RESUMO
RATIONALE: The volatile organic compounds (VOCs) of Lonicerae Japonicae flos (LJF) and Lonicera flos (LF) play a pivotal role in determining their sensory characteristics, medicinal properties, and subsequent impact on market pricing and consumer preferences. However, the differences and specificity of these VOCs remain obscure. Hence, it is crucial to conduct a comprehensive characterization of the VOCs in LJF and LF and pinpoint their potential differential VOCs. METHODS: In this study, headspace gas chromatography-ion mobility spectrometry (HS-GC/IMS) and headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC/MS) were employed to comprehensively investigate the compositional characteristics and distinctions in VOCs between LJF and LF. Multivariate statistical analysis was used to identify candidate differential VOCs of LJF and LF samples. RESULTS: A total of 54 and 88 VOCs were identified using HS-GC/IMS and HS-SPME-GC/MS analysis, respectively. Primary VOCs detected in LJF include leaf alcohol, (E)-2-hexen-1-ol dimer, 2-octyn-1-ol, and (E)-3-hexen-1-ol. Key VOCs prevalent in LF encompass farnesol, heptanoic acid, octanoic acid, and valeric acid. Multivariate statistical analysis indicates that compounds such as phenethyl alcohol and leaf alcohol were selected as potential VOCs for distinguishing between LJF and LF. CONCLUSION: This research conducted a comprehensive analysis of the fundamental volatile components in both LJF and LF. It subsequently elucidated the distinctions and specificities within their respective VOC profiles. And this study enables differentiation between LJF and LF through the analysis of VOCs, offering valuable insights for enhancing the quality control of both LJF and LF.
Assuntos
Lonicera , Extratos Vegetais , Compostos Orgânicos Voláteis , Cromatografia Gasosa-Espectrometria de Massas/métodos , Compostos Orgânicos Voláteis/análise , Microextração em Fase Sólida/métodos , Espectrometria de Mobilidade Iônica , EtanolRESUMO
Andrographis paniculata is a medicinal plant traditionally used to produce diterpene lactones and flavonoids, which possess various biological activities. Widely distributed in China, India, and other Southeast Asia countries, A. paniculata has become an important economic crop, significantly treating SARS-CoV-2, and is being cultivated on a large scale in southern China. The biosynthesis of active ingredients in A. paniculata are regulated and controlled by genes, but their specific roles are still not fully understood. To further explore the growth regulation factors and utilization of its medicinal parts of this industrial crop, chemical and transcriptome analyses were conducted on the roots, stems, and leaves of A. paniculata to identify the biosynthesis pathways and related candidate genes of the active ingredients. The chemical analysis revealed that the main components of A. paniculata were diterpene lactones and flavonoids, which displayed potential ability to treat SARS-CoV-2 through molecular docking. Moreover, the transcriptome sequencing annotated a total of 40,850 unigenes, including 7962 differentially expressed genes. Among these, 120 genes were involved in diterpene lactone biosynthesis and 60 genes were involved in flavonoid biosynthesis. The expression of diterpene lactone-related genes was the highest in leaves and the lowest in roots, consistent with our content determination results. It is speculated that these highly expressed genes in leaves may be involved in the biosynthesis pathway of diterpenes. Furthermore, two class â terpene synthases in A. paniculata transcriptome were also annotated, providing reference for the downstream pathway of the diterpene lactone biosynthesis. With their excellent market value, our experiments will promote the study of the biosynthetic genes for active ingredients in A. paniculata and provide insights for subsequent in vitro biosynthesis.
Assuntos
Andrographis , Diterpenos , Terpenos/metabolismo , Transcriptoma , Andrographis/genética , Andrographis/química , Flavonoides/metabolismo , Simulação de Acoplamento Molecular , Diterpenos/química , Lactonas/metabolismo , Antivirais/metabolismoRESUMO
The flower buds of three Panax species (PGF: P. ginseng; PQF: P. quinquefolius; PNF: P. notoginseng) widely consumed as health tea are easily confused in market circulation. We aimed to develop a green, fast, and easy analysis strategy to distinguish PGF, PQF, and PNF. In this work, fast gas chromatography electronic nose (fast GC e-nose), headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS), and headspace solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) were utilized to comprehensively analyze the volatile organic components (VOCs) of three flowers. Meanwhile, a principal component analysis (PCA) and heatmap were applied to distinguish the VOCs identified in PGF, PQF, and PNF. A random forest (RF) analysis was used to screen key factors affecting the discrimination. As a result, 39, 68, and 78 VOCs were identified in three flowers using fast GC e-nose, HS-GC-IMS, and HS-SPME-GC-MS. Nine VOCs were selected as potential chemical markers based on a model of RF for distinguishing these three species. Conclusively, a complete VOC analysis strategy was created to provide a methodological reference for the rapid, simple, and environmentally friendly detection and identification of food products (tea, oil, honey, etc.) and herbs with flavor characteristics and to provide a basis for further specification of their quality and base sources.
Assuntos
Panax , Compostos Orgânicos Voláteis , Cromatografia Gasosa-Espectrometria de Massas/métodos , Nariz Eletrônico , Microextração em Fase Sólida/métodos , Panax/química , Espectrometria de Mobilidade Iônica , Compostos Orgânicos Voláteis/análise , Flores/química , CháRESUMO
RATIONALE: Shuang-Huang-Lian powder injection (SHLPI) is a well-known modern traditional Chinese medicine formula preparation (TCMFP) widely used to treat acute upper respiratory infections. However, SHLPI is extracted from pure Chinese medicine and administered through an injection, and many adverse reactions have been reported clinically. Therefore, it is necessary to characterize in depth the chemical composition of SHLPI and quantitatively analyze its potential allergenic components. METHODS: In this study, the samples were analyzed using ion mobility ultra-high-performance liquid chromatography-quadrupole time-of-flight-mass spectrometry (UHPLC-QTOF-MS) combined with a self-built database. Furthermore, the parallel reaction monitoring (PRM) model of ultra-high-performance liquid chromatography-quadrupole-Orbitrap-mass spectrometry (UHPLC-Q-Orbitrap-MS) was used to successfully quantify 10 representative bioactive components. RESULTS: Using this strategy 90 compounds were identified, the fragmentation pathways of five representative compounds in the five main components of SHLPI were summarized, and 10 components (neochlorogenic acid, chlorogenic acid, sweroside, forsythiaside A, luteoloside, isochlorogenic acid B, isochlorogenic acid C, baicalin, phillyrin, and baicalein) were determine as the quality markers of SHLPI based on UPLC-Q-Orbitrap-MS. CONCLUSIONS: This work comprehensively characterized the material basis of SHLPI, summarized the cracking laws of representative substances, and quantitatively analyzed 10 potential allergenic components. Therefore, this study could provide a basis for the quality control of SHLPI and the clinical rational use of drugs to reduce its adverse reactions.
Assuntos
Medicamentos de Ervas Chinesas , Cromatografia Líquida de Alta Pressão/métodos , Pós , Medicamentos de Ervas Chinesas/química , Espectrometria de MassasRESUMO
RATIONALE: Many methods have been reported for the production of rare ginsenosides, including heat treatment, acid hydrolysis, alkaline hydrolysis, enzymatic hydrolysis, and microbial transformation. However, the conversion of original ginsenosides to rare ginsenosides under the dual conditions of citric acid and high-pressure steam sterilization has rarely been reported. METHODS: In this study, a method involving ultrahigh-performance liquid chromatography coupled to ion mobility quadrupole time-of-flight mass spectrometry was developed for analysis of chemical transformation of protopanaxatriol (PPT)-type ginsenosides Rg1 and Re, protopanaxadiol (PPD)-type ginsenoside Rb1 , and total ginsenosides in the dual conditions of citric acid and high-pressure steam sterilization. An internal ginsenoside database containing 126 known ginsenosides and 18 ginsenoside reference compounds was established to identify the transformation products and explore possible transformation pathways and mechanisms. RESULTS: A total of 54 ginsenosides have been preliminarily identified in the transformation products of PPD-type ginsenosides Rg1 and Re, PPD-type ginsenoside Rb1 , and total ginsenosides, and the possible transformation pathways were as follows: Rg1 , Re â 20(S)-Rh12 , 20(R)-Rh12 ; Rg1 , Re â 20(S)-Rh1 , 20(R)-Rh1 â Rk3 , Rh4 , Rh5 ; Rb1 â gypenoside LXXV; Rb1 â 20(S)-Rg3 , 20(R)-Rg3 â Rk1 , Rg5 ; Re â 20(S)-Rg2 , 20(R)-Rg2 â 20(S)-Rf2 , 20(R)-Rf2 , Rg4 , F4 . CONCLUSIONS: The results elucidated the possible transformation pathways and mechanisms of ginsenosides in the dual conditions of citric acid and high-pressure steam sterilization, which were helpful for revealing the mechanisms of ginsenosides and enhanced safety and quality control of pharmaceuticals and nutraceuticals. Meanwhile, a simple, efficient, and practical method was developed for the production of rare ginsenosides, which has the potential to produce diverse rare ginsenosides on an industrial scale.
Assuntos
Ginsenosídeos , Panax , Cromatografia Líquida , Ácido Cítrico , Ginsenosídeos/química , Espectrometria de Massas , Panax/química , Saponinas , Vapor/análise , TriterpenosRESUMO
Ganoderma sinense, with more than 2000 years of medicinal history, is a fungus of the basidiomycetes that is rich in polysaccharides and terpenoids. However, the biosynthesis of terpenes, especially sesquiterpenes, has been little studied. The functional identification of sesquiterpene synthases from G. sinense is of great significance to the study of fungal terpenoid biosynthesis and regulation. Our research group has completed the functional characterization of 21 sesquiterpene synthase genes from G. sinense. It was found that gleenol, biosynthesis of which is catalyzed by the sesquiterpene synthase GsSTS26 and GsSTS27, has the functions of killing termites, antihelminth, and plant growth regulation. In the unmodified E. coli Rosetta (DE3) strain, the content of gleenol produced by sesquiterpene synthase from G. sinense is low, which makes it difficult to meet the demand of industrial production and the market. Therefore, it is of great significance to obtain high-yielding strains by means of synthetic biology. In this study, we constructed eight recombinant strains by using tandem gene expression and promoter engineering, and the content of gleenol was increased by up to 23-fold. In this study, we realized the de novo synthesis of gleenol in E. coli and provided a basis for the biosynthesis of terpenoids in basidiomycetes. KEY POINTS: ⢠Eight recombinant expression systems were constructed by using tandem genes and promoter engineering. ⢠The recombinant strain promoted the efficient production of gleenol in E. coli Rosetta (DE3). ⢠The recombinant strain achieved de novo production of gleenol in E. coli.
Assuntos
Alquil e Aril Transferases , Sesquiterpenos , Escherichia coli/genética , Escherichia coli/metabolismo , Sesquiterpenos/metabolismo , Terpenos/metabolismo , Alquil e Aril Transferases/metabolismoRESUMO
Volatile organic compounds (VOCs) are the main chemical components of Schizonepetae Spica (SS), which have positive effects on the quality evaluation of SS. In this study, HS-SPME-GC-MS (headspace solid-phase microextraction-gas chromatography-mass spectrometry) and HS-GC-IMS (headspace-gas chromatography-ion mobility spectrometry) were performed to characterize the VOCs of SS from six different regions. A total of 82 VOCs were identified. In addition, this work compared the suitability of two instruments to distinguish SS from different habitats. The regional classification using orthogonal partial least squares discriminant analysis (OPLS-DA) shows that the HS-GC-IMS method can classify samples better than the HS-SPME-GC-MS. This study provided a reference method for identification of the SS from different origins.
Assuntos
Microextração em Fase Sólida , Compostos Orgânicos Voláteis , Cromatografia Gasosa-Espectrometria de Massas/métodos , Espectrometria de Mobilidade Iônica , Análise dos Mínimos Quadrados , Microextração em Fase Sólida/métodos , Compostos Orgânicos Voláteis/análiseRESUMO
RATIONALE: Kaixin San (KXS) is a prescription traditional Chinese medicine (TCM) with the effects of "tonifying the kidney and brain" and "improving memory". The volatile organic compounds (VOCs) in KXS could effectively improve senile dementia and depression, but only few studies have focused on the overall characterization of VOCs in KXS and the quantitative study of the main active components. METHODS: We have developed a strategy to correlate the results from headspace gas chromatography/ion mobility spectrometry (HS-GC/IMS) and headspace gas chromatography/mass spectrometry (HS-GC/MS) for the comprehensive characterization of VOCs in KXS and the quantitative analysis of the main pharmacodynamic substances. RESULTS: A totsal of 68 low molecular weight VOCs were identified in KXS by HS-GC/IMS at room temperature and atmospheric pressure; 117 VOCs were identified and 10 components (isocalamenediol, α-asarone, ß-asarone, methyl eugenol, isoeugenol methyl ether, camphor, anethol, 2,4-di-tert-butylphol, linalool, asarylaldehyde) as the quality markers of KXS based on HS-GC/MS. CONCLUSIONS: This results from this study provide a foundation for quality control, pharmacodynamic mechanism research and further development of KXS, and provides more convincing data supporting the VOCs of other natural products.
Assuntos
Medicamentos de Ervas Chinesas/química , Cromatografia Gasosa-Espectrometria de Massas/métodos , Espectrometria de Mobilidade Iônica/métodos , Compostos Orgânicos Voláteis/análise , Controle de QualidadeRESUMO
Cissampelos is a significant genus comprising of approximately 21 species of the medicinal plants (Menispermaceae). The plants of this genus are used in traditional medicine for the treatment of various ailments such as asthma, arthritis, dysentery, hyperglycemia, cardiopathy, hypertension and other related problems. These plants are rich in bioactive dibenzylisoquinoline and aborphine as well as small amounts of other ingredients. In recent years, the chemical constituents and pharmacological activities of Cissampelos genus have been paid more and more attention due to their diversity. Herein, we compile the chemical constituents and biological activities on this genus, and summarize the 13 C-NMR data of the main bioactive ingredients. All information comes from scientific databases such as Google Scholar, PubMed, Sci-Finder, ScienceDirect, Web of Science and CNKI. It provides valuable data for the future research and development of Cissampelos genus.
Assuntos
Cissampelos/química , Compostos Fitoquímicos/uso terapêutico , Artrite/tratamento farmacológico , Asma/tratamento farmacológico , Disenteria/tratamento farmacológico , Cardiopatias/tratamento farmacológico , Humanos , Hiperglicemia/tratamento farmacológico , Hipertensão/tratamento farmacológico , Estrutura Molecular , Compostos Fitoquímicos/química , Compostos Fitoquímicos/isolamento & purificaçãoRESUMO
Trimethylamine N-oxide (TMAO), as a gut-derived metabolite, has been found to be associated with enhanced risk for atherosclerosis and cardiovascular disease. We presented a method for targeted profiling of TMAO and betaine in serum and food samples based on a combination of one-step sample pretreatment and proton nuclear magnetic resonance spectroscopy. The key step included a processing of sample preparation using a selective solid-phase extraction column for retention of basic metabolites. Proton signals at δ 3.29 and δ 3.28 were employed to quantify TMAO and betaine, respectively. The developed method was examined with acceptable linear relationship, precision, stability, repeatability, and accuracy. It was successfully applied to detect serum levels of TMAO and betaine in TMAO-fed mice and high-fructose-fed rats and also used to determine the contents of TMAO and betaine in several kinds of food, such as fish, pork, milk, and egg yolk.
Assuntos
Betaína/análise , Análise de Alimentos/métodos , Metabolômica/métodos , Metilaminas/análise , Óxidos/química , Animais , Betaína/sangue , Betaína/metabolismo , Feminino , Masculino , Metilaminas/sangue , Metilaminas/metabolismo , Camundongos , Camundongos Endogâmicos C57BL , Ratos , Ratos WistarRESUMO
Peiyuan Tongnao capsule (PTC) is a prescription medicine of traditional Chinese medicine with the effects of "nourishing the kidney," "replenishing essence," "extinguishing wind," and "opening the meridian". PTC is also widely used in clinic for the treatment of stroke and chronic cerebral circulation insufficiency. However, the quality control studies of PTC are hitherto quite limited. Here, we aim to fully utilize an advanced chromatography-mass spectrometry hyphenation technique to qualitatively and quantitatively evaluate the quality of PTC. Firstly, a two-dimensional liquid chromatography/quadrupole-Orbitrap mass spectrometry (2D-LC/Q-Orbitrap-MS) approach was established for multicomponent characterization. An offline 2D-LC system fitted with an Xbridge Amide column and an HSS T3 column showed an orthogonality of 0.63 and a theoretical peak capacity of 6930. Eleven fractions of PTC, after hydrophilic interaction chromatography (first dimension), were further analyzed by reversed-phase ultrahigh-performance liquid chromatography/Q-Orbitrap-MS (UHPLC/Q-Orbitrap-MS, second dimension) using a rapid negative/positive switching mode. Consequently, 178 compounds were separated, 96 of which were identified or tentatively characterized. Secondly, co-condition fingerprint analysis of seven constituted herbal medicines of PTC was performed to unveil ten active ingredients (citric acid, rehmannioside D, echinacoside, paeoniflorin, verbascoside, liquiritin, 2,3,5,4'-tetrahydroxystilbene-2-O-ß-D-glucoside, cinnamic aldehyde, glycyrrhizic acid, and emodin) as the quality markers of PTC. Thirdly, a UHPLC/PRMad (adjusted parallel reaction monitoring) method was established and validated to quantify the ten marker compounds in 14 batches of PTC. To the best of our knowledge, this is the first study to report comprehensive multicomponent characterization, authentication, and quality evaluation of PTC, which could be used to lay the foundation for quality control, biological efficacy research, and further development. Graphical abstract.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Medicina Tradicional Chinesa , Espectrometria de Massas por Ionização por Electrospray/métodos , Biomarcadores/análise , Medicamentos de Ervas Chinesas/química , Controle de Qualidade , Reprodutibilidade dos TestesRESUMO
A phytochemical study on the seeds of Cassia obtusifolia was carried out, which finally led to obtain two naphthalenes (1 and 2), two naphthopyrans (3 and 4) and twelve anthraquinones (5-16). The structures of all compounds were established mainly by NMR and MS experiments as well as the necessary chemical evidence. Among them, 1 and 2 (obtusinaphthalensides A and B) were identified to be new naphthalene glycosides.
Assuntos
Cassia/química , Naftalenos/isolamento & purificação , Sementes/química , Antraquinonas/química , Hidrólise , Espectroscopia de Ressonância Magnética , Espectrometria de Massas , Estrutura Molecular , Extratos Vegetais/químicaRESUMO
Chinese medical preparation has complicated chemical constituents. Consequently, the proper quality control methods for these Chinese medical preparations have been great challenges to the traditional Chinese medicine modernization and internationalization. What components should be chosen for quality control is a big challenge in the development of traditional Chinese medicine. A new concept of "Quality Marker" was proposed by Liu et al. to solve this problem and established a new research paradigm for traditional Chinese medicine quality study. Several strategies were proposed by the researchers in traditional Chinese medicine, here, we used Shengmai injection as an example to discuss a strategy for selecting "Quality Markers" of Chinese medical preparation by the components transfer process analysis in the Shengmai injection manufacturing process. Firstly, a total of 87 compounds were identified or partially characterized in shengmai injection. Secondly, referenced to the quality control method in China pharmacopeia and considered the biomarkers in the original medicines and representative components in the manufacturing process, four ginsenosides in Panax ginseng (Hongshen), two compounds in Schisandra chinensis (Wuweizi), and a sugar from Ophiopogon japonicas (Maidong) were quantified. As a result, these seven representative compounds exhibited an acceptable transitivity throughout the Shengmai injection manufacturing process. Finally, combined with the active ingredients, components transfer process analysis, and comprehensive evaluation by "Spider-web" analysis, six compounds were selected as the quality markers for the quality control of Shengmai injection. Through this strategy of optimization for quality markers of Shengmai injection, we found that these six compounds could represent the main bioactive substances and be easily detected in the whole process of production. Furthermore, the quality control method was developed for quality assessment and control of these six quality markers in the Shengmai injection. The total content range of the selected quality markers in the 10 batches of the Shengmai injection is 13.844-22.557 mg/mL.
Assuntos
Medicina Tradicional Chinesa/métodos , Cromatografia Líquida de Alta Pressão , Combinação de Medicamentos , Medicamentos de Ervas Chinesas/química , Panax/química , Controle de Qualidade , Schisandra/químicaRESUMO
Russula vinosa Lindbl is a wild edible mushroom that is usually used for original material of food and soup and has rich nutritional value. What are the nutritional ingredients? In order to answer this question, we investigated the chemical constituents of this wild functional food. Six new compounds (1-6), together with nine known ones (7-15), were isolated from R. vinosa. The six new compounds were named as vinosane (1), rulepidadione C (2), (24E)-3,4-seco-cucurbita-4,24-diene-26,29-dioic acid-3-methyl ester (3), (24E)-3,4-seco-cucurbita-4,24-diene-26-oic acid-3-ethyl ester (4), (24E)-3ß-hydroxycucurbita-5,24-diene-26,29-dioic acid (5), and (2S,3S,4R,2'R)-2-(2'-hydroxydocosanoylamino)eicosane-1,3,4-triol (6). Their structures were determined based on spectroscopic methods including HR-ESI-MS, 1D, and 2D NMR. Moreover, a cell counting kit-8 (CCK-8 kit) was used to screen for the cytotoxicity of compounds 1-5 and 7-13 on mouse macrophage RAW 264.7 cells. The results showed that compounds 1-5 and 7-13 had no obvious cytotoxicity. In addition, the inhibitory effects on nitric oxide (NO) production in lipopolysaccharide (LPS)-activated mouse macrophage RAW 264.7 cells were evaluated. Compounds 1, 3, 4, 7, 12, and 13 showed moderate inhibitory activity on NO production.
Assuntos
Agaricales/química , Produtos Biológicos/química , Produtos Biológicos/farmacologia , Óxido Nítrico/biossíntese , Nutrientes/química , Animais , Produtos Biológicos/isolamento & purificação , Cromatografia Líquida de Alta Pressão , Camundongos , Estrutura Molecular , Nutrientes/isolamento & purificação , Células RAW 264.7 , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz , Análise EspectralRESUMO
The flower buds of three Panax species (PGF: flower bud of P. ginseng; PQF: flower bud of P. quinquefolius; PNF: flower bud of P. notoginseng), widely consumed as healthcare products, are easily confused particularly in the extracts or traditional Chinese medicine (TCM) formulae. We are aimed to develop an untargeted metabolomics approach, by ultra-high performance liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry (UHPLC/IM-QTOF-MS) to unveil the chemical markers diagnostic for the differentiation of PGF, PQF, and PNF. Key parameters affecting chromatographic separation and MS detection were optimized in sequence. Forty-two batches of flower bud samples were analyzed in negative high-definition MSE (HDMSE; enabling three-dimensional separations). Efficient metabolomics data processing was performed by Progenesis QI (Waters, Milford, MA, USA), while pattern-recognition chemometrics was applied for species classification and potential markers discovery. Reference compounds comparison, analysis of both HDMSE and targeted MS/MS data, and retrieval of an in-house ginsenoside library, were simultaneously utilized for the identification of discovered potential markers. Satisfactory conditions for metabolite profiling were achieved on a BEH Shield RP18 column and Vion™ IMS-QTOF instrument (Waters; by setting the capillary voltage of 1.0 kV and the cone of voltage 20 V) within 37 min. A total of 32 components were identified as the potential markers, of which Rb3, Ra1, isomer of m-Rc/m-Rb2/m-Rb3, isomer of Ra1/Ra2, Rb1, and isomer of Ra3, were the most important for differentiating among PGF, PQF, and PNF. Conclusively, UHPLC/IM-QTOF-MS-based metabolomics is a powerful tool for the authentication of TCM at the metabolome level.
Assuntos
Cromatografia Líquida de Alta Pressão , Flores/química , Metaboloma , Metabolômica , Panax/química , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz , Metabolômica/métodos , Estrutura MolecularRESUMO
The complexity of herbal matrix necessitates the development of powerful analytical strategies to enable comprehensive multicomponent characterization. In this work, targeting the multicomponents from Panax japonicus C.A. Meyer, both data dependent acquisition (DDA) and data-independent high-definition MSE (HDMSE) in the negative electrospray ionization mode were used to extend the coverage of untargeted metabolites characterization by ultra-high-performance liquid chromatography (UHPLC) coupled to a VionTM IM-QTOF (ion-mobility/quadrupole time-of-flight) high-resolution mass spectrometer. Efficient chromatographic separation was achieved by using a BEH Shield RP18 column. Optimized mass-dependent ramp collision energy of DDA enabled more balanced MS/MS fragmentation for mono- to penta-glycosidic ginsenosides. An in-house ginsenoside database containing 504 known ginsenosides and 60 reference compounds was established and incorporated into UNIFITM, by which efficient and automated peak annotation was accomplished. By streamlined data processing workflows, we could identify or tentatively characterize 178 saponins from P. japonicus, of which 75 may have not been isolated from the Panax genus. Amongst them, 168 ginsenosides were characterized based on the DDA data, while 10 ones were newly identified from the HDMSE data, which indicated their complementary role. Conclusively, the in-depth deconvolution and characterization of multicomponents from P. japonicus were achieved, and the approaches we developed can be an example for comprehensive chemical basis elucidation of traditional Chinese medicine (TCM).
Assuntos
Cromatografia Líquida de Alta Pressão , Mineração de Dados , Metaboloma , Metabolômica , Panax/química , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz , Cromatografia Líquida de Alta Pressão/métodos , Mineração de Dados/métodos , Metabolômica/métodos , Estrutura Molecular , Panax/metabolismo , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz/métodos , Fluxo de TrabalhoRESUMO
An on-line large volume sample stacking with polarity switching (LVSS) method was proposed for simultaneously determining lignanoids and ginsenosides in MEEKC. The parameters including the pH value and concentration of buffer solution, SDS, organic modifier, oil phase, running voltage, and temperature as well as injection time, sample matrix, stacking voltage, and time influencing separation and stacking were systematically optimized. The method was verified by performing precision, accuracy, stability, and recovery. Its reliability was proved by separating and quantifying two lignanoids and three ginsenosides in Shengmai injectionSMI. The sensitivity of these compounds was improved by MEEKC-LVSS method for 6-11 times than conventional MEEKC. Thus, this developed on-line MEEKC-LVSS method was sensitive, practical, and reliable.
Assuntos
Cromatografia Capilar Eletrocinética Micelar/métodos , Ginsenosídeos/análise , Lignanas/análise , Emulsões/química , Ginsenosídeos/química , Ginsenosídeos/isolamento & purificação , Lignanas/química , Lignanas/isolamento & purificação , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos TestesRESUMO
A continuous phytochemical study on the roots of Marsdenia tenacissima led to the isolation and identification of 13 new polyoxypregnane glycosides named marstenacissides B10-B17 (1, 2, 4, 7, 8, 11, 12, and 14) and marstenacissides A8-A12 (3, 9, 10, 13, and 15) in addition to two known polyoxypregnane glycosides marsdenosides M and L (5 and 6). Their structures were established by spectroscopic techniques and by comparison with the reported data in the literature. Moreover, the anti-HIV activities of these isolates and the previous isolated marstenacissides A1-A7 and B1-B9 were assessed, some of which exhibited slight or negligible effects against HIV-1.
Assuntos
Fármacos Anti-HIV/farmacologia , Medicamentos de Ervas Chinesas/química , Infecções por HIV/tratamento farmacológico , HIV-1/efeitos dos fármacos , Marsdenia/química , Saponinas/farmacologia , Fármacos Anti-HIV/química , Fármacos Anti-HIV/isolamento & purificação , Infecções por HIV/virologia , Medicina Tradicional Chinesa , Estrutura Molecular , Ressonância Magnética Nuclear Biomolecular , Raízes de Plantas/química , Caules de Planta/química , Saponinas/química , Saponinas/isolamento & purificaçãoRESUMO
Lutein (L) and zeaxanthin (Z) are dietary carotenoids derived from dark green leafy vegetables, orange and yellow fruits that form the macular pigment of the human eyes. It was hypothesized that they protect against visual disorders and cognition diseases, such as age-related macular degeneration (AMD), age-related cataract (ARC), cognition diseases, ischemic/hypoxia induced retinopathy, light damage of the retina, retinitis pigmentosa, retinal detachment, uveitis and diabetic retinopathy. The mechanism by which they are involved in the prevention of eye diseases may be due their physical blue light filtration properties and local antioxidant activity. In addition to their protective roles against light-induced oxidative damage, there are increasing evidences that L and Z may also improve normal ocular function by enhancing contrast sensitivity and by reducing glare disability. Surveys about L and Z supplementation have indicated that moderate intakes of L and Z are associated with decreased AMD risk and less visual impairment. Furthermore, this review discusses the appropriate consumption quantities, the consumption safety of L, side effects and future research directions.
Assuntos
Transtornos Cognitivos/prevenção & controle , Luteína/farmacologia , Transtornos da Visão/prevenção & controle , Zeaxantinas/farmacologia , Fatores Etários , Animais , Cognição/efeitos dos fármacos , Transtornos Cognitivos/diagnóstico , Transtornos Cognitivos/etiologia , Transtornos Cognitivos/metabolismo , Suplementos Nutricionais , Humanos , Luteína/administração & dosagem , Luteína/química , Degeneração Macular/diagnóstico , Degeneração Macular/etiologia , Degeneração Macular/metabolismo , Degeneração Macular/prevenção & controle , Estrutura Molecular , Transtornos da Visão/diagnóstico , Transtornos da Visão/etiologia , Transtornos da Visão/metabolismo , Zeaxantinas/administração & dosagem , Zeaxantinas/químicaRESUMO
The manufacture of traditional Chinese medicine (TCM) products is always accompanied by processing complex raw materials and real-time monitoring of the manufacturing process. In this study, we investigated different modeling strategies for the extraction process of licorice. Near-infrared spectra associate with the extraction time was used to detemine the states of the extraction processes. Three modeling approaches, i.e., principal component analysis (PCA), partial least squares regression (PLSR) and parallel factor analysis-PLSR (PARAFAC-PLSR), were adopted for the prediction of the real-time status of the process. The overall results indicated that PCA, PLSR and PARAFAC-PLSR can effectively detect the errors in the extraction procedure and predict the process trajectories, which has important significance for the monitoring and controlling of the extraction processes.