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1.
Steroids ; 156: 108587, 2020 Jan 23.
Artigo em Inglês | MEDLINE | ID: mdl-31982423

RESUMO

A phytochemical study on the rhizomes of Trillium tschonoskii led to the isolation of fourteen new steroidal saponins, trillitschosides S1-S14 (1-14), along with ten known analogues (15-24). Their structures were established mainly by spectroscopic analyses as well as necessary chemical evidence. All isolated compounds were screened for the cytotoxicity against HepG2 cells, and the results demonstrated that only the known compounds 21-24 exhibited the remarkable cytotoxic activity against HepG2 cells which is much better than the positive control of 5-FU.

2.
Zhongguo Zhong Yao Za Zhi ; 44(15): 3297-3304, 2019 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-31602886

RESUMO

The contents of terrestroside B and terrestrosin K in Tribuli Fructus with different degree of stir-frying were determined by high performance liquid chromatography with evaporative light-scattering detector( HPLC-ELSD). The results showed that the contents of terrestroside B and terrestrosin K were increased at first and then decreased,and both of them had the highest content at the best time of heating. The results of simulated processing of Tribulus Terrestris saponins showed that when the processing time kept constant,the contents of terrestroside B and terrestrosin K were decreased gradually with the increase of processing temperature from 180 ℃ to240 ℃. At a certain temperature,the content of terrestrosin K was increased first and then decreased with the prolongation of processing time,and reached the highest level at 5 min. However,the content of terrestroside B was increased first and then decreased with the increase of processing time only at 180 ℃,and reached the highest level at 10 min. When the processing temperature was controlled at200,220 and 240 ℃ respectively,the content of terrestroside B was decreased gradually with the increase of processing time. The simulated processing products of tribuluside A,terrestroside B and terrestrosin K were qualitatively characterized by ultra-performance liquid chromatography-time of flight mass spectrometry( UPLC-TOF/MS). It was proved that tribuluside A and terrestrosin Ⅰ containing C-22-OH were dehydroxylated in the processing of Tribuli Fructus and transformed respectively into terrestroside B and terrestrosin K containing C-20-C-22 double bond. As a result,the contents of terrestroside B and terrestrosin K were increased. The sugar chains at C-3 and C-26 positions of terrestroside B and terrestrosin K could be deglycosylated and converted into monosaccharide chain saponins and short sugar chain saponins,so the contents of terrestroside B and terrestrosin K were reduced. The study provides reference for further revealing the processing principle of Tribuli Fructus.


Assuntos
Medicamentos de Ervas Chinesas/análise , Saponinas/análise , Tribulus/química , Química Farmacêutica , Cromatografia Líquida de Alta Pressão , Frutas/química , Espectrometria de Massas em Tandem
3.
Zhongguo Zhong Yao Za Zhi ; 44(9): 1857-1861, 2019 May.
Artigo em Chinês | MEDLINE | ID: mdl-31342713

RESUMO

The change of icariin( ICA) content in thirty-three samples of five Epimedium species listed in the Chinese Pharmacopoeia( 2015 edition),including E. brevicornu,E. sagittatum,E. pubescens,E. koreanum,and E. wushanense has been investigated in this study. The results indicated that the optimized process procedure was baking at 150 ℃ for 30 min,and 3'''-carbonyl-2″-ß-L-quinovosyl icariin( CQICA) could not be translated into ICA and ICA could be converted under this heating process condition. ICA increased remarkably after the heating process by 1-3 times in E. brevicornu,E. wushanense and E. koreanum,and increased lightly in E. brevicornum and E. pubescens,while ICA slightly increased or decreased in E. sagittatum and E. wushanense.


Assuntos
Medicamentos de Ervas Chinesas/química , Epimedium/química , Flavonoides/análise , Temperatura Alta , Compostos Fitoquímicos/análise , Manejo de Espécimes
4.
Zhongguo Zhong Yao Za Zhi ; 44(12): 2552-2558, 2019 Jun.
Artigo em Chinês | MEDLINE | ID: mdl-31359723

RESUMO

This study aimed to comprehensively assess the difference of alkaloid components between old stems and tender stems of Gelsemium elegans by using ultra high-performance liquid chromatography coupled with photo-diode array and quadrupole time-of-flight mass spectrometry( UPLC-Q-TOF/MS~E) and high-performance liquid chromatography coupled with UV detector( HPLC-UV). Firstly,the different components in old stems and tender stems were analyzed by UHPLC-Q-TOF/MSEcombined with principal component analysis( PCA) and orthogonal partial least squares discriminant analysis( OPLS-DA),respectively. As a result,17 major different components were found. At the same time,the distribution of these alkaloids in old stems and tender stems was determined,and the alkaloids with higher polarity are relatively higher in the tender stems,while the old stems are in the opposite case. In addition,three main components in the G. elegans were quantified by HPLC-UV. The results showed that the contents of koumine and humantenmine in old stems were higher than those in tender stems,and the content of gelsemine in tender stems was relatively high. This study systematically evaluated the differences of alkaloids between the old stems and tender stems of G. elegans,and quantified the main three alkaloids. It laid the foundation of the safe and effective application of G. elegans.


Assuntos
Alcaloides/análise , Gelsemium/química , Caules de Planta/química , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas , Extratos Vegetais
5.
Zhongguo Zhong Yao Za Zhi ; 44(2): 332-337, 2019 Jan.
Artigo em Chinês | MEDLINE | ID: mdl-30989954

RESUMO

UPLC-Q-TOF-MS was used to analyze the chemical differences in Bupleurum. chinense,B. marginatum,B. marginatum var. stenophyllum and B. smithii var. parvifolium. Chromatographic separation was carried out on an Acquity HSS T3 C_(18) column( 2. 1 mm ×100 mm,1. 8 µm,Waters) with the mobile phase composed of 0. 1% formic acid in water-acetonitrile in the gradient elution. A hybrid quadrupole time-of-flight tandem mass spectrometry( Q-TOF-MS~E) was used for mass spectrometric analysis. Finally,25 peaks were identified based on their exact mass data and fragmentation characteristics. B.chinense,B.marginatum,B. marginatum var. stenophyllum and B. smithii var. parvifolium were obviously clustered into 3 types through processing by principal component analysis( PCA). There was almost no difference between B. chinense and B. marginatum. However,the compounds existed in B. chinense were different from those in B. marginatum var. stenophyllum,and B. smithii var. parvifolium.


Assuntos
Bupleurum/química , Bupleurum/classificação , Medicamentos de Ervas Chinesas/química , Compostos Fitoquímicos/análise , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas em Tandem
6.
Int J Syst Evol Microbiol ; 68(5): 1578-1583, 2018 May.
Artigo em Inglês | MEDLINE | ID: mdl-29547096

RESUMO

Three actinomycete strains originating from the surface-sterilized roots of Paris polyphylla were characterized by using a polyphasic approach. Phylogenetic analyses based on the 16S rRNA gene sequence showed that they formed a deep, monophyletic branch in the genus Glycomyces, and were most closely related to the type strains of the species Glycomyces harbinensis and Glycomycesscopariae. Morphological and chemotaxonomic data supported the affiliation of strains CPCC 204357T, CPCC 204354 and CPCC 204355 to the genus Glycomyces. The results of physiological and biochemical tests allowed phenotypic differentiation of strains CPCC 204357T, CPCC 204354 and CPCC 204355 from their closest phylogenetic related species in the genus Glycomyces. Low levels of DNA-DNA relatedness with its closest type strains of G. harbinensis and G. scopariaeindicated that strain CPCC 204357T represent a novel species, for which the name Glycomyces paridis sp. nov. is proposed, with CPCC 204357T (=DSM 102295T=KCTC 39745T) as the type strain.


Assuntos
Actinomycetales/classificação , Melanthiaceae/microbiologia , Filogenia , Raízes de Plantas/microbiologia , Actinomycetales/genética , Actinomycetales/isolamento & purificação , Técnicas de Tipagem Bacteriana , Composição de Bases , China , DNA Bacteriano/genética , Ácidos Graxos/química , Hibridização de Ácido Nucleico , Fosfolipídeos/química , Plantas Medicinais/microbiologia , RNA Ribossômico 16S/genética , Análise de Sequência de DNA , Ubiquinona/química
7.
J Asian Nat Prod Res ; 20(8): 770-780, 2018 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-29110541

RESUMO

Three new minor oleanane triterpenoid saponins, cylindrosides B (1), C (2), and D (3), were isolated from the seed of Cylindrokelupha dalatensis using chromatographic method. Their structures were established on the basis of the chemical and spectroscopic evidences. They displayed significant antitumor activity in vitro against HL60 cancer cell lines and IC50 values were 7.15 ± 0.63, 10.07 ± 0.97, and 4.74 ± 0.57 µM, respectively, by MTT method.


Assuntos
Antineoplásicos Fitogênicos/química , Antineoplásicos Fitogênicos/farmacologia , Plantas Medicinais/química , Saponinas/química , Saponinas/farmacologia , Triterpenos/química , Triterpenos/farmacologia , Ensaios de Seleção de Medicamentos Antitumorais , Medicamentos de Ervas Chinesas , Células HL-60 , Humanos , Espectroscopia de Ressonância Magnética , Modelos Moleculares , Espectrometria de Massas por Ionização por Electrospray
8.
J Nat Med ; 72(1): 166-180, 2018 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-28914410

RESUMO

Twenty-three new C21 steroidal glycosides, marstenacissides C1-C10 (1-10), D1-D7 (11-17) and E1-E6 (18-23), and four new C21 steroids, 11α,12ß-O-ditigloyl-tenacigenin C (24), 11α-O-benzoyl-12ß-O-tigloyl-tenacigenin C (25), 11α-O-tigloyl-12ß-O-benzoyl-tenacigenin C (26) and 11α-O-tigloyl-12ß-O-benzoyl-marsdenin (27), were isolated from the Dai herbal medicine Dai-Bai-Jie, derived from the roots of Marsdenia tenacissima. The chemical structures of all compounds were established by spectroscopic techniques, including high-resolution mass spectrometry and NMR spectroscopy, as well as by comparison with reported spectral data. The anti-HIV activities of these compounds were screened, and the compounds obtained displayed inhibitory effects against HIV-1 with inhibition rates of 36.4-81.3% at 30 µM.


Assuntos
Infecções por HIV/tratamento farmacológico , Medicina Herbária/métodos , Marsdenia/química , Fitoterapia/métodos , Raízes de Plantas/química , Plantas Medicinais/química
9.
Zhongguo Zhong Yao Za Zhi ; 42(18): 3530-3536, 2017 Sep.
Artigo em Chinês | MEDLINE | ID: mdl-29218938

RESUMO

Sulfur-containing Anemarrhenae Rhizoma decoction pieces were prepared by using sulfur-fumigating procedure. The difference components before and after sulfur fumigation in Anemarrhenae Rhizoma were analyzed and on-line identified by UPLC-Q-TOF-MSE combined with UNIFI informatics platform, principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) respectively. As a result, 16 major differences components were identified, and among them, 9 components were mainly from sulfur-fumigated samples. The main chemical markers in sulfur-fumigated Anemarrhenae Rhizoma were identified as the sulfite derivatives newly produced after sulfur-fumigating. Meanwhile, UPLC-Q-TOF-MSE was used to find the main chemical marker anemarrhena saponin BⅡ sulfite (m/z 983). By using this method, a rapid screening method for sulfur-fumigated Anemarrhenae Rhizoma was established. This was a convenient and accurate detection method for sulfur dioxide residue, and it can be used as an effective assistant method to control the quality of Anemarrhenae Rhizoma. At the same time, it was the first time to identify sulfited derivatives of steroidal saponins, and screen the sulfur-fumigated Anemarrhenae Rhizoma.


Assuntos
Anemarrhena/química , Medicamentos de Ervas Chinesas/química , Rizoma/química , Enxofre , Cromatografia Líquida de Alta Pressão , Fumigação , Compostos Fitoquímicos/análise , Saponinas/análise
10.
Zhongguo Zhong Yao Za Zhi ; 42(6): 1146-1151, 2017 Mar.
Artigo em Chinês | MEDLINE | ID: mdl-29027431

RESUMO

To compare the differences of main components between in rhizoma and fibrous root of Trillium tschonoskii and T. kamtschaticum, a simple, accurate and reliable high performance liquid chromatography coupled with the charged aerosol detector (HPLC-CAD) method was developed and then successfully applied for simultaneous quantitative analysis of three compounds, including polyphyllin Ⅶ (T1),pennogenin 3-O-α-L-rhamnopyranosyl-(1→2) [α-L-rhamnopyranosyl-(1→4)]-ß-D-glucopyranoside (T2),polyphyllin Ⅵ (T3), in 16 batches of rhizome and 14 batches of fibrous root. The analytes were well separated from other constituents on TSK gel ODS (4.6 mm×250 mm, 5 µm) with acetonitrile-water (43∶57) at a flow rate of 1.0 mL•min⁻¹. The injection volume was 20 µL. The nitrogen inlet pressure for the CAD system was 35 psi and the nebulizer chamber temperature was 35 ℃.The method was validated for linearity (r>0.999 0), intra and inter-day precision (0.29%-3.0%), repeatability (0.45%-1.4%), stability (1.9%-2.6%), recovery (100.1%-100.2%, 1.2%-1.8%), limits of detection (0.002 g•L⁻¹), and limits of quantification (0.005 g•L⁻¹).The obtained datasets were processed by principal component analysis (PCA) and it showed that there was almost no difference in rhizoma of T. tschonoskii and T. kamtschaticum from different areas of China. However, the 3 major compounds existed in rhizoma were different from those in fibrous root of T. tschonoskii and T. kamtschaticum.


Assuntos
Rizoma/química , Saponinas/isolamento & purificação , Trillium/química , China , Cromatografia Líquida de Alta Pressão , Trillium/classificação
11.
Int J Syst Evol Microbiol ; 67(11): 4541-4545, 2017 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-28945533

RESUMO

A Gram-positive bacterium originating from the surface-sterilized leaf of Paris polyphylla var. yunnanensis (Franch.) was characterized by using a polyphasic approach. The isolate formed yellow, smooth, circular colonies on nutrient agar with 0.2 % starch (NSA). Cells were non-motile, non-sporulating, irregular rods or cocci. Strain CPCC 203535T had the highest 16S rRNA gene sequence similarity to the type strain of Ornithinimicrobium kibberense (96.9 %) and formed the deepest branch in the genus Ornithinimicrobium in the neighbour-joining (NJ) phylogenetic tree based on 16S rRNA gene sequences. The major menaquinones of strain CPCC 203535T were MK-8(H4), MK-8(H2) and MK-8. The peptidoglycan contained ornithine as the diagnostic diamino acid. The polar lipid profile consisted of diphosphatidylglycerol (DPG), phosphatidylglycerol (PG), phosphatidylinositol (PI) and unknown lipid (UL). The major fatty acids iso-C14 : 0, iso-C15 : 0, iso-C16 : 0 and anteiso-C15 : 0 were consistent with the fatty acid patterns reported for members of the genus Ornithinimicrobium. The DNA G+C composition is 71.4 mol%. The results of physiological and biochemical tests allowed phenotypic differentiation of strain CPCC 203535T from its closest phylogenetic species in the genus Ornithinimicrobium. Strain CPCC 203535T represents a novel species of the genus Ornithinimicrobium, for which the name Ornithinimicrobium flavum sp. nov. is proposed, with CPCC 203535T (=NBRC 109452 T=KCTC 29164T) as the type strain.


Assuntos
Actinomycetales/classificação , Liliaceae/microbiologia , Filogenia , Actinomycetales/genética , Actinomycetales/isolamento & purificação , Técnicas de Tipagem Bacteriana , Composição de Bases , Parede Celular/química , China , DNA Bacteriano/genética , Ácidos Graxos/química , Hibridização de Ácido Nucleico , Peptidoglicano/química , Fosfolipídeos/química , Folhas de Planta/microbiologia , RNA Ribossômico 16S/genética , Análise de Sequência de DNA , Vitamina K 2/análogos & derivados , Vitamina K 2/química
12.
Molecules ; 22(8)2017 Aug 02.
Artigo em Inglês | MEDLINE | ID: mdl-28767079

RESUMO

Three new sesquiterpene glycosides, possessing a rare aglycone with a sulfonyl between C-1 and C-15 positions, named 3-(3'E-7'R,8'-dihydroxy-4',8'-dimethyl-3'-nonenyl)-2,5-dihydro-1,1-dioxo-thiophen 7'-O-ß-d-glucopyranosyl-(1→4)-O-ß-d-glucopyranosyl-(1→4)-O-ß-d-glucopyranoside (1), 3-(3'E-7'R,8'-dihydroxy-4',8'-dimethyl-3'-nonenyl)-2,5-dihydro-1,1-dioxo-thiophen 7'-O-ß-d-glucopyranosyl-(1→4)-O-ß-d-glucopyranoside (2), and 3-(3'E-7'R,8'-dihydroxy-4',8'-dimethyl-3'-nonenyl)-2,5-dihydro-1,1-dioxo-thiophen 7'-O-ß-d-glucopyranosyl-6'-O-acetyl-(1→4)-O-ß-d-glucopyranosyl-(1→4)-O-ß-d-glucopyranoside (3), respectively, were isolated from the rhizomes of Trillium tschonoskii. Their structures were established on the basis of spectroscopic data, including HR-ESI-MS, IR, 1D and 2D NMR. The cytotoxic properties of the three compounds were investigated using human hepatic L02 cells.


Assuntos
Glicosídeos/química , Rizoma/química , Sesquiterpenos/química , Trillium/química , Sobrevivência Celular/efeitos dos fármacos , Descoberta de Drogas , Glicosídeos/farmacologia , Glicosídeos/toxicidade , Hepatócitos/citologia , Hepatócitos/efeitos dos fármacos , Humanos , Espectroscopia de Ressonância Magnética , Estrutura Molecular , Extratos Vegetais/química , Sesquiterpenos/farmacologia , Sesquiterpenos/toxicidade , Espectrometria de Massas por Ionização por Electrospray
13.
Biomed Pharmacother ; 91: 890-898, 2017 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-28511342

RESUMO

The combined effect of Oroxylum indicum seed extracts (OISE) or major flavonoids from OISE and acarbose on reducing postprandial blood glucose (PBG) levels was investigated in vitro and in vivo. In vitro, the IC50 values of OISE and baicalein against α-glucosidase were 43.4±0.731µgmL-1 and 25.9±0.412µgmL-1 respectively. A combination of acarbose with OISE or baicalein synergistically inhibited rat intestinal α-glucosidase. The combination index (CI) values for acarbose with OISE ranged from 0.33 to 0.75, suggesting a synergistic but not additive effect. OISE was determined to be a non-competitive inhibitor of maltose-hydrolyzing activity. In vivo, OISE were administered to normoglycemic and diabetic mice, either alone or in combination with acarbose. At doses between 50 and 200mgkg-1, OISE enhanced the efficacy of acarbose by up to 5-fold. These results demonstrated that OISE enhances the efficacy of acarbose in vivo, and that the combination of OISE and acarbose displayed a synergistic effect in vitro. Therefore, OISE can be used to design dietary supplements to treat diabetes.


Assuntos
Bignoniaceae/química , Glicemia/metabolismo , Flavonoides/farmacologia , Extratos Vegetais/farmacologia , Sementes/química , 1-Desoxinojirimicina/análogos & derivados , 1-Desoxinojirimicina/farmacologia , Acarbose/farmacologia , Animais , Sinergismo Farmacológico , Flavanonas/farmacologia , Hipoglicemiantes/farmacologia , Intestinos/enzimologia , Masculino , Camundongos , Pâncreas/enzimologia , Período Pós-Prandial/efeitos dos fármacos , Ratos Sprague-Dawley , alfa-Amilases/antagonistas & inibidores , alfa-Amilases/metabolismo , alfa-Glucosidases/metabolismo
14.
Yao Xue Xue Bao ; 52(3): 456-61, 2017 Mar.
Artigo em Chinês | MEDLINE | ID: mdl-29979860

RESUMO

A new method was developed for the chromatographic fingerprint analysis of Toosendan Fructus by HPLC coupled with the charged aerosol detector (CAD) in the present study. Samples were well separated on an Agilent ZOBAX SB C18 column (4.6 mm × 250 mm, 5 µm) by gradient elution using acetonitrile and water containing 0.1 % formic acid (v/v) at the flow rate of 1.0 mL·min−1. The column temperature was 30 ℃ and the injection volume was 5 µL. The nitrogen inlet pressure of the charged aerosol detector (CAD) was 35 psi, and the nebulizer chamber temperature was 35 ℃. In addition, the method of the chromatographic fingerprints combined with multivariate statistical analysis was effective and reasonable lead to an accurate classification of 20 batches of samples from different locations. The results showed that 28 common peaks were observed in the fingerprint and the samples were classified into three clusters. The established method was well validated, and showed high precision, good repeatability, and satisfactory stability. It may serve in the quality control and evaluation of Toosendan Fructus.


Assuntos
Medicamentos de Ervas Chinesas/química , Melia/química , Cromatografia Líquida de Alta Pressão , Frutas/química , Controle de Qualidade
15.
Planta Med ; 83(1-02): 126-134, 2017 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-27272399

RESUMO

A continuous phytochemical study on the roots of Marsdenia tenacissima led to the isolation and identification of 13 new polyoxypregnane glycosides named marstenacissides B10-B17 (1, 2, 4, 7, 8, 11, 12, and 14) and marstenacissides A8-A12 (3, 9, 10, 13, and 15) in addition to two known polyoxypregnane glycosides marsdenosides M and L (5 and 6). Their structures were established by spectroscopic techniques and by comparison with the reported data in the literature. Moreover, the anti-HIV activities of these isolates and the previous isolated marstenacissides A1-A7 and B1-B9 were assessed, some of which exhibited slight or negligible effects against HIV-1.


Assuntos
Fármacos Anti-HIV/farmacologia , Medicamentos de Ervas Chinesas/química , Infecções por HIV/tratamento farmacológico , HIV-1/efeitos dos fármacos , Marsdenia/química , Saponinas/farmacologia , Fármacos Anti-HIV/química , Fármacos Anti-HIV/isolamento & purificação , Infecções por HIV/virologia , Medicina Tradicional Chinesa , Estrutura Molecular , Ressonância Magnética Nuclear Biomolecular , Raízes de Plantas/química , Caules de Planta/química , Saponinas/química , Saponinas/isolamento & purificação
16.
Int J Syst Evol Microbiol ; 67(4): 993-997, 2017 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-27959785

RESUMO

The taxonomic status of a novel bacterium, designated strain CPCC 100226T, isolated from a traditional Chinese medicinal herbal plant, Eucommia ulmoides Oliver, was characterized by using a polyphasic approach. The aerobic isolate formed pale white colonies on tryptic soy agar. Cells were Gram-stain-positive, rod-shaped, motile and endospore-forming. Chemotaxonomic investigations revealed the presence of meso-diaminopimelic acid as the diagnostic diamino acid, MK-7 as the predominant menaquinone, anteiso-C15 : 0, iso-C15 : 0, iso-C16 : 0 and C16 : 0 as the major fatty acids, and the strain had a phospholipid pattern of phosphatidylethanolamine, diphosphatidylglycerol, phosphatidylglycerol and unidentified aminophospholipids. Phylogenetic analysis based on the 16S rRNA gene sequence revealed that the isolate was closely related to Paenibacillus aestuarii DSM 23861T with 95.1 % similarity. The G+C content of the genomic DNA was 47.9 mol%. On the basis of the genotypic and phenotypic data, the isolate is considered to represent a novel species of the genus Paenibacillus. The name proposed for this taxon is Paenibacillus eucommiae sp. nov. with CPCC 100226T (=DSM 26048T=KCTC 33054T) as the type strain.


Assuntos
Eucommiaceae/microbiologia , Paenibacillus/classificação , Filogenia , Técnicas de Tipagem Bacteriana , Composição de Bases , DNA Bacteriano/genética , Ácido Diaminopimélico/química , Ácidos Graxos/química , Hibridização de Ácido Nucleico , Paenibacillus/genética , Paenibacillus/isolamento & purificação , Peptidoglicano/química , Fosfolipídeos/química , Plantas Medicinais/microbiologia , RNA Ribossômico 16S/genética , Análise de Sequência de DNA , Vitamina K 2/análogos & derivados , Vitamina K 2/química
17.
J Pharm Biomed Anal ; 129: 105-116, 2016 Sep 10.
Artigo em Inglês | MEDLINE | ID: mdl-27416524

RESUMO

An ultra high-performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry approach coupled with multivariate statistical analysis was established and applied to rapidly distinguish the chemical differences between fibrous root and rhizome of Anemarrhena asphodeloides. The datasets of tR-m/z pairs, ion intensity and sample code were processed by principal component analysis and orthogonal partial least squares discriminant analysis. Chemical markers could be identified based on their exact mass data, fragmentation characteristics, and retention times. And the new compounds among chemical markers could be isolated rapidly guided by the ultra high-performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry and their definitive structures would be further elucidated by NMR spectra. Using this approach, twenty-four markers were identified on line including nine new saponins and five new steroidal saponins of them were obtained in pure form. The study validated this proposed approach as a suitable method for identification of the chemical differences between various medicinal parts in order to expand medicinal parts and increase the utilization rate of resources.


Assuntos
Anemarrhena/química , Extratos Vegetais/análise , Extratos Vegetais/química , Raízes de Plantas/química , Rizoma/química , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida de Alta Pressão/normas , Análise Multivariada , Espectrometria de Massas em Tandem/normas
18.
PLoS One ; 11(3): e0150595, 2016.
Artigo em Inglês | MEDLINE | ID: mdl-26937954

RESUMO

Eleven new furostanol saponins, typaspidosides B-L (1-11), one new spirostanol saponin, typaspidoside M (12), and five known spirostanol saponins, 25S-atropuroside (13), neoaspidistrin (14), (25S)-pratioside D1 (15), 25S-aspidistrin (16) and 25S-neosibiricoside (17) were isolated from the rhizomes of Aspidistra typica Baill. The structures of the new compounds were established using 1D and 2D NMR (1H-1H COSY, HMQC, HMBC and ROESY) spectroscopy, high resolution mass spectrometry, and chemical methods. The aglycones of 1-3 (unusual furostanol saponins with opened E ring type), 9 and 10 (the methoxyl substituent at C-23 position) were found, identified from natural products for the first time. Moreover, the anti-HIV activities of the isolated steroidal glycosides were assessed, and compounds 13, 14, 16 and 17 exhibited high active against HIV-1.


Assuntos
Fármacos Anti-HIV/farmacologia , HIV-1/efeitos dos fármacos , Liliaceae/química , Vírus Reordenados/efeitos dos fármacos , Rizoma/química , Saponinas/farmacologia , Esteróis/farmacologia , Fármacos Anti-HIV/isolamento & purificação , Proteínas do Capsídeo/antagonistas & inibidores , Proteínas do Capsídeo/genética , Proteínas do Capsídeo/metabolismo , Expressão Gênica , Genes Reporter , Células HEK293 , HIV-1/genética , HIV-1/crescimento & desenvolvimento , Humanos , Luciferases/antagonistas & inibidores , Luciferases/genética , Luciferases/metabolismo , Espectroscopia de Ressonância Magnética , Extratos Vegetais/química , Vírus Reordenados/genética , Vírus Reordenados/crescimento & desenvolvimento , Saponinas/isolamento & purificação , Espirostanos/isolamento & purificação , Espirostanos/farmacologia , Esteroides/isolamento & purificação , Esteroides/farmacologia , Esteróis/isolamento & purificação , Relação Estrutura-Atividade , Vesiculovirus/genética , Replicação Viral/efeitos dos fármacos
19.
J Pharm Biomed Anal ; 120: 72-8, 2016 Feb 20.
Artigo em Inglês | MEDLINE | ID: mdl-26707085

RESUMO

Spirostanol saponins are important active components of some herb medicines, and their isolation and purification are crucial for the research and development of traditional Chinese medicines. We aimed to compare the separation of spirostanol saponins by ultra-high performance supercritical fluid chromatography (UHPSFC) and ultra-high performance liquid chromatography (UHPLC). Four groups of spirostanol saponins were separated respectively by UHPSFC and UHPLC. After optimization, UHPSFC was performed with a HSS C18 SB column or a Diol column and with methanol as the co-solvent. A BEH C18 column and mobile phase containing water (with 0.1% formic acid) and acetonitrile were used in UHPLC. We found that UHPSFC could be performed automatically and quickly. It is effective in separating the spirostanol saponins which share the same aglycone and vary in sugar chains, and is very sensitive to the number and the position of hydroxyl groups in aglycones. However, the resolution of spirostanol saponins with different aglycones and the same sugar moiety by UHPSFC was not ideal and could be resolved by UHPLC instead. UHPLC is good at differentiating the variation in aglycones, and is influenced by double bonds in aglycones. Therefore, UHPLC and UHPSFC are complementary in separating spirostanol saponins. Considering the naturally produced spirostanol saponins in herb medicines are different both in aglycones and in sugar chains, a better separation can be achieved by combination of UHPLC and UHPSFC. UHPSFC is a powerful technique for improving the resolution when UHPLC cannot resolve a mixture of spirostanol saponins and vice versa.


Assuntos
Saponinas/química , Espirostanos/química , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia com Fluido Supercrítico/métodos , Metanol/química , Plantas Medicinais/química , Água/química
20.
J Asian Nat Prod Res ; 18(6): 520-7, 2016 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-26699736

RESUMO

A new sesquiterpenoid glycoside, cryptomeridiol 11-O-ß-d-xylopyranosyl-(1→6)-ß-d- glucopyranoside (1), two new phenylpropanoid glycosides, 3,4-dihydroxy-allylbenzene 3-O-ß-d-glucopyranosyl-4-O-ß-d-apiofuranosyl-(1→6)-ß-d-glucopyranoside (2), and 3,4,5-trihydroxy-allylbenzene 3-O-ß-d-glucopyranosyl-4-O-ß-d-glucopyranoside (3), along with four known phenylpropanoid glycosides (4-7), were isolated from the tuber of Ophiopogon japonicus. Compounds 4-7 were obtained from the genus Ophiopogon for the first time. Their structures were elucidated by spectroscopic methods, including 1D and 2D NMR and HR-ESI-MS.


Assuntos
Medicamentos de Ervas Chinesas/isolamento & purificação , Glicosídeos/isolamento & purificação , Ophiopogon/química , Fenilpropionatos/isolamento & purificação , Tubérculos/química , Sesquiterpenos/isolamento & purificação , Medicamentos de Ervas Chinesas/química , Glicosídeos/química , Estrutura Molecular , Ressonância Magnética Nuclear Biomolecular , Fenilpropionatos/química , Sesquiterpenos/química , Estereoisomerismo
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