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Objective: To investigate and analyze antioxidant activities in vitro and the active ingredients of the methanol extract of Actinidia arguta. Methods: In this study, antioxidant activities of extract of A. arguta were carried out by using DPPH and ABTS radical scavenging assays in vitro. Qualitative analysis of major active components was performed by HPLC-DAD-ESI-MS/MS. Results: Extract of A. arguta had good scavenging effect on DPPH and ABTS free radical in vitro, and the EC50 values of scavenging effect of extract of A. arguta on DPPH and ABTS free radical were (26.275 ± 1.464) and (29.826 ± 1.309) mg/mL, respectively. On the basis of UV and mass spectral analysis, a total of 19 chemical compositions were preliminarily identified. Conclusion: extract of A. arguta has good antioxidant activity in vitro, and polyhydroxyl and unsaturated double bonds are the main active constituents.
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Objective: To investigate the chemical constituents from Rhamnus heterophylla. Methods: Multiple chromatographic separation techniques including silica gel, Sephadex LH-20 gel and MCI gel were employed to isolate and purify the compounds. Their structures were identified by means of the nuclear magnetic resonance (NMR) and physicochemical properties. The chemical compositions were quickly analyzed by HPLC-DAD-ESI-MS/MS and scanned in negative ions. Results: These compounds were isolated and determined as cis-aloeemodin bianthrone (1), trans-aloeemodin bianthrone (2), emodin-8-O-rhamnoside (3), citreorosein (4), emodin (5), chrysophanol (6), physcion (7), kaempferol (8), luteolin (9), and quercetin (10). In addition to compounds 5, 8, the other compounds are isolated from R. heterophylla for the first time, and the compound 3 is isolated from the genus Rhamnus for the first time. 28 Compounds were speculated via comparing MS data (detected mass and MS2 fragment ions) and coupled with related literature, including three hydroxybenzoic acids, eight anthraquinones and 17 flavonoids. Conclusion: The analysis of chemical constituents from R. heterophylla could provide the references for the study on pharmacodynamic material basis and reasonable application and development.
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The fruits of Paulownia catalpifolia Gong Tong are used as a Chinese folk herbal medicine for the treatment of enteritis, tonsillitis, bronchitis, and dysentery, etc. Our previous study has identified new C-geranylated flavanones with obvious anti-proliferative effects in lung cancer A549 cells. In the present study, a new C-geranylated flavone, paucatalinone C (1) and five known C-geranylated flavanones (2-6) were isolated. In addition, a total of 34 C-geranylated flavonoids were detected by HPLC-DAD-ESI-MS/MS coupling techniques from the CHCl extract of P. catalpifolia. Futhermore, anti-aging effects of isolated compounds were evaluated in vitro with premature senescent 2BS cells induced by HO. Phytochemical results indicated that P. catalpifolia was a natural resource of abundant C-geranylated flavonoids. Diplacone (3) and paucatalinone A (5) were the potent anti-aging agents in the premature senescent 2BS cells induced by HO and the C-geranyl substituent may be an important factor because of its lipophilic character.
Subject(s)
Humans , Aging , Cell Line , Chromatography, High Pressure Liquid , Flavonoids , Chemistry , Pharmacology , Fruit , Chemistry , Hydrogen Peroxide , Toxicity , Magnoliopsida , Chemistry , Molecular Structure , Plant Extracts , Chemistry , Pharmacology , Tandem Mass SpectrometryABSTRACT
A comprehensive field research had been focused on growing status, underground biomass and active constituents of Notopterygium incisum and N. franchetii to evaluate the ecological suitability and appropriate cultivation zones by growing the two species seedlings along different elevation gradient. The results showed that compared to the survival rate and underground biomass, the beneficial altitude region to N. incisum was ranged from 2 600 m to 4 100 m, while N. franchetii required a lower altitude which ranges from 1 700 m to 3 600 m. For the active constituent contents, the values were higher in the range of 2 600 to 3 600 m for N. incisum, but for N. franchetii, the range was form 1 700 to 3 600 m. This result provides instructional guidance and scientific basis for artificial cultivation of N. incisum and N. franchetii.
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Tilia species, among which is Tilia cordata Mill. (Tiliaceae), have been used in folk medicine as anxiolytic. The hydroethanolic extract was analyzed by using liquid chromatography with mass spectrometry HPLC-DAD-ESI-MS/MS in negative ion mode, and its chemical composition was compared to flavonoids reported as anxiolytics. The major flavonoids found were: quercetin-3,7-di-O-rhamnoside, kaempferol-3,7-di-O-rhamnoside and kaempferol 3-O-(6"-p-coumaroyl glucoside) or tiliroside. The anxiolytic activity of the genus Tilia has been attributed to the presence of quercetin and kaempferol derivatives, while the anxiolytic activity of T. americana var. Mexicana was attributed to tiliroside, which was also found among the major constituents of this species.
As espécies de Tilia, entre elas, a Tilia cordata Mill. (Tiliaceae) são utilizadas como ansiolíticas na medicina popular. O extrato hidroalcoólico foi analisado usando cromatografia líquida acoplada à espectrometria de massas HPLC-DAD-ESI/MS/MS no modo negativo e a sua composição química foi comparada com os flavonóides já reportados como ansiolíticos. Os principais flavonóides encontrados foram: quercetina-3,7-di-O-rhamnosideo, canferol-3,7-di-O-rhamnosideo, e canferol 3-O-(6"-p-cumaroil glucosideo) ou tilirosideo. A atividade ansiolítica do gênero Tília tem sido atribuída à presença de derivados de canferol e quercetina, enquanto que a atividade ansiolítica da T. americana var. Mexicana foi atribuída ao tilirosideo, o qual também foi encontrado entre os principais constituintes desta espécie.
Subject(s)
Anti-Anxiety Agents , Tilia europaea/analysis , Quercetin , Glycosides , Gas Chromatography-Mass Spectrometry/methodsABSTRACT
The diversified genus Passiflora is well distributed all over Brazil, and many species have been long used as medicinal plants, mainly against anxiety disturbances. This effect has been attributed to its rich flavonoid composition. Flavonoids main class, flavonoid glycosides, has presented central action, particularly as sedative-hypnotic, anxiolytic and analgesic. The objective of the present study was to make a phytochemical screening of five little studied Passiflora species, in order to evaluate their phenolic composition. For this aim, HPLC-DAD-ESI-MS/MS was used. After the preparation of the hydroalcoholic extracts, each species was evaluated by direct injection electrospray ionization (ESI) and tandem mass spectrometry. Although belonging to the same genus, the composition of each species presented particularities; this justifies the importance of studies aiming for the phenolic composition of different Passiflora species. Flavones C-glycosides were detected in all extracts, and are found as the main constituents in P. vitifolia, P. coccinea, P. bahiensis and P. sidifolia. In this last one, flavone-6,8-di-C-glycoside, apigenin-6-C-rhamnosyl-8-C-arabinoside are present in high content. Cyclopassiflosides were found in high content together with cyanogenic glycosides in P. quadrangularis, while in P. coccinea, besides flavones-C-glycosides were also found procyanidins.
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Siparuna guianensis Aubl., Siparunaceae, is used as anxiolytic plants in folk medicine by South-American indians, "caboclos" and river-dwellers. This work focused the evaluation of phenolic composition of hydroethanolic extract of S. guianensis through HPLC-DAD-ESI/MS/MS. The constituents exhibited protonated, deprotonated and sodiated molecules and the MS/MS fragmentation of protonated, deprotonated and sodiated molecules provided product ions with rich structural information. Vicenin-2 (apigenin-6,8-di-C-glucoside) was the main constituent found in S. guianensis together quercetin-3,7-di-O-rhamnoside and kaempferol-3,7di-O-rhamnoside. A commercial extract of Passiflora incarnata (Phytomedicine) was used as surrogate standard and also was analyzed through HPLC-DAD-ESI/ MS/MS, showing flavones C-glycosides as constituents, among them, vicenin-2 and vitexin. The main constituent was vitexin. Flavonols triglycosides was also found in low content in S. guianensis and were tentatively characterized as quercetin-3O-rutinoside-7-O-rhamnoside, quercetin-3-O-pentosyl-pentoside-7-O-rhamnoside and kaempferol-3-O-pentosyl-pentoside-7-O-rhamnoside. Apigenin and kaempferol derivatives had been reported as anxiolytic agents. Flavonoids present in this extract were correlated with flavonoids reported as anxiolytics.
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A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill.The chemical profile of the twelve compounds,including geniposidic acid（1）,geniposide（2）,gentiopicroside（3）,liquiritin（4）,crocin（5）,baicalin（6）,wogonoside（7）,baicalein（8）,glycyrrhizic acid（9）,wogonin（10）,oroxylin A（11）and aristolochic acid A（12）,was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer（HPLC-DAD-ESI-MS）.The analysis was performed on a Dikma Platisil ODS C18 column（250 mm×4.6 mm,5 μm）with a gradient solvent system of acetonitrile-0.1% aqueous formic acid.The validation was carried out and the linearities（r〉0.9996）,repeatability（RSD〈1.8%）,intra-and inter-day precision（RSD〈1.3%）,and recoveries（ranging from 96.6% to 103.4%）were acceptable.The limits of detection（LOD）of these compounds ranged from 0.29 to 4.17 ng.Aristolochic acid A,which is the toxic ingredient,was not detected in all the batches of Longdan Xiegan Pill.Furthermore,hierarchical cluster analysis was used to evaluate the variation of the herbal prescription.The proposed method is simple,effective and suitable for the quality control of this traditional Chinese medicine（TCM）.
ABSTRACT
A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill.The chemical profile of the twelve compounds,including geniposidic acid (1),geniposide(2),gentiopicroside(3),liquiritin(4),crocin(5),baicalin(6),wogonoside(7),baicalein(8),glycyrrhizic acid (9),wogonin (10),oroxylin A ( 11 ) and aristolochic acid A (12),was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS).The analysis was performed on a Dikma Platisil ODS C18 column (250 mm × 4.6 mm,5 μm ) with a gradient solvent system of acetonitrile-0.1％ aqueous formic acid.The validation was carried out and the linearities ( r ＞ 0.9996),repeatability (RSD＜1.8％),intra- and inter-day precision (RSD＜1.3％),and recoveries (ranging from 96.6％ to 103.4％ ) were acceptable.The limits of detection (LOD) of these compounds ranged from 0.29 to 4.17 ng.Aristolochic acid A,which is the toxic ingredient,was not detected in all the batches of Longdan Xiegan Pill.Furthermore,hierarchical cluster analysis was used to evaluate the variation of the herbal prescription.The proposed method is simple,effective and suitable for the quality control of this traditional Chinese medicine (TCM).
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Objective: To analyze the chemical constituents of Rhizoma belamcandae by using high-performance liquid chromatography-diode array detector/electrospray ionization-mass spectrometry (HPLC-DAD/ESI-MS). Methods: Dried Belamcanda chinensis powder was extracted with 70% ethanol by sonication. The chromatographic separation was performed on a YMC ODS-C18 column (250 mm X 4.6 mm I. D., 5 μm) with a mobile phase composed of 20%CH 3OH(A)-70%ACN(B) (0→ 30→45→65 min, 20→30→90→100 B), eluted at a flow rate of 0.45 ml/min, and the UV detection wavelength was set at 265 nm. Positive ionization mode with a needle voltage of 5 000 V, a capillary voltage of 20 V, a gas (N2) press of 20 psi and a temperature of the drying gas of 300°C was selected. Relative molecular mass data acquisition was performed from m/z 250 to 550 in full MS scan mode. Results: Nine major isoflavones were identified from Rhizoma belamcandae based on their retention behavior obtained on-line by their UV spectra and the HPLC-DAD/ESI-MS. Conclusion: A rapid and efficient HPLC-DAD/ESI-MS method for identifying the chemical constituents of Belamcandae chinensis has been established, which provides more scientific information for quality control of Rhizoma belamcandae.
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Objective:To analyze the chemical constituents of Rhizoma belamcandae by using high-performance liquid chromatography-diode array detector/electrospray ionization-mass spectrometry (HPLC-DAD/ESI-MS).Methods: Dried Belamcanda chinensis powder was extracted with 70% ethanol by sonication.The chromatographic separation was performed on a YMC ODS-C18 column (250 mm?4.6 mm I.D.,5 ?m) with a mobile phase composed of 20%CH3OH(A)-70%ACN(B) (0→30→45→65 min,20→30→90→100 B),eluted at a flow rate of 0.45 ml/min,and the UV detection wavelength was set at 265 nm.Positive ionization mode with a needle voltage of 5 000 V,a capillary voltage of 20 V,a gas(N2)press of 20 psi and a temperature of the drying gas of 300℃ was selected.Relative molecular mass data acquisition was performed from m/z 250 to 550 in full MS scan mode.Results: Nine major isoflavones were identified from Rhizoma belamcandae based on their retention behavior obtained on-line by their UV spectra and the HPLC-DAD/ESI-MS.Conclusion: A rapid and efficient HPLC-DAD/ESI-MS method for identifying the chemical constituents of Belamcandae chinensis has been established,which provides more scientific information for quality control of Rhizoma belamcandae.
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Objective To establish the analytical method for fingerprint of Aristolochia manshuriensis by HPLC-DAD-ESI/MS,which can be used as the basis for quality control of the drug and for the further studies on kidney toxicity metabolite.Methods Samples A.manshuriensis from different habitats were extracted by 75% methanol and analyzed by HPLC-DAD-ESI/MS,whose chromatographic fingerprints were established.Two ways to calculate the similarity were selected to compare the results by determining the common peaks.Results There were 30 main characteristic components in A.manshuriensis.The HPLC-DAD-ESI/MS fingerprint of the 30 common peaks was established preliminarily.The samples of A.manshuriensis from different habitats was found having a good similarity,and the range of similarities for 24 balches of A.manshuriensis were 0.871—0.998.Conclusion The method is reliable,accurate,and of good stability,and can be used for the quality control and variety identification of A.manshuriensis.