Background:Qingyangshen(Cynanchum otophyllum C.K.Schneid)is a folk drug for treating depression and other mental disorders induced by social defeat stress.Neuroplasticity in the hippocampus is essential for the modula...Background:Qingyangshen(Cynanchum otophyllum C.K.Schneid)is a folk drug for treating depression and other mental disorders induced by social defeat stress.Neuroplasticity in the hippocampus is essential for the modulation of cognition and emotion,and its impairment may contribute to the development and progression of depression.Our previous studies have found that Qingyangshen glycosides(QYS)can improve depression-like behavior in social failure mouse models,mainly through PGC-1α/FNDC5/BDNF signaling pathways activation,but its effects and mechanisms on hippocampal neuroplasticity remain unknown.Methods:Chronic social defeat stress(CSDS)was used to induce social defeat in mice.Morphological changes in the hippocampus were observed by H&E staining and Golgi staining.Immunofluorescence double staining was used to detect the expression of synaptophysin(SYN)and postsynaptic density protein-95(PSD-95),while western blot was employed to evaluate PSD-95,SYN,and doublecortin(DCX)proteins.The pathological processing of social defeat and the therapeutic effects of QYS on it was confirmed through behavioral assessment associated with morpho-logic observation.Results:During the whole study,the sucrose preference indices and OFT activity time of CSDS mice were significantly decreased(p≤0.05),and the tail suspension immobil-ity time was significantly increased(p≤0.05),suggesting that the mice had significant depressive symptoms.Treatment with QYS(25,50,and 100 mg/kg)significantly al-leviated depressive symptoms in CSDS mice,which was demonstrated by significantly(p≤0.05 or p≤0.01)reducing the duration of tail-hanging immobility and increasing the tendency of sucrose preference indices and OFT activity time.QYS treatment also significantly increased the expression of DCX,PSD-95,and SYN proteins,which play a crucial role in depression.Conclusions:QYS alleviated these symptoms by enhancing hippocampal neuroplasti-city through upregulating the expression of synapse-associated proteins(SAPs).The therapeutic mechanism of QYS may involve modulating the neuroplasticity of hip-pocampus neurons by altering the expression of SAPs.展开更多
Five new flavan-4-ol glycosides jixueqiosides A-E(1-5)and two new flavan glycosides jixueqiosides F and G(6 and 7),along with twelve known flavan-4-ol glycosides(8-19),were isolated from the roots of Pronephrium penan...Five new flavan-4-ol glycosides jixueqiosides A-E(1-5)and two new flavan glycosides jixueqiosides F and G(6 and 7),along with twelve known flavan-4-ol glycosides(8-19),were isolated from the roots of Pronephrium penangianum.Comprehensive spectral analyses,X-ray single-crystal diffraction,and theoretical electronic circular dichroism(ECD)calculations established structures and absolute configurations.A single crystal structure of flavan-4-ol glycoside(14)was reported for the first time,while the characteristic ECD and NMR data for all isolated flavan-4-ol glycosides(1-5,8-19)were analyzed,establishing a set of empirical rules.Activity screening of these isolates showed that 8 and 9 could inhibit the proliferation of MDA-MB-231 and MCF-7 cells with IC50 values of 7.93±2.85μmol·L^(-1)and 5.87±1.58μmol·L^(-1)(MDA-MB-231),and 2.21±1.38μmol·L^(-1)and 3.52±1.55μmol·L^(-1)(MCF-7),respectively.Western blotting and flow cytometry analyses demonstrated that 8 and 9 dose-dependently induced apoptosis in MDA-MB-231 cells by up-regulating BAX,activating caspase-3 and down-regulating BCL-2.Additionally,compound 8 affected autophagy-related proteins,increasing the ratio of LC3-II/LC3-I and Beclin-1 levels to inhibit MDA-MB-231 cell proliferation.Moreover,anti-inflammatory studies indicated that 2,3,7,13,14,and 18 moderately inhibited tumor necrosis factor-α(TNF-α),interleukin-6(IL-6),and nitric oxide(NO)release.展开更多
The high content of cyanogenic glycosides(CG)in cassava tubers affects food safety.CG are involved in the plant growth and development and protect cassava leaves from herbivorous predators.However,the regulatory mecha...The high content of cyanogenic glycosides(CG)in cassava tubers affects food safety.CG are involved in the plant growth and development and protect cassava leaves from herbivorous predators.However,the regulatory mechanism of CG biosynthesis remains poorly understood.Here,yeast one-hybrid assays were performed using a mixed cDNA library of cassava tubers and leaves as prey and the promoter of MeCYP79D2 as bait.MeCYP79D2,a cytochrome P450 protein,is the rate-limiting enzyme for CG synthesis in cassava.From this information,a candidate regulator of MeCYP79D2 was selected and identified as transcription factor MePHD1.2.MePHD1.2,located in the nucleus and exhibiting an inhibitory transcription activity directly bound to an AT-rich motif in the promoter of MeCYP79D2.In cassava,the transcriptional activity of MeCYP79D2 was considerably enhanced in mephd1.2 mutant lines leading to increased linamarin and lotaustralin contents.Deletion of MePHD1.2 promoted the production of CGs in cassava and decreased transcription inhibition on MeCYP79D2,exposing a novel regulatory module governing biosynthesis of CGs.展开更多
Phytochemical study of the n-BuOH extract of Ilex asprella resulted in the discovery of ten new pentacyclic triterpenoid glycosides,comprising nine ursane-type glycosides(1-9)and one oleanane-type glycoside(10),along ...Phytochemical study of the n-BuOH extract of Ilex asprella resulted in the discovery of ten new pentacyclic triterpenoid glycosides,comprising nine ursane-type glycosides(1-9)and one oleanane-type glycoside(10),along with seven known compounds(11-17).Compound 1 is the first reported 19,22-epoxy ursane triterpenoid glycoside,whereas 4 and 5 are rare examples of ursane triterpenoid glycosides containing a 28,19-lactone group.The structural characterization of these compounds was achieved using spectroscopic and chemical techniques,as well as single-crystal X-ray analysis.Compounds 7,12,15,and 17 exhibited moderate cytotoxic activities against H1975 and HCC827 cancer cells.展开更多
Rheumatoid arthritis(RA),a globally increasing autoimmune disorder,is associated with increased disability rates due to the disruption of iron metabolism.Tripterygium glycoside tablets(TGTs),a Tripterygium wilfordii H...Rheumatoid arthritis(RA),a globally increasing autoimmune disorder,is associated with increased disability rates due to the disruption of iron metabolism.Tripterygium glycoside tablets(TGTs),a Tripterygium wilfordii Hook.f.(TwHF)-based therapy,exhibit satisfactory clinical efficacy for RA treatment.However,drug-induced liver injury(DILI)remains a critical issue that hinders the clinical application of TGTs,and the molecular mechanisms underlying the efficacy and toxicity of TGTs in RA have not been fully elucidated.To address this problem,we integrated clinical multi-omics data associated with the anti-RA efficacy and DILI of TGTs with the chemical and target profiling of TGTs to perform a systematic network analysis.Subsequently,we identified effective and toxic targets following experimental validation in a collagen-induced arthritis(CIA)mouse model.Significantly different transcriptome–protein–metabolite profiles distinguishing patients with favorable TGTs responses from those with poor outcomes were identified.Intriguingly,the clinical efficacy and DILI of TGTs against RA were associated with metabolic homeostasis between iron and bone and between iron and lipids,respectively.Particularly,the signal transducer and activator of transcription 3(STAT3)–hepcidin(HAMP)/lipocalin 2(LCN2)–tartrate-resis tant acid phosphatase type 5(ACP5)and STAT3–HAMP–acyl-CoA synthetase long-chain family member 4(ACSL4)–lysophosphatidylcholine acyltransferase 3(LPCAT3)axes were identified as key drivers of the efficacy and toxicity of TGTs.TGTs play dual roles in ameliorating CIA-induced pathology and in inducing hepatic dysfunction,disruption of lipid metabolism,and hepatic lipid peroxidation.Notably,TGTs effectively reversed“iron–bone”disruptions in the inflamed joint tissues of CIA mice by inhibiting the STAT3–HAMP/LCN2–ACP5 axis,subsequently leading to“iron–lipid”disturbances in the liver tissues via modulation of the STAT3–HAMP–ACSL4–LPCAT3 axis.Additional bidirectional validation experiments were conducted using MH7A and AML12 cells to confirm the bidirectional regulatory effects of TGTs on key targets.Collectively,our data highlight the association between iron-mediated metabolic homeostasis and the clinical efficacy and toxicity of TGT in RA therapy,offering guidance for the rational clinical use of TwHF-based therapy with dual therapeutic and toxic potential.展开更多
Ten previously undescribed dammarane-type triterpenoid glycosides,cyclocarysaponins A–J(1–10),were isolated from the leaves of Cyclocarya paliurus(Batal.)Iljinskaja.The structures of these compounds were characteriz...Ten previously undescribed dammarane-type triterpenoid glycosides,cyclocarysaponins A–J(1–10),were isolated from the leaves of Cyclocarya paliurus(Batal.)Iljinskaja.The structures of these compounds were characterized through detailed spectroscopic analysis,including 1D and 2D nuclear magnetic resonance(NMR)and high-resolution electrospray ionization mass spectrometry(HR-ESI-MS).The cytotoxic activities of all isolates were assessed against five human cancer cell lines(Bel-7402,Caski,BGC-823,A2780,and HCT-116).Of the tested compounds,compounds 1,7,and 9 exhibited selective cytotoxicity against one or more human cancer cell lines.展开更多
[Objectives]To study the inhibitory activity of two flavonoid glycosides isolated from Chlorophytum comosum Laxum R.Br on human nasopharyngeal carcinoma(NPC)cell line 5-8F in vitro and its mechanism.[Methods]The flavo...[Objectives]To study the inhibitory activity of two flavonoid glycosides isolated from Chlorophytum comosum Laxum R.Br on human nasopharyngeal carcinoma(NPC)cell line 5-8F in vitro and its mechanism.[Methods]The flavonoid glycosides were isolated and purified from the ethanol alcoholic extract of the roots of Liliaceae plant Chlorophytum comosum by silica gel column chromatography,macroporous resin column chromatography,Sephadex LH-20,and reverse column chromatography(ODS).The inhibitory activity of flavonoid glycosides on human nasopharyngeal carcinoma cells was analyzed by CCK-8 method,and the potential mechanism was preliminarily analyzed by molecular docking.[Results]Two flavonoid glycosides were identified as isovitexin 2″-0-rhamnoside and 7-2″-di-O-β-glucopyranosylisovitexin.Two flavonoid glycosides showed promising inhibitory effect on human nasopharyngeal carcinoma cell line 5-8F,with IC_(50) values of 24.8 and 27.5μmol/L,respectively.Molecular docking results showed that the potential targets of two flavonoid glycosides include CyclinD1,Bcl-2β-Catenin,ILK,TGF-β,in addition,two glycosides showed higher predicted binding affinity towards CyclinD1,which verifies the cytotoxicity of the two compounds on human nasopharyngeal carcinoma cell line 5-8F in vitro.[Conclusions]Two flavonoid glycosides are the active molecules in Chlorophytum comosum that can inhibit the proliferation of human nasopharyngeal carcinoma cells,and have the potential to be used in the research and development of anti nasopharyngeal carcinoma drugs.展开更多
Our continued works on the chemical constituents of Ginkgo biloba(G.biloba)leaves has led to the isolation of two novel phenylbutenoids(1,2),along with five previously unidentified terpene glycosides(3−7).Among them,c...Our continued works on the chemical constituents of Ginkgo biloba(G.biloba)leaves has led to the isolation of two novel phenylbutenoids(1,2),along with five previously unidentified terpene glycosides(3−7).Among them,compounds 1 and 2 represent unique(Z)-phenylbutenoids,3−6 are megastigmane glycosides,and 7 is identified as a rare bilobanone glycoside(Fig.1).This study marks the first reported isolation of phenylbutenoid and bilobanone glycoside from G.biloba.The chemical structures of these compounds were elucidated through extensive spectroscopic analysis,including HR-ESI-MS and various 1D and 2D NMR experiments.Furthermore,the absolute configurations of these molecules were determined using Mosher’s method,ECD experiments,and Cu-KαX-ray crystallographic analyses.展开更多
Introduction The plants of genus Cistanche G. Beck, which belong to Orobanchaceae family, include about twenty species, and there are four species and one variety are distributed in the northwest part of China. The d...Introduction The plants of genus Cistanche G. Beck, which belong to Orobanchaceae family, include about twenty species, and there are four species and one variety are distributed in the northwest part of China. The dried fleshy stem of Cistanche genus plant known as ＇Roucongrong＇ in Chinese traditional medicine, has long been used for kidney deficiency, female infertility, morbid leucorrhea, and neurasthenia. Studies on active components and pharmacological activities show that it possesses significant activities in enhancing potency, anti-fatigue, immuno-modulability, etc, and phenylethanoid glycosides are the major active components. Due to excessive exploitation, its natural resources are facing with exhaustion. In order to improve this situation, the plant has been cultivated on a large scale in the northwest part of China. Up to now, the chemical investigations of the cultivated Cistartcbe salsa have not been undertaken. In this paper we report seven phenylethanoid glycosides from the cultivated Cistanche salsa： echinacoside （1）, cistanoside A （2）, acteoside （3）, isoacteoside （4）, 2＇-acetylacteoside （5）, tubuloside B （6）, and eutigoside A （7）. Among them, compound 7 isolated fronl family Orobanchaceae was reported previously, and compounds 1, 2, 3, 4, 5 and 6 from the cultivated Cistanche salsa are reported for the first time.展开更多
Two new phenylpropanetriol glycosides, named as meliadanoside A (3 - methoxy- 5 - hydroxy-9- (1' - O-β-D-glucopyranosyl) - threo - phenylpropanetriol ) and meliadanoside B (4- hydroxy-7, 8- (2', 1' - O- ...Two new phenylpropanetriol glycosides, named as meliadanoside A (3 - methoxy- 5 - hydroxy-9- (1' - O-β-D-glucopyranosyl) - threo - phenylpropanetriol ) and meliadanoside B (4- hydroxy-7, 8- (2', 1' - O- β- D -glucopyranosyl) - phenylpropanetriol), were isolated from the water-soluble extract of the fruits of Meliatoosendan Sieb. et Zucc., along with threo-guaiacylglycerol. Their structures were elucidated by spectroscopic and chendcal analysis.展开更多
Two new C 27 steroidal glycosides, named ophiopojaponin A (1) and B (2), together with two known ones, were isolated from the tubers of the famous traditional Chinese herb Ophiopogon japonicus Ker_Gawl. The spect...Two new C 27 steroidal glycosides, named ophiopojaponin A (1) and B (2), together with two known ones, were isolated from the tubers of the famous traditional Chinese herb Ophiopogon japonicus Ker_Gawl. The spectroscopic and chemical evidence revealed their structures to be pennogenin 3_O_[2′_O_acetyl_α_L_rhamnopyranosyl (1→2)]_β_D_xylopyranosyl (1→3)_β_D_glucopyranoside (1), 26_O_β_D_glucopyranosyl_(22ξ, 25R)_3β, 14α, 22ξ, 26_tetrahydroxyfurost_5_ene 3_O_α_L_rhamnopyranosyl (1→2)_β_D_glucopyranoside (2), diosgenin 3_O_[α_L_rhamnopyranosyl (1→2)]_β_D_xylopyrano_syl (1→3)_β_D_glucopyranoside (3) and ruscogenin 1_O_[α_L_rhamnopyranosyl (1→2)]_β_D_xylopyranosyl (1→3)_β_D_fucopyranoside (4).展开更多
Three new phenolic glycosides, named as equisetumoside A (3-methoxy-11,12-dihydroxy-phenylhexane-9- one-4-O-beta -D-glucopyranoside), equisetumoside B (3-methoxy-4,11-dihydroxy-phenylhexane-9-one12-O-beta -D-glucopyra...Three new phenolic glycosides, named as equisetumoside A (3-methoxy-11,12-dihydroxy-phenylhexane-9- one-4-O-beta -D-glucopyranoside), equisetumoside B (3-methoxy-4,11-dihydroxy-phenylhexane-9-one12-O-beta -D-glucopyranoside) and equisetumoside C ( cis-ferulic acid potassium salt 4-O-beta -D-glucopyranoside) were isolated from the water-soluble extract of fertile sprouts of Equisetum, arvense L. (Equisetaceae), together with uridine, inosine, 2'-deoxyinosine, 2'-deoxycytidine, tryptophan, thymidine, 5-carboxy-2'-deoxyuridine, coniferin, and kaempferol 3-O-beta -D-sophoroside-7-O-beta -D-glucopyranoside. Their structures were elucidated by spectroscopic analysis and chemical transformation.展开更多
A reversed-phase high-performance liquid chromatography （RP-HPLC） method with diode array detector was established to simultaneously determine nine bioactive compounds in Wuzhuyu decoction, namely dehydroevodiamine,...A reversed-phase high-performance liquid chromatography （RP-HPLC） method with diode array detector was established to simultaneously determine nine bioactive compounds in Wuzhuyu decoction, namely dehydroevodiamine, isorhanmetin-7-O- rutinoside, 10-hydroxyrutaecarpine, diosmetin-7-O-13-D-glucopyranoside, evodiamine, rutaecarpine, 1-metbyl-2-n-nonyl-4（1H） quinolone, evocarpine, and dihydroevocarpine. The RP-HPLC assay was performed on a reversed-phase Cl8 column with a gradient elution. The mobile phases consisted of methanol and water containing 1% （v/v） acetic acid. The flow rate was 1.0 mL/min and the detection wavelength was set at 300 nm. All calibration curves showed good linearity （r2〉0.9941） within test ranges. The results of intra-day precision, inter-day precision, and accuracy were satisfactory. The overall recoveries were in the range of 90.13%-102.48%. The method was successfully applied to quantify nine bioactive compounds in six samples. Baseline resolution for all nine major compounds was achieved. This method could be used as a suitable quality control assay for Wuzhuyu decoction.展开更多
Two new alkaloids,hordenine-O- -L-rhamnopyranoside(Ⅰ)and hordenine -0-(6′-trans-cinnamoyl)-4′-O-β-D-glucopyranosyl- -L-rhamnopyranoside(Ⅲ) isolated from Selaginella doederleinii have been synthesized the first ti...Two new alkaloids,hordenine-O- -L-rhamnopyranoside(Ⅰ)and hordenine -0-(6′-trans-cinnamoyl)-4′-O-β-D-glucopyranosyl- -L-rhamnopyranoside(Ⅲ) isolated from Selaginella doederleinii have been synthesized the first time. A new method,in which trifluoroacetoxyl group was used both as a good leaving group and a protecting group for synthesis of O-glycosides with high stereo- selectivity was reported.展开更多
A simple, sensitive and specific high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）method combined with solid phase extraction has been developed and validated for the simultaneous quantifi...A simple, sensitive and specific high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）method combined with solid phase extraction has been developed and validated for the simultaneous quantification of paeoniflorinand albiflorin in rats plasma and tissue homogenate after administration of total glycosides of paeony （TGP）. Chromatographicseparation was achieved on a C15 column （150 mmx4.6 mm, 5 pro） with mobile phase consisted of acetonitrile-0.05% formicacid aqueous （20： 80, v/v） at a flow rate of 0.5 mL/min. The analytes were detected with triple-quadrupole mass spectrometer usingturbo ion spray with negative ionization in the multiple reaction-monitoring （MRM） modes. The results of method validationconformed to the requirements for the determination of biological samples. This method was successfully applied to thepharmacokinetics and tissue distribution study of TGP in rats. The results showed that paeonifiorin and albiflorin wereabsorbed and reached peak value quickly, and had the similar pharmacokinetic characteristics. Both of them underwent a rapid andwide distribution in the tissues throughout the whole body, among which stomach was the main distribution tissue. Moreover, theyhad the ability to cross the blood-brain barrier.展开更多
Monoterpene glycosides are the major bioactive compounds of Paeonia lactiflora Pall（P. lactiflora）. Characteristic neutral loss of 30 Da has been extensively reported for monoterpene glycosides in tandem mass spectr...Monoterpene glycosides are the major bioactive compounds of Paeonia lactiflora Pall（P. lactiflora）. Characteristic neutral loss of 30 Da has been extensively reported for monoterpene glycosides in tandem mass spectrometry. However, little is known about mechanism of this fragmentation. The neutral loss of 30 Da was studied for eleven monoterpene glycosides（1–11） from P. lactiflora by ion trap mass spectrometry in this report. Compounds 1–5 with a hemiacetal structure could readily lose 30 Da at low collision energy of 30% in MS/MS by ion trap mass spectrometry. For compounds 6–11, neutral loss of 30 Da could also be observed at low abundance, but the collision energy had to be increased to 60%. In both cases, high-accuracy mass spectrometry assigned the 30 Da as CH_2O. After careful analysis of the structures and mass spectra, we believe that the neutral loss of 30 Da in compounds 1–5 was due to cleavage of the hemiacetal structure, whereas it was ascribed to the cleavage of 5＇-hydroxymethyl group of the glucosyl residue in other monoterpene glycosides. Furthermore, the characteristic neutral loss of 30 Da at low collision energy was used to screen hemiacetals from crude extracts of P. lactiflora and related plant species. Significant differences among Paeonia species were observed by 30 Da neutral loss analysis.展开更多
Abstract： In the present study, we established an ultra performance liquid chromatography coupled with time-of-flight mass spectrometry （UPLC-QTOF-MSE） method to simultaneously quantify 33 components in Ginkgo bilo...Abstract： In the present study, we established an ultra performance liquid chromatography coupled with time-of-flight mass spectrometry （UPLC-QTOF-MSE） method to simultaneously quantify 33 components in Ginkgo biloba leaf extracts （GBEs）, including 17 flavonol glycosides, five terpene trilactones （TTLs）, four polyphenols and seven carboxylic acids. This optimized method was successfully applied to analyze the explicit compositions of GBE samples collected from different places. Furthermore, the data were processed through unsupervised principal component analysis （PCA） and supervised orthogonal partial least squared discrimination analysis （OPLS-DA） to evaluate the quality and compare the differences between the samples according to the contents of the 33 chemical constituents. Bilobalide, protocatechuic acid, shikimic acid, quinic acid, ginkgolide B, ginkgolide J, kaempferol-3-O-rutinoside, isorhamnetin-3-O-rutinoside, quercetin-3-O-ct-L-rhamnopyranocyl-2＂-（6＇＂-p-coumaroyl）-β-D-glucoside and rutin were recognized as characteristic chemical markers that contributed most to control the quality of GBEs. Based on the fact that GBEs should be standardized with the characteristic components as quality control chemical markers, it is most important to maintain the quality of GBEs stable and reliable, and this method also provided a good strategy to further rectify and standardize the GBEs market.展开更多
Two new stilbene glycosides (1 and 2), together with nine known compounds (3-11), were isolated from the water extract of Polygonum multiflorum Thunb. The structures of the new compounds were elucidated by their c...Two new stilbene glycosides (1 and 2), together with nine known compounds (3-11), were isolated from the water extract of Polygonum multiflorum Thunb. The structures of the new compounds were elucidated by their chemical properties and spectroscopic analyses, including extensive 2D NMR experiments. Compound 2 showed strong DNA cleavage activity, and compounds 1, 2 and 10 (2, 3, 4′, 5_tetrahydroxy_ trans _stilbene_2_O_β_ D _glucopyranoside) exhibited significant inhibition of lipid peroxidation.展开更多
AIM: To develop and validate a high performance liquid chromatography(HPLC) coupled with diode array and evaporative light scattering detectors(DAD-ELSD) method for the quantitative determination and fingerprint analy...AIM: To develop and validate a high performance liquid chromatography(HPLC) coupled with diode array and evaporative light scattering detectors(DAD-ELSD) method for the quantitative determination and fingerprint analysis of ten active constituents in three chemical classes(namely, xanthone glycosides, steroidal saponins, and alkaloids) in Zhimu-Huangbai herb pair(ZB). METHOD: Chromatographic separation was performed on a Diamonsil C18 column(4.6 mm × 250 mm, 5 μm, Dikma) by gradient elution using acetic acid in acetonitrile solution at a flow rate of 1.0 mL·min–1 at 260 nm. The drift tube temperature of ELSD was set to 60 ℃ and nebulizer gas pressure was 4.0 Bar. Method validation was performed to assure its linearity, limits of detection and quantification, precision, repeatability, stability, and accuracy. RESULTS: The HPLC-DAD-ELSD method allowed the quantification of ten compounds(phellodendrine, jatrorrhizine, palmatine, berberine, neomangiferin, mangiferin, timosaponin E-I, timosaponin B-II, timosaponin B, and timosaponin A-III), and was successfully applied to fingerprint analysis for ten batches of ZB samples. CONCLUSION: This was the first time to apply the combination of DAD and ELSD for the simultaneous determination of ten active ingredients in ZB. The results showed that the combination of quantitative analysis for marker ingredients and chemical fingerprint for the TCM herb pair provides a potentially powerful, widely introduced, and internationally accepted strategy for assessment of complex TCM formulas.展开更多
Two new phenolic glycosides, 2,3-dihydroxybenzoic acid methyl ester 3-O-β-o-glucopyranosyl-（1-6）-β-D-glucopyranoside （1） and 2,5-dihydroxylbenzofuran 5-O-β-D-xylopyranosyl-（1-6）-O-β-D-glucopyranoside （2）, ...Two new phenolic glycosides, 2,3-dihydroxybenzoic acid methyl ester 3-O-β-o-glucopyranosyl-（1-6）-β-D-glucopyranoside （1） and 2,5-dihydroxylbenzofuran 5-O-β-D-xylopyranosyl-（1-6）-O-β-D-glucopyranoside （2）, were isolated as the minor chemical constituents from the roots of Gentiana rigescens, along with 15 known compounds. Their structures were elucidated by detailed spectroscopic analysis, including 1D, 2D NMR and chemical method. All of these compounds were isolated for the first time from the title plant. Moreover, compounds 1 and 2 were tested for the antifungal activities on three plant pathogens Peronophythora litchi, Glomerella cingulata, and Glorosprium musarum.展开更多
基金Guizhou Administration of TCM,Traditional Chinese medicine,Ethnic Medicine Science and Technology Research Special Project,Grant/Award Number:QZYY-2022-008Subsidy Fund for Scientific Research and Innovation Exploration Project,National Natural Science Foundation of China of Guizhou University of Traditional Chinese Medicine,Grant/Award Number:2018YFC170810502+1 种基金Science and Technology Fund Project of Guizhou Provincial Health Commission,Grant/Award Number:gzwkj2023-147Development of animal models for drug discovery-brain diseases.National Research and Development Project of China,MOST,Grant/Award Number:2023YFF0724802.
文摘Background:Qingyangshen(Cynanchum otophyllum C.K.Schneid)is a folk drug for treating depression and other mental disorders induced by social defeat stress.Neuroplasticity in the hippocampus is essential for the modulation of cognition and emotion,and its impairment may contribute to the development and progression of depression.Our previous studies have found that Qingyangshen glycosides(QYS)can improve depression-like behavior in social failure mouse models,mainly through PGC-1α/FNDC5/BDNF signaling pathways activation,but its effects and mechanisms on hippocampal neuroplasticity remain unknown.Methods:Chronic social defeat stress(CSDS)was used to induce social defeat in mice.Morphological changes in the hippocampus were observed by H&E staining and Golgi staining.Immunofluorescence double staining was used to detect the expression of synaptophysin(SYN)and postsynaptic density protein-95(PSD-95),while western blot was employed to evaluate PSD-95,SYN,and doublecortin(DCX)proteins.The pathological processing of social defeat and the therapeutic effects of QYS on it was confirmed through behavioral assessment associated with morpho-logic observation.Results:During the whole study,the sucrose preference indices and OFT activity time of CSDS mice were significantly decreased(p≤0.05),and the tail suspension immobil-ity time was significantly increased(p≤0.05),suggesting that the mice had significant depressive symptoms.Treatment with QYS(25,50,and 100 mg/kg)significantly al-leviated depressive symptoms in CSDS mice,which was demonstrated by significantly(p≤0.05 or p≤0.01)reducing the duration of tail-hanging immobility and increasing the tendency of sucrose preference indices and OFT activity time.QYS treatment also significantly increased the expression of DCX,PSD-95,and SYN proteins,which play a crucial role in depression.Conclusions:QYS alleviated these symptoms by enhancing hippocampal neuroplasti-city through upregulating the expression of synapse-associated proteins(SAPs).The therapeutic mechanism of QYS may involve modulating the neuroplasticity of hip-pocampus neurons by altering the expression of SAPs.
基金supported by the National Natural Science Foundation of China(No.81874369)the Excellent Youth Project of the Hunan Provincial Department of Education(No.22B0388)the Project of Hunan Administration of Traditional Chinese Medicine(No.B2023143)。
文摘Five new flavan-4-ol glycosides jixueqiosides A-E(1-5)and two new flavan glycosides jixueqiosides F and G(6 and 7),along with twelve known flavan-4-ol glycosides(8-19),were isolated from the roots of Pronephrium penangianum.Comprehensive spectral analyses,X-ray single-crystal diffraction,and theoretical electronic circular dichroism(ECD)calculations established structures and absolute configurations.A single crystal structure of flavan-4-ol glycoside(14)was reported for the first time,while the characteristic ECD and NMR data for all isolated flavan-4-ol glycosides(1-5,8-19)were analyzed,establishing a set of empirical rules.Activity screening of these isolates showed that 8 and 9 could inhibit the proliferation of MDA-MB-231 and MCF-7 cells with IC50 values of 7.93±2.85μmol·L^(-1)and 5.87±1.58μmol·L^(-1)(MDA-MB-231),and 2.21±1.38μmol·L^(-1)and 3.52±1.55μmol·L^(-1)(MCF-7),respectively.Western blotting and flow cytometry analyses demonstrated that 8 and 9 dose-dependently induced apoptosis in MDA-MB-231 cells by up-regulating BAX,activating caspase-3 and down-regulating BCL-2.Additionally,compound 8 affected autophagy-related proteins,increasing the ratio of LC3-II/LC3-I and Beclin-1 levels to inhibit MDA-MB-231 cell proliferation.Moreover,anti-inflammatory studies indicated that 2,3,7,13,14,and 18 moderately inhibited tumor necrosis factor-α(TNF-α),interleukin-6(IL-6),and nitric oxide(NO)release.
基金supported by grants from the National Natural Science Foundation of China(32460505)China Agriculture Research System(CARS-11)+2 种基金the Chinese Academy of Tropical Agricultural Sciences for the Science and Technology Innovation Team of the National Tropical Agricultural Science Center(CATASCXTD202301)Additional support was provided by the Hainan Province Graduate Innovation Research Project(Hyb2020-09)the Key Laboratory of Tropical Fruits and Vegetables Quality and Safety for State Market Regulation(KF-2023016).
文摘The high content of cyanogenic glycosides(CG)in cassava tubers affects food safety.CG are involved in the plant growth and development and protect cassava leaves from herbivorous predators.However,the regulatory mechanism of CG biosynthesis remains poorly understood.Here,yeast one-hybrid assays were performed using a mixed cDNA library of cassava tubers and leaves as prey and the promoter of MeCYP79D2 as bait.MeCYP79D2,a cytochrome P450 protein,is the rate-limiting enzyme for CG synthesis in cassava.From this information,a candidate regulator of MeCYP79D2 was selected and identified as transcription factor MePHD1.2.MePHD1.2,located in the nucleus and exhibiting an inhibitory transcription activity directly bound to an AT-rich motif in the promoter of MeCYP79D2.In cassava,the transcriptional activity of MeCYP79D2 was considerably enhanced in mephd1.2 mutant lines leading to increased linamarin and lotaustralin contents.Deletion of MePHD1.2 promoted the production of CGs in cassava and decreased transcription inhibition on MeCYP79D2,exposing a novel regulatory module governing biosynthesis of CGs.
基金supported by the Qi-Huang Chief Scientist Project of the National Administration of Traditional Chinese Medicine(2020).
文摘Phytochemical study of the n-BuOH extract of Ilex asprella resulted in the discovery of ten new pentacyclic triterpenoid glycosides,comprising nine ursane-type glycosides(1-9)and one oleanane-type glycoside(10),along with seven known compounds(11-17).Compound 1 is the first reported 19,22-epoxy ursane triterpenoid glycoside,whereas 4 and 5 are rare examples of ursane triterpenoid glycosides containing a 28,19-lactone group.The structural characterization of these compounds was achieved using spectroscopic and chemical techniques,as well as single-crystal X-ray analysis.Compounds 7,12,15,and 17 exhibited moderate cytotoxic activities against H1975 and HCC827 cancer cells.
基金supported by the Scientific and Technological Innovation Project of the China Academy of Chinese Medical Sciences(CI2021A03807 and CI2021A01501)the National Natural Science Foundation of China(82330124)+2 种基金the Beijing Municipal Natural Science Foundation(7212186)the Innovation Team and Talents Cultivation Program of National Administration of Traditional Chinese Medicine(ZYYCXTD-C-202002)the Key Laboratory of Beijing for Identification and Safety Evaluation of Chinese Medicine,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences.
文摘Rheumatoid arthritis(RA),a globally increasing autoimmune disorder,is associated with increased disability rates due to the disruption of iron metabolism.Tripterygium glycoside tablets(TGTs),a Tripterygium wilfordii Hook.f.(TwHF)-based therapy,exhibit satisfactory clinical efficacy for RA treatment.However,drug-induced liver injury(DILI)remains a critical issue that hinders the clinical application of TGTs,and the molecular mechanisms underlying the efficacy and toxicity of TGTs in RA have not been fully elucidated.To address this problem,we integrated clinical multi-omics data associated with the anti-RA efficacy and DILI of TGTs with the chemical and target profiling of TGTs to perform a systematic network analysis.Subsequently,we identified effective and toxic targets following experimental validation in a collagen-induced arthritis(CIA)mouse model.Significantly different transcriptome–protein–metabolite profiles distinguishing patients with favorable TGTs responses from those with poor outcomes were identified.Intriguingly,the clinical efficacy and DILI of TGTs against RA were associated with metabolic homeostasis between iron and bone and between iron and lipids,respectively.Particularly,the signal transducer and activator of transcription 3(STAT3)–hepcidin(HAMP)/lipocalin 2(LCN2)–tartrate-resis tant acid phosphatase type 5(ACP5)and STAT3–HAMP–acyl-CoA synthetase long-chain family member 4(ACSL4)–lysophosphatidylcholine acyltransferase 3(LPCAT3)axes were identified as key drivers of the efficacy and toxicity of TGTs.TGTs play dual roles in ameliorating CIA-induced pathology and in inducing hepatic dysfunction,disruption of lipid metabolism,and hepatic lipid peroxidation.Notably,TGTs effectively reversed“iron–bone”disruptions in the inflamed joint tissues of CIA mice by inhibiting the STAT3–HAMP/LCN2–ACP5 axis,subsequently leading to“iron–lipid”disturbances in the liver tissues via modulation of the STAT3–HAMP–ACSL4–LPCAT3 axis.Additional bidirectional validation experiments were conducted using MH7A and AML12 cells to confirm the bidirectional regulatory effects of TGTs on key targets.Collectively,our data highlight the association between iron-mediated metabolic homeostasis and the clinical efficacy and toxicity of TGT in RA therapy,offering guidance for the rational clinical use of TwHF-based therapy with dual therapeutic and toxic potential.
基金supported by the National Natural Science Foundation of China(Nos.31960090 and 32160562)the State Key Laboratory of Food Science and Resources,Nanchang University(No.SKLF-ZZB-202129)。
文摘Ten previously undescribed dammarane-type triterpenoid glycosides,cyclocarysaponins A–J(1–10),were isolated from the leaves of Cyclocarya paliurus(Batal.)Iljinskaja.The structures of these compounds were characterized through detailed spectroscopic analysis,including 1D and 2D nuclear magnetic resonance(NMR)and high-resolution electrospray ionization mass spectrometry(HR-ESI-MS).The cytotoxic activities of all isolates were assessed against five human cancer cell lines(Bel-7402,Caski,BGC-823,A2780,and HCT-116).Of the tested compounds,compounds 1,7,and 9 exhibited selective cytotoxicity against one or more human cancer cell lines.
基金Supported by Youth Fund Project of Zhaoqing University(QZ202235)Zhaoqing Science and Technology Plan Project(2022040311011).
文摘[Objectives]To study the inhibitory activity of two flavonoid glycosides isolated from Chlorophytum comosum Laxum R.Br on human nasopharyngeal carcinoma(NPC)cell line 5-8F in vitro and its mechanism.[Methods]The flavonoid glycosides were isolated and purified from the ethanol alcoholic extract of the roots of Liliaceae plant Chlorophytum comosum by silica gel column chromatography,macroporous resin column chromatography,Sephadex LH-20,and reverse column chromatography(ODS).The inhibitory activity of flavonoid glycosides on human nasopharyngeal carcinoma cells was analyzed by CCK-8 method,and the potential mechanism was preliminarily analyzed by molecular docking.[Results]Two flavonoid glycosides were identified as isovitexin 2″-0-rhamnoside and 7-2″-di-O-β-glucopyranosylisovitexin.Two flavonoid glycosides showed promising inhibitory effect on human nasopharyngeal carcinoma cell line 5-8F,with IC_(50) values of 24.8 and 27.5μmol/L,respectively.Molecular docking results showed that the potential targets of two flavonoid glycosides include CyclinD1,Bcl-2β-Catenin,ILK,TGF-β,in addition,two glycosides showed higher predicted binding affinity towards CyclinD1,which verifies the cytotoxicity of the two compounds on human nasopharyngeal carcinoma cell line 5-8F in vitro.[Conclusions]Two flavonoid glycosides are the active molecules in Chlorophytum comosum that can inhibit the proliferation of human nasopharyngeal carcinoma cells,and have the potential to be used in the research and development of anti nasopharyngeal carcinoma drugs.
基金supported by the National Natural Science Foundation of China(Nos.82141203,82003624,82004003,82004215)the Science and Technology Commission of Shanghai Municipality(Nos.20YF1458700,20YF1459000)+1 种基金the Innovation Team and Talents Cultivation Program of National Administration of Traditional Chinese Medicine(No.ZYYCXTDD-202004)Shanghai Frontiers Science Center of TCM Chemical Biology,Shanghai Engineering Research Center for the Preparation of Bioactive Natural Products(No.16DZ2280200).
文摘Our continued works on the chemical constituents of Ginkgo biloba(G.biloba)leaves has led to the isolation of two novel phenylbutenoids(1,2),along with five previously unidentified terpene glycosides(3−7).Among them,compounds 1 and 2 represent unique(Z)-phenylbutenoids,3−6 are megastigmane glycosides,and 7 is identified as a rare bilobanone glycoside(Fig.1).This study marks the first reported isolation of phenylbutenoid and bilobanone glycoside from G.biloba.The chemical structures of these compounds were elucidated through extensive spectroscopic analysis,including HR-ESI-MS and various 1D and 2D NMR experiments.Furthermore,the absolute configurations of these molecules were determined using Mosher’s method,ECD experiments,and Cu-KαX-ray crystallographic analyses.
文摘Introduction The plants of genus Cistanche G. Beck, which belong to Orobanchaceae family, include about twenty species, and there are four species and one variety are distributed in the northwest part of China. The dried fleshy stem of Cistanche genus plant known as ＇Roucongrong＇ in Chinese traditional medicine, has long been used for kidney deficiency, female infertility, morbid leucorrhea, and neurasthenia. Studies on active components and pharmacological activities show that it possesses significant activities in enhancing potency, anti-fatigue, immuno-modulability, etc, and phenylethanoid glycosides are the major active components. Due to excessive exploitation, its natural resources are facing with exhaustion. In order to improve this situation, the plant has been cultivated on a large scale in the northwest part of China. Up to now, the chemical investigations of the cultivated Cistartcbe salsa have not been undertaken. In this paper we report seven phenylethanoid glycosides from the cultivated Cistanche salsa： echinacoside （1）, cistanoside A （2）, acteoside （3）, isoacteoside （4）, 2＇-acetylacteoside （5）, tubuloside B （6）, and eutigoside A （7）. Among them, compound 7 isolated fronl family Orobanchaceae was reported previously, and compounds 1, 2, 3, 4, 5 and 6 from the cultivated Cistanche salsa are reported for the first time.
文摘Two new phenylpropanetriol glycosides, named as meliadanoside A (3 - methoxy- 5 - hydroxy-9- (1' - O-β-D-glucopyranosyl) - threo - phenylpropanetriol ) and meliadanoside B (4- hydroxy-7, 8- (2', 1' - O- β- D -glucopyranosyl) - phenylpropanetriol), were isolated from the water-soluble extract of the fruits of Meliatoosendan Sieb. et Zucc., along with threo-guaiacylglycerol. Their structures were elucidated by spectroscopic and chendcal analysis.
文摘Two new C 27 steroidal glycosides, named ophiopojaponin A (1) and B (2), together with two known ones, were isolated from the tubers of the famous traditional Chinese herb Ophiopogon japonicus Ker_Gawl. The spectroscopic and chemical evidence revealed their structures to be pennogenin 3_O_[2′_O_acetyl_α_L_rhamnopyranosyl (1→2)]_β_D_xylopyranosyl (1→3)_β_D_glucopyranoside (1), 26_O_β_D_glucopyranosyl_(22ξ, 25R)_3β, 14α, 22ξ, 26_tetrahydroxyfurost_5_ene 3_O_α_L_rhamnopyranosyl (1→2)_β_D_glucopyranoside (2), diosgenin 3_O_[α_L_rhamnopyranosyl (1→2)]_β_D_xylopyrano_syl (1→3)_β_D_glucopyranoside (3) and ruscogenin 1_O_[α_L_rhamnopyranosyl (1→2)]_β_D_xylopyranosyl (1→3)_β_D_fucopyranoside (4).
文摘Three new phenolic glycosides, named as equisetumoside A (3-methoxy-11,12-dihydroxy-phenylhexane-9- one-4-O-beta -D-glucopyranoside), equisetumoside B (3-methoxy-4,11-dihydroxy-phenylhexane-9-one12-O-beta -D-glucopyranoside) and equisetumoside C ( cis-ferulic acid potassium salt 4-O-beta -D-glucopyranoside) were isolated from the water-soluble extract of fertile sprouts of Equisetum, arvense L. (Equisetaceae), together with uridine, inosine, 2'-deoxyinosine, 2'-deoxycytidine, tryptophan, thymidine, 5-carboxy-2'-deoxyuridine, coniferin, and kaempferol 3-O-beta -D-sophoroside-7-O-beta -D-glucopyranoside. Their structures were elucidated by spectroscopic analysis and chemical transformation.
基金National Sciences and Technology Program of China (Grant No. 2011BAI07B08,2006BAI06A01-02,2006BAI08B03-09)
文摘A reversed-phase high-performance liquid chromatography （RP-HPLC） method with diode array detector was established to simultaneously determine nine bioactive compounds in Wuzhuyu decoction, namely dehydroevodiamine, isorhanmetin-7-O- rutinoside, 10-hydroxyrutaecarpine, diosmetin-7-O-13-D-glucopyranoside, evodiamine, rutaecarpine, 1-metbyl-2-n-nonyl-4（1H） quinolone, evocarpine, and dihydroevocarpine. The RP-HPLC assay was performed on a reversed-phase Cl8 column with a gradient elution. The mobile phases consisted of methanol and water containing 1% （v/v） acetic acid. The flow rate was 1.0 mL/min and the detection wavelength was set at 300 nm. All calibration curves showed good linearity （r2〉0.9941） within test ranges. The results of intra-day precision, inter-day precision, and accuracy were satisfactory. The overall recoveries were in the range of 90.13%-102.48%. The method was successfully applied to quantify nine bioactive compounds in six samples. Baseline resolution for all nine major compounds was achieved. This method could be used as a suitable quality control assay for Wuzhuyu decoction.
文摘Two new alkaloids,hordenine-O- -L-rhamnopyranoside(Ⅰ)and hordenine -0-(6′-trans-cinnamoyl)-4′-O-β-D-glucopyranosyl- -L-rhamnopyranoside(Ⅲ) isolated from Selaginella doederleinii have been synthesized the first time. A new method,in which trifluoroacetoxyl group was used both as a good leaving group and a protecting group for synthesis of O-glycosides with high stereo- selectivity was reported.
基金Natural Science Foundation of Hebei Province of China(Grant No.C2011206158,08B031)Hundreds of Innovative Talents Project of Hebei Education Department of China
文摘A simple, sensitive and specific high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）method combined with solid phase extraction has been developed and validated for the simultaneous quantification of paeoniflorinand albiflorin in rats plasma and tissue homogenate after administration of total glycosides of paeony （TGP）. Chromatographicseparation was achieved on a C15 column （150 mmx4.6 mm, 5 pro） with mobile phase consisted of acetonitrile-0.05% formicacid aqueous （20： 80, v/v） at a flow rate of 0.5 mL/min. The analytes were detected with triple-quadrupole mass spectrometer usingturbo ion spray with negative ionization in the multiple reaction-monitoring （MRM） modes. The results of method validationconformed to the requirements for the determination of biological samples. This method was successfully applied to thepharmacokinetics and tissue distribution study of TGP in rats. The results showed that paeonifiorin and albiflorin wereabsorbed and reached peak value quickly, and had the similar pharmacokinetic characteristics. Both of them underwent a rapid andwide distribution in the tissues throughout the whole body, among which stomach was the main distribution tissue. Moreover, theyhad the ability to cross the blood-brain barrier.
基金National Natural Science Foundation of China(Grant No.81222054)the Program for New Century Excellent Talents in University from Chinese Ministry of Education(Grant No.NCET-11-0019)Chinese Pharmacopoeia Commission
文摘Monoterpene glycosides are the major bioactive compounds of Paeonia lactiflora Pall（P. lactiflora）. Characteristic neutral loss of 30 Da has been extensively reported for monoterpene glycosides in tandem mass spectrometry. However, little is known about mechanism of this fragmentation. The neutral loss of 30 Da was studied for eleven monoterpene glycosides（1–11） from P. lactiflora by ion trap mass spectrometry in this report. Compounds 1–5 with a hemiacetal structure could readily lose 30 Da at low collision energy of 30% in MS/MS by ion trap mass spectrometry. For compounds 6–11, neutral loss of 30 Da could also be observed at low abundance, but the collision energy had to be increased to 60%. In both cases, high-accuracy mass spectrometry assigned the 30 Da as CH_2O. After careful analysis of the structures and mass spectra, we believe that the neutral loss of 30 Da in compounds 1–5 was due to cleavage of the hemiacetal structure, whereas it was ascribed to the cleavage of 5＇-hydroxymethyl group of the glucosyl residue in other monoterpene glycosides. Furthermore, the characteristic neutral loss of 30 Da at low collision energy was used to screen hemiacetals from crude extracts of P. lactiflora and related plant species. Significant differences among Paeonia species were observed by 30 Da neutral loss analysis.
文摘Abstract： In the present study, we established an ultra performance liquid chromatography coupled with time-of-flight mass spectrometry （UPLC-QTOF-MSE） method to simultaneously quantify 33 components in Ginkgo biloba leaf extracts （GBEs）, including 17 flavonol glycosides, five terpene trilactones （TTLs）, four polyphenols and seven carboxylic acids. This optimized method was successfully applied to analyze the explicit compositions of GBE samples collected from different places. Furthermore, the data were processed through unsupervised principal component analysis （PCA） and supervised orthogonal partial least squared discrimination analysis （OPLS-DA） to evaluate the quality and compare the differences between the samples according to the contents of the 33 chemical constituents. Bilobalide, protocatechuic acid, shikimic acid, quinic acid, ginkgolide B, ginkgolide J, kaempferol-3-O-rutinoside, isorhamnetin-3-O-rutinoside, quercetin-3-O-ct-L-rhamnopyranocyl-2＂-（6＇＂-p-coumaroyl）-β-D-glucoside and rutin were recognized as characteristic chemical markers that contributed most to control the quality of GBEs. Based on the fact that GBEs should be standardized with the characteristic components as quality control chemical markers, it is most important to maintain the quality of GBEs stable and reliable, and this method also provided a good strategy to further rectify and standardize the GBEs market.
文摘Two new stilbene glycosides (1 and 2), together with nine known compounds (3-11), were isolated from the water extract of Polygonum multiflorum Thunb. The structures of the new compounds were elucidated by their chemical properties and spectroscopic analyses, including extensive 2D NMR experiments. Compound 2 showed strong DNA cleavage activity, and compounds 1, 2 and 10 (2, 3, 4′, 5_tetrahydroxy_ trans _stilbene_2_O_β_ D _glucopyranoside) exhibited significant inhibition of lipid peroxidation.
基金supported by the Natural Science Foundation of Shanghai City,China(No.10411969800)the National Nature Science Foundation of China(Nos.81202866 and 81302856)
文摘AIM: To develop and validate a high performance liquid chromatography(HPLC) coupled with diode array and evaporative light scattering detectors(DAD-ELSD) method for the quantitative determination and fingerprint analysis of ten active constituents in three chemical classes(namely, xanthone glycosides, steroidal saponins, and alkaloids) in Zhimu-Huangbai herb pair(ZB). METHOD: Chromatographic separation was performed on a Diamonsil C18 column(4.6 mm × 250 mm, 5 μm, Dikma) by gradient elution using acetic acid in acetonitrile solution at a flow rate of 1.0 mL·min–1 at 260 nm. The drift tube temperature of ELSD was set to 60 ℃ and nebulizer gas pressure was 4.0 Bar. Method validation was performed to assure its linearity, limits of detection and quantification, precision, repeatability, stability, and accuracy. RESULTS: The HPLC-DAD-ELSD method allowed the quantification of ten compounds(phellodendrine, jatrorrhizine, palmatine, berberine, neomangiferin, mangiferin, timosaponin E-I, timosaponin B-II, timosaponin B, and timosaponin A-III), and was successfully applied to fingerprint analysis for ten batches of ZB samples. CONCLUSION: This was the first time to apply the combination of DAD and ELSD for the simultaneous determination of ten active ingredients in ZB. The results showed that the combination of quantitative analysis for marker ingredients and chemical fingerprint for the TCM herb pair provides a potentially powerful, widely introduced, and internationally accepted strategy for assessment of complex TCM formulas.
文摘Two new phenolic glycosides, 2,3-dihydroxybenzoic acid methyl ester 3-O-β-o-glucopyranosyl-（1-6）-β-D-glucopyranoside （1） and 2,5-dihydroxylbenzofuran 5-O-β-D-xylopyranosyl-（1-6）-O-β-D-glucopyranoside （2）, were isolated as the minor chemical constituents from the roots of Gentiana rigescens, along with 15 known compounds. Their structures were elucidated by detailed spectroscopic analysis, including 1D, 2D NMR and chemical method. All of these compounds were isolated for the first time from the title plant. Moreover, compounds 1 and 2 were tested for the antifungal activities on three plant pathogens Peronophythora litchi, Glomerella cingulata, and Glorosprium musarum.
