química , Íons/análise , Espectrometria de Massas
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