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1.
Zhongguo Zhong Yao Za Zhi ; 46(18): 4841-4848, 2021 Sep.
Artigo em Chinês | MEDLINE | ID: mdl-34581096

RESUMO

Longxue Tongluo Capsules(LTC) has good efficacy against blood stasis syndrome during the recovery period of ischemic stroke. Its main active ingredient is the phenolic extract of Chinese dragon's blood. In our previous study, the primary mass fragmentation pathways of phenolic derivatives from LTC were clarified. Herein, the metabolites in rat plasma were characterized following the oral administration of loureirin A and loureirin C using liquid chromatography coupled with hybrid ion trap/time-of-flight mass spectro-metry(LC-IT-TOF-MS), with 18 and 55 metabolites identified, respectively. On this basis, with the help of the obtained accurate molecular weight, characteristic fragment ions, reference comparison, combined with LTC database and natural products database self-created in our group, 18 prototypes and 106 metabolites were tentatively identified in rat plasma after oral gavage of LTC at a dose of 500 mg·kg~(-1). Glucuronidation, sulfonation, and methylation were major biotransformation pathways of LTC. This study preliminarily clarified the LTC constituents absorbed into blood and laid the foundation for clarifying the effective substances of LTC.


Assuntos
Medicamentos de Ervas Chinesas , Administração Oral , Animais , Cápsulas , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , Cromatografia Gasosa-Espectrometria de Massas , Ratos
2.
Zhongguo Zhong Yao Za Zhi ; 46(16): 4131-4138, 2021 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-34467724

RESUMO

Eleven condensed tannins were isolated from the roots of Indigofera stachyodes by various column chromatography techniques including silica gel, octadecyl silica(ODS), Sephadex LH-20, and semi-preparative high performance liquid chromatography(HPLC). These compounds were identified on the basis of physicochemical properties, nuclear magnetic resonance(NMR) and mass spectrometry(MS) data as stachyotannin A(1), epicatechin-(2ß→O→7,4ß→8)-epiafzelechin-(4ß→8)-catechin(2), cinnamtannin D1(3), cinnamtannin B1(4), epicatechin-(2ß→O→7,4ß→8)-epiafzelechin-(4α→8)-epicatechin(5), gambiriin C(6), proanthocyanidin A1(7), proanthocyanidin A2(8), aesculitannin B(9), proanthocyanidin A4(10), and procyanidin B5(11). Compound 1 is a new compound. Compounds 2-11 were isolated from Indigofera for the first time. Furthermore, compounds 1, 2, and 4-11 showed inhibitory effects on thrombin-induced ATP release in platelets.


Assuntos
Indigofera , Proantocianidinas , Cromatografia Líquida de Alta Pressão , Espectroscopia de Ressonância Magnética , Extratos Vegetais
3.
Zhongguo Zhong Yao Za Zhi ; 46(16): 4150-4156, 2021 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-34467727

RESUMO

The current study aims to rapidly and comprehensively profile the chemical composition of Cistanche salsa using direct infusion coupled with MS/MS~(ALL)(DI-MS/MS~(ALL)). The C. salsa extract was directly imported into electrospray ionization(ESI) source of quadrupole time-of-flight(Q-TOF) mass spectrometer with an infusion pump at a flow rate of 10 µL·min~(-1). Acquisition program was applied under negative ionization polarity to collect one MS~1 spectrum(m/z 50-1 200), followed by 1 150 MS~2 spectra with precursor isolation window(m/z 1) amongst mass range m/z 50-1 200. After each MS~2 spectrum was matched to its precursor ion, putative identification was conducted through matching mass spectral data with literature and database. A total of 31 components were identified from C. salsa, including 9 phenylethanoid glycosides, 2 iridoids, 4 saccharides, 9 organic acids, and 7 other compounds, similar to those from C. tubulosa and C. deserticola. In conclusion, DI-MS/MS~(ALL), a facile and reliable analytical tool, can be employed for qualitative analysis of chemical constituents in C. salsa. The research offers a promising strategy to achieve rapid chemome profiling of herbal medicine and provides an alternative source of Cistanches Herba.


Assuntos
Cistanche , Medicamentos de Ervas Chinesas , Plantas Medicinais , Cromatografia Líquida de Alta Pressão , Glicosídeos , Espectrometria de Massas em Tandem
4.
Zhongguo Zhong Yao Za Zhi ; 46(14): 3599-3604, 2021 Jul.
Artigo em Chinês | MEDLINE | ID: mdl-34402283

RESUMO

Isomers are widely distributed in Chinese herbal medicines,and can be discriminated by energy-resolved mass spectrometry( ER-MS). However,ER-MS was performed through direct injection of reference compounds with syringe pump,which encountered a significant technical barrier for high-throughput and automated measurements. Herein,online ER-MS was conducted using LC-MS platform,and a pair of isomers,kaempferol vs luteolin,were employed as a case study to illustrate and assess the utility of online ER-MS for isomeric discrimination. High-resolution tandem mass spectrometry data of both flavonoids were acquired on LC-QE-Orbitrap-MS,and the fragmentation pathways responsible for the primary fragment ions were proposed. The primary signal in MS1 occurred at m/z 285( [M-H]-),and the primary signals of either compound generated by retro-Diels-Alder fragmentation were observed at m/z 151 and 133. The spectral information was subsequently transferred onto LC-Qtrap-MS platform to carry out online ER-MS. Two precursor-to-product ion transition candidates were constructed as m/z 285>151 and 285>133,and either afterward derived a set of pseudo-ion transitions( PITs) and so forth,exactly corresponding to a series of progressive collision energies( eg-5,-8,-11 e V,and so on). All PITs were typed into the monitoring list of multiple reaction monitoring program to generate the peak area datasets. Either dataset was normalized using the highest values in the set and imported into Graph Pad Prism software to plot the Gaus-sian-shaped curve that was termed as the break-down graph. The apex of the regressive curve was termed as optimal collision energy( OCE). The OCE values corresponding to m/z 285>151 were calculated as-29. 06 e V and-35. 71 e V for kaempferol and luteolin,respectively. In the case of m/z 285>133,the OCEs were yielded as-44. 15 e V for kaempferol and-49. 01 e V for luteolin. With re-ference to their chemical structures,the location of hydroxyl group was regarded to be responsible for the differences of either m/z 285>151 or 285>133 between the isomers,attributing to their different bond properties. Above all,online ER-MS offers an eligible tool for isomeric discrimination,and provides meaningful information for the accurate chemical composition characterization based on LC-MS,which is not limited to Chinese herbal medicines.


Assuntos
Quempferóis , Luteolina , Cromatografia Líquida , Flavonoides , Espectrometria de Massas em Tandem
5.
Zhongguo Zhong Yao Za Zhi ; 46(9): 2215-2219, 2021 May.
Artigo em Chinês | MEDLINE | ID: mdl-34047123

RESUMO

This study aims to study the chemical components from the gum resin of Boswellia carterii. Five cembranoid diterpenes were isolated from the gum resin of B. carterii by various of column chromatographies including silica gel, Sephadex LH-20, and semi-preparative HPLC. Their structures were identified on the basis of physicochemical properties, mass spectrometry(MS), nuclear magnetic resonance(NMR), Ultraviolet(UV) and infrared(IR) spectroscopic data. These compounds were identified as(1S,2E,4R,5S,7E,11E)-4-methoxy-5-hydroxycembrane(1),(1R~*,4R~*,5E,8E,12E,15E)-4-hydroxycembra-5,8,12,15-tetraene(2), cembrene A(3),(3S,4S,7R)-4-hydroxycembrane(4), and pavidolide D(5). Compound 1 was a new compound. Compounds 2, 4, and 5 were obtained from the gum resin of B. carterii for the first time. Compound 2 showed weak inhibition on the human liver cancer cell line HepG2.


Assuntos
Boswellia , Diterpenos , Linhagem Celular , Humanos , Estrutura Molecular , Resinas Vegetais
6.
Zhongguo Zhong Yao Za Zhi ; 46(9): 2220-2228, 2021 May.
Artigo em Chinês | MEDLINE | ID: mdl-34047124

RESUMO

A new method of MS/MS~(ALL) was designed to sequentially record a MS~2 spectrum at each unit mass window through gas phase fractionation concept, so as to offer an opportunity for universal MS~2 spectral recording with direct infusion(DI). As a proof-of-concept, DI-MS/MS~(ALL) was applied for rapid chemome profiling of a famous herbal medicine named Lonicerae Japonicae Flos. After each MS~2 spectrum was correlated to its precursor ion, the structural annotation was conducted by applying well-defined mass cracking rules, matching the mass spectral data with literatures and referring to those accessible databases. As a result, a total of 54 components were identified from Lonicerae Japonicae Flos extract, including 21 phenolic acids, 13 flavonoids, 12 iridoids, 4 triterpenoids and 4 other compounds. Therefore, DI-MS/MS~(ALL) is a powerful tool for comprehensive, rapid qualitative analysis of chemical profiles of traditional Chinese medicine and other chemical components of complex systems.


Assuntos
Medicamentos de Ervas Chinesas , Lonicera , Cromatografia Líquida de Alta Pressão , Extratos Vegetais , Espectrometria de Massas em Tandem
7.
Zhongguo Zhong Yao Za Zhi ; 46(1): 130-138, 2021 Jan.
Artigo em Chinês | MEDLINE | ID: mdl-33645062

RESUMO

As a precious traditional Chinese medicine(TCM), snake bile has been widely used in numerous Chinese medicine prescriptions. Bile acid(BA) derivatives have been demonstrated as the primary chemical family in snake bile. In-depth chemical characterization of BAs is of great importance towards the establishment of quality standards and clarification of the effective material basis for snake bile. This study firstly employed ~1H-NMR to preliminarily analyze the chemical profiles of snake bile, an automated fraction collector was subsequently implemented to obtain the fractions-of-interest. The fraction was then concentrated and re-analyzed by LC-MS. Based on ~1H-NMR, BAs were found to be the main components of snake bile, and six BAs including CDCA, CA, TCDCA, TCA, TDCA and GCA were tentatively identified from the representative spectrum with the assistance of literature and reference compounds. Whereas the content of TCA in snake bile was too great, resulting in a great obstacle for the detection of trace components, the automated fraction collector was subsequently implemented to obtain the fractions-of-interest for LC-MS analysis. According to matching MS/MS information and retention time with reference compounds as well as database retrieval, a total of 57 BAs were detected and annotated. Because of the combination of ~1H-NMR and LC-MS platforms, the findings are beneficial for the in-depth characterization of BAs in snake bile, which provides references for the establishment of quality control and evaluation methods of snake bile.


Assuntos
Ácidos e Sais Biliares , Espectrometria de Massas em Tandem , Animais , Bile , Cromatografia Líquida , Serpentes
8.
Zhongguo Zhong Yao Za Zhi ; 45(13): 3175-3182, 2020 Jul.
Artigo em Chinês | MEDLINE | ID: mdl-32726027

RESUMO

Several Orobanche medicinal plants sometimes served as alternative sources of Cistanches Herba, attributing to the benefits such as tonifying kidney, strengthening tendons and bones. Among them, O. coerulescens, O. cernua and O. pycnostachya have been widely utilized in northern China for treatments of pains in the loins and knees, impotence, and spermatorrhea. However, their chemical profiles haven't been elucidated. In the present study, UHPLC-IT-TOF-MS was implemented to conduct in-depth chemome profiling of O. coerulescens, O. cernua and O. pycnostachya, aiming to achieve a comprehensive chemical characterization and to provide pronounced information for the quality control and clinical applications. An ACE Ultra-Core 2.5 Super C_(18)(3.0 mm×150 mm, 2.5 µm) column was deployed for chromatographic separations, and high-resolution MS~n spectra were recorded by IT-TOF-MS. Forty-eight components, in total, were observed, and thirty-eight ones were structurally annotated according to proposing mass fragmentation patterns, matching with relevant databases. Particularly, nine ones were confirmed by reference compounds. Overall, the chemical compositions of O. coerulescens and O. cernua are quite similar, and differences occur between O. pycnostachya and the prior two ones; primary chemical family is phenylethanoid glycosides, and several lignan glycosides as well as iridoid glycosides are also observed; the primary components include acteoside, isoacteoside, crenatoside and 2'-acetylacteoside, etc.


Assuntos
Cistanche , Orobanche , Plantas Medicinais , China , Glicosídeos , Masculino
9.
Zhongguo Zhong Yao Za Zhi ; 45(4): 899-909, 2020 Feb.
Artigo em Chinês | MEDLINE | ID: mdl-32237492

RESUMO

Citri Reticulatae Pericarpium(CRP, Chinese name: Chenpi) is one of the most famous edible traditional Chinese medicines(TCMs). CRP was first recorded as top grade TCM in Shennong Bencao Jing attributing to the benefits such as regulating Qi, tonifying spleen, eliminating dampness and eliminating phlegm, and has been widely utilized for the treatments of abdominal fullness and distention, vomiting and diarrhea, as well as phlegm cough. CRP is also widely popular as spice in food industry. Because of the wide cultivation, a number of brands that exhibit extensive price range can be found in the market, resulting in a great challenge for grading. Herein, an attempt was made to in-depth chemome profiling for the sake of providing meaningful information of the universal quality control of CRP. A new core-shell column packed with adamantylethyl substituted silica gel particles was deployed for chromatographic separations and IT-TOF-MS that is advantageous at providing abundant high resolution molecular and fragment ions was employed for qualitative detection. A total of 62 components were observed and 61 ones were structurally annotated according to proposing mass fragmentation patterns, matching with reference compounds and relevant databases, and the chemical families included flavone, limonin, etc. In particular, ten compounds bearing 3-hydroxy-3-methylglutarate substitute were detected from CRP for the first time. Above all, the chemical profile of CRP was characterized and the findings are meaningful for the in-depth quality assessment and efficacy material clarification of CRP.


Assuntos
Citrus/química , Medicamentos de Ervas Chinesas/química , Compostos Fitoquímicos/análise , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas , Medicina Tradicional Chinesa
10.
Zhongguo Zhong Yao Za Zhi ; 44(21): 4720-4727, 2019 Nov.
Artigo em Chinês | MEDLINE | ID: mdl-31872670

RESUMO

An ultra-performance liquid chromatography hybrid triple quadrupole-linear ion trap mass spectrometry(UPLC-QtrapMS) method was established to identify the metabolites in rat plasma,bile,urine and feces after oral administration of Cinnamomi Cortex(CC) aqueous extract. Several survey experiments,such as enhanced mass spectrum scan(EMS),precursor ion scan(PI),neutral loss scan(NL) and multiple ions monitoring(MIM) were applied to search target components,and two separate enhanced product ion(EPI) scans were triggered via information-dependent acquisition(IDA) method to generate the MS/MS spectra. According to the mass spectrometric data collected from reference standards and reported literature,the structures of metabolites were deduced. A total of76 metabolites and 5 original compounds were tentatively identified in rats after oral administration of CC aqueous extract. Deglycosylation,methylation,sulfonation,and glucuronidation were observed as the primary metabolic pathways for the chemical constituents of CC. These data are able to benefit the clarification of the therapeutic material basis,the clinical usage and further R&D of CC.


Assuntos
Bile , Medicamentos de Ervas Chinesas/metabolismo , Espectrometria de Massas em Tandem , Administração Oral , Animais , Cromatografia Líquida de Alta Pressão , Cinnamomum zeylanicum , Fezes , Ratos
11.
J Ethnopharmacol ; 244: 112138, 2019 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-31390529

RESUMO

ETHNOPHARMACOLOGICAL RELEVANCE: Dragon's blood (Chinese name: Xuejie), which comprises red resins obtained from several plants (27 species from 4 families), is drawing worldwide interests in medicinal applications owing to its broad pharmacological spectrum such as promoting blood circulation, regenerating muscle, relieving swelling and pain, maintaining hemostasis, etc. AIM OF THE STUDY: This work aims to evaluate current research progress on phenolic constituents, pharmacological activities, quality control, and metabolism of six Dracaena plants, namely, Dracaena cochinchinensis (Lour.) S.C.Chen, D. cambodiana Pierre ex Gagnep., D. cinnabari Balf. f., D. draco (L.) L., D. loureiroi Gagnep., and D. schizantha Baker, figure out the shortcomings of existing studies, and provide meaningful guidelines for future investigations. METHODS: Extensive database retrieval, such as SciFinder, PubMed, CNKI, ChemSpider, etc., was performed by using the keywords "Dracaena," "dragon's blood," as well as the Latin names of the six Dracaena species. In addition, relevant textbooks, patents, reviews, and documents were also employed to ensure sufficient information is collected. RESULTS: Flavonoids and their oligomers are the primary chemical clusters distributed in Dracaena plants. Pharmacological activities including analgesic, anti-inflammatory, antibacterial, hypolipidemic, hypoglycemic, and cytotoxic effects; bi-directional regulation effects on hemorheology; and cardiovascular and cerebrovascular effects have been disclosed by modern pharmacological evaluations. The chemical and metabolic profiles after oral administration of dragon's blood extract were preliminarily characterized. However, some of the pharmacological investigations reported only elementary methodologies and unreliable findings, and even worse, some important aspects were questionable or missing in these articles. CONCLUSIONS: Dragon's blood is a valuable source of bioactive compounds, mainly flavonoids and their oligomers. Its potential therapeutic effects on different diseases are attractive, such as the notable effect on cardiovascular diseases. In future studies, there is an urgent need to test the effect of this extract on appropriate cell lines and animal models to analyze its ethnopharmacological applications; moreover, "composition-effect correlation" methods and omics technologies are demanded for identifying the effective material basis and therapeutic mechanisms before entering into clinical trials. Moreover, attention should be paid to the chemical profiling and quality evaluation of this precious herbal medicine.


Assuntos
Dracaena , Animais , Etnofarmacologia , Humanos , Fenóis/análise , Fenóis/farmacologia , Compostos Fitoquímicos/análise , Compostos Fitoquímicos/farmacologia , Extratos Vegetais/química , Extratos Vegetais/farmacocinética , Controle de Qualidade
12.
Zhongguo Zhong Yao Za Zhi ; 44(13): 2667-2674, 2019 Jul.
Artigo em Chinês | MEDLINE | ID: mdl-31359675

RESUMO

Chemical profiling of a given herbal medicine( HM) is the prerequisite for clarifying the effective material basis and therapeutic mechanisms,and it is an important integral part of traditional Chinese medicine chemical biology( TCMCB). In current study,we aimed to propose a new strategy for fast chemical characterization of HM by using reversed phase liquid chromatography-hydrophilic interaction chromatography-predictive multiple reaction monitoring( RPLC-HILIC-p MRM),and Artemisiae Scopariae Herba was employed in this study to illustrate the entire strategy. In response to wide polarity spanning of the diverse chemical clusters in Artemisiae Scopariae Herba,RPLC and HILIC were coupled in series to retain and separate hydrophilic and hydrophobic components simultaneously by identifying the characteristics of chromatographic separation. Most of the chemical constituents in traditional Chinese medicine can be predicted by summarizing the results of chemical constituents of the same genera and introducing primary metabolites and possible substitution reaction types. Therefore,we constructed predictive ion pairs to rapidly identify the chemical constituents of Artemisiae Scopariae Herba. After comparison with control products,discussion on fragmentation pattern,and access to relevant information from literature and databases,a total of 139 components were detected and structurally annotated by matching the obtained spectral data with the information of authentic compounds. Above all,RPLC-HILIC-p MRM could be used as an eligible analytical tool for the chemical profiling of HMs.


Assuntos
Artemisia/química , Cromatografia de Fase Reversa , Plantas Medicinais/química , Interações Hidrofóbicas e Hidrofílicas , Medicina Tradicional Chinesa
13.
Zhongguo Zhong Yao Za Zhi ; 44(12): 2538-2543, 2019 Jun.
Artigo em Chinês | MEDLINE | ID: mdl-31359721

RESUMO

Bile acids( BAs),the major constituents of bile,are also known to be potential biomarkers of various diseases,especially liver disease. The systematic analysis of BAs is believed to be of great importance towards the clarification of the effective material basis for bile-type medicines,and the diagnosis and therapy of related diseases as well. As a part of systematic study on bile-type medicine ongoing in our group,this study lays emphasis on the isomer discrimination,and the improvement of analytical method of BAs. Further,this method was subsequently applied to elucidate in depth the chemical profile of BAs in yak bile. Regarding isomer discrimination for BAs,we constructed relative response-collision energy curves( RRCECs) by high performance liquid chromatographyion trap-time of flight-mass spectrometry( HPLC-IT-TOF-MS) in combination with high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry( HPLC-Qtrap-MS). As a result,both the optimum collision energy( OCE) and CE_(50) exhibited great correlations with structural characteristics,thus enabling the isomer distinguishing,such as unconjugated BAs,glycine-conjugated BAs,and taurine-conjugated BAs. According to information provided by mass spectrometry,the comparison of OCE and CE_(50),retention time matching,combined with reference substances and database retrieval,a total of 30 bile acid derivatives were observed and identified in yak bile. The newly developed method could serve as a feasible tool for the in-depth characterization of BAs in bile and biological samples.


Assuntos
Ácidos e Sais Biliares/química , Bile/química , Animais , Bovinos , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas , Taurina
14.
Zhongguo Zhong Yao Za Zhi ; 44(5): 849-860, 2019 Mar.
Artigo em Chinês | MEDLINE | ID: mdl-30989839

RESUMO

Traditional Chinese medicine(TCM) is a research area with highly original innovation features,and is also a Chinese name card to the world. However,TCM owns a unique theoretical system which is quite different from western modern medicine,leading to an awkward situation of deficient modern social identity as well as poor international spread. Therefore,how to establish a research strategy in line with the characteristics of TCM itself to systematically interpret the unique scientific connotation of TCM is always a public hot topic. Based on persistent practical exploration and scientific consideration in TCM,our group firstly promoted the concept of traditional Chinese medicine chemical biology(TCM chemical biology,TCMCB). The major idea of TCMCB is to clarify the nature of TCM regulating life progress to link TCM to modern medicine by using TCM components as chemical tools. Notably,TCMCB mainly focuses on TCM target identification and TCM-guided disease molecular mechanism exploration,further to clarify the basic law of TCM mediating disease process. Finally,TCMCB-guided scientific studies can help explain TCM theory and promote the developmentof modern innovative drugs based on identified targets using TCM active components. Moreover,TCMCB is of vital importance for investigating the scientific nature of biological progress and the pattern of disease occurrence and development,indicating a key significance for modern life science and medicine. This review introduces the definition of TCMCB as well as its academic thought,research method,technology system and scientific significance,for providing new research ideas and scientific thoughts for TCM development.


Assuntos
Pesquisa Interdisciplinar , Medicina Tradicional Chinesa , Biologia , Química , Medicina , Projetos de Pesquisa
15.
J Chromatogr Sci ; 57(4): 381-384, 2019 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-30721939

RESUMO

In this study, determination of adenosine in Cordyceps was accomplished by an online pressurized liquid extraction HPLC, and a poroshell column was employed for rapid HPLC separation. The Cordyceps sample powder was filled into a hollow guard column and extracted by thermal and pressurized water (75°C, 150 bar) for 3 min. Chromatographic separation was conducted on a poroshell 120 SB-Aq (4.6 × 50 mm, 2.7 µm) column and gradient elution was performed by water and methanol at a flow rate of 1.5 mL/min. The detection wavelength was set at 260 nm. The total measurement time including sample extraction and separation was <6 min. The calibration curve of adenosine was Y = 4.502 × 106X + 1.731 × 104, which showed good linearity (r2 > 0.9993) within tested range (4.03-80.5 µg/mL). The intra- and inter-day precisions of adenosine were 0.24% and 0.94%, respectively, and the recoveries of adenosine was 96.1% (relative standard deviation, 4.49%). The validated method was then applied to determinate adenosine in six batches of Cordyceps, and the contents of adenosine were 0.28-0.48 mg/g. The developed method is beneficial for the quality control of Cordyceps.


Assuntos
Adenosina/análise , Produtos Biológicos/análise , Cromatografia Líquida de Alta Pressão/métodos , Cordyceps/química , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos Testes
16.
Phytochemistry ; 158: 46-55, 2019 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-30453219

RESUMO

Fifteen previously undescribed 2-(2-phenylethyl)chromone dimers, along with two known analogues were isolated from Chinese agarwood (Aquilaria sinensis) by a LC-MS-guided fractionation procedure. Their structures were elucidated on the basis of spectroscopic and spectrometric data (1D and 2D NMR, IR, and HRESIMS). The isolated compounds exhibited significant inhibition of nitric oxide production in lipopolysaccharide-stimulated RAW264.7 cells with IC50 values in the range 0.6-37.1 µM.


Assuntos
Anti-Inflamatórios não Esteroides/química , Anti-Inflamatórios não Esteroides/farmacologia , Cromonas/química , Thymelaeaceae/química , Animais , Anti-Inflamatórios não Esteroides/isolamento & purificação , Cromatografia Líquida , Cromonas/isolamento & purificação , Dimerização , Avaliação Pré-Clínica de Medicamentos/métodos , Concentração Inibidora 50 , Lipopolissacarídeos/farmacologia , Espectroscopia de Ressonância Magnética , Camundongos , Estrutura Molecular , Óxido Nítrico/antagonistas & inibidores , Óxido Nítrico/metabolismo , Plantas Medicinais/química , Células RAW 264.7 , Espectrometria de Massas por Ionização por Electrospray
17.
Zhongguo Zhong Yao Za Zhi ; 43(18): 3708-3714, 2018 Sep.
Artigo em Chinês | MEDLINE | ID: mdl-30384537

RESUMO

As a holoparasitic plant, Cistanche deserticola is one of the two original sources of Cistanches Herba that is one of the most famous tonic medicines, in Chinese Pharmacopoeia. The succulent stems are used for medicinal usage, whereas those lignified stems as well as flowers of less pharmacological importance are usually deserted, suggesting extensive resource waste. Herein, chemical characterization of the flowers along with lignified stems was conducted using HPLC-IT-TOF-MS aiming to explore the medicinal valu of those non-medicinal parts. Following ultrasonication-assisted extraction with 50% aqueous methanol, either flower or lignified stem extract was subjected onto LC-IT-TOF-MS equipped with a Capcell core ADME column to acquire both MS¹ and MSº spectra, and gradient elution was carried out with combinatory 0.1% aqueous formic acid and acetonitrile. Both positive and negative ionization polarities were deployed, resulting in the observation of 62 components, in total. Thirty-nine signals were structurally annotated, including phenylethanoid glycosides, iridoids, lignans and saccharides according to matching with authentic components and literature information, as well as applying the proposed mass fragmentation rules. A total of 62 ones were putatively identified. Above all, lignified stems and flowers should not the qualified substitutes for the succulent stems attributing to the significant differences between the medicinal portion and those parts with less medicinal values.


Assuntos
Cistanche/química , Flores/química , Compostos Fitoquímicos/química , Caules de Planta/química , Cromatografia Líquida de Alta Pressão , Medicamentos de Ervas Chinesas/química , Compostos Fitoquímicos/isolamento & purificação
18.
Zhongguo Zhong Yao Za Zhi ; 43(17): 3506-3512, 2018 Sep.
Artigo em Chinês | MEDLINE | ID: mdl-30347919

RESUMO

As a famous tonic medicine, Cistanche tubulosa has been honored as "ginseng of the deserts" for centuries. Aiming to address the resource shortage as well as the wild resource protection towards this herbal medicine, wide cultivation has been achieved in the southern Xinjiang. Herein, in-depth chemome comparison was conducted between cultivated and wild plants using ¹H-NMR spectroscopy that is capable of comprehensively providing qualitative and quantitative information of given complicated matrices. Multivariate statistical analysis was employed to process the dataset as well as to consolidate that the cultivated plants are comparable to those wild ones in term of chemome. ¹H-NMR spectra of both wild and cultivated plants were acquired in parallel after extraction. Following direct overlaying, great similarity occurred between these two groups. A total of 28 compounds were tentatively identified by referring to authentic compounds together with those available databases, such as HMDB and BMRB. Following principal component analysis, none significant difference was observed between wild and cultivated groups. Above all, from the viewpoint of chemical profile, the cultivated plants were almost equal to the wild plants; therefore, the cultivated plants are able to take the load of wild plants in clinical usage. Moreover, ¹H-NMR spectroscopy is a promising tool for chemical profiling traditional Chinese medicines because of the potential towards simultaneously exhibiting both quantitative and qualitative information for complicated matrices.


Assuntos
Cistanche/química , Compostos Fitoquímicos/análise , Plantas Medicinais/química , Espectroscopia de Ressonância Magnética , Espectroscopia de Prótons por Ressonância Magnética
19.
Fitoterapia ; 131: 105-111, 2018 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-30339923

RESUMO

Five new homoisoflavonoid derivatives, including three meta-homoisoflavanes (1-3), one homoisoflavanone (4), and one homoisoflavan (5), along with five known analogues (6-10), were isolated from the red resin of Dracaena cochinchinensis (Chinese dragon's blood). Their structures were elucidated by analysis of spectroscopic data (1D and 2D NMR, IR, and HRESIMS). The absolute configuration of compound 1 was determined by single-crystal X-ray crystallographic analysis, and those of 2-5 were established on the basis of experimental and computed ECD data. Compounds 4, 6, and 9 exhibited moderate inhibition of nitric oxide production in lipopolysaccharide-stimulated BV-2 microglial cells with IC50 values of 60.4-75.6 µM.


Assuntos
Dracaena/química , Isoflavonas/isolamento & purificação , Resinas Vegetais/química , Animais , Linhagem Celular , Cristalografia por Raios X , Camundongos , Microglia/efeitos dos fármacos , Estrutura Molecular , Óxido Nítrico/metabolismo , Compostos Fitoquímicos/isolamento & purificação , Extratos Vegetais/química
20.
Zhongguo Zhong Yao Za Zhi ; 43(12): 2556-2562, 2018 Jun.
Artigo em Chinês | MEDLINE | ID: mdl-29950075

RESUMO

Two new polypeptides were isolated and purified from the extract of deer bone (constitutive part of Cucumis and Cervus polypeptide injection) by various column chromatography including C4 300Å and Sephadex G-50, as well as semipreparative HPLC. Their N-terminal amino acid sequences were identified by De Novo sequencing on the basis of MALDI-TOF-MS data and Explorer™ software. The N-terminal amino acid sequences of polypeptides were identified as NH2-Gly-Pro-Val-Gly-Pro-Thr-Gly-Pro-Val-Gly-Ala-Ala-Gly-Pro-Ser-Gly-Pro-Asp (Mei18 peptide, 1) and NH2-Ala-Gly-Pro-Ala-Gly-Pro-Leu-Gly-Pro-Leu-Gly-Pro-Leu-Gly-Pro-Leu-Gly-Pro-Pro-Asp-Ser-Try-Asp (Mei23 peptide, 2), respectively. Mei18 and Mei 23 peptides are new polypeptides.


Assuntos
Osso e Ossos/química , Cervos , Materia Medica/química , Peptídeos/química , Sequência de Aminoácidos , Animais , Espectrometria de Massas
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