RESUMO
INTRODUCTION: Spirodela polyrrhiza (L.) Schleid. is a traditional Chinese herbal medicine for the treatment of influenza. Despite its wide use in Chinese medicine, no report on quality control of this herb is available so far. OBJECTIVE: To establish qualitative and quantitative analytical methods by high-performance liquid chromatography (HPLC) coupled with mass spectrometry (MS) for the quality control of S. polyrrhiza. METHODOLOGY: The methanol extract of S. polyrrhiza was analysed by HPLC/ESI-MS(n). Flavonoids were identified by comparing with reference standards or according to their MS(n) (n = 2-4) fragmentation behaviours. Based on LC/MS data, a standardised HPLC fingerprint was established by analysing 15 batches of commercial herbal samples. Furthermore, quantitative analysis was conducted by determining five major flavonoids, namely luteolin 8-C-glucoside, apigenin 8-C-glucoside, luteolin 7-O-glucoside, apigenin 7-O-glucoside and luteolin. RESULTS: A total of 18 flavonoids were identified by LC/MS, and 14 of them were reported from this herb for the first time. The HPLC fingerprints contained 10 common peaks, and could differentiate good quality batches from counterfeits. The total contents of five major flavonoids in S. polyrrhiza varied significantly from 4.28 to 19.87 mg/g. CONCLUSION: Qualitative LC/MS and quantitative HPLC analytical methods were established for the comprehensive quality control of S. polyrrhiza.
Assuntos
Araceae/química , Flavonoides/análise , Espectrometria de Massas por Ionização por Electrospray/métodos , Apigenina/análise , Apigenina/química , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida de Alta Pressão/normas , Medicamentos de Ervas Chinesas/análise , Medicamentos de Ervas Chinesas/química , Flavonas/análise , Flavonas/química , Flavonoides/química , Glucosídeos/análise , Glucosídeos/química , Estrutura Molecular , Controle de Qualidade , Espectrometria de Massas por Ionização por Electrospray/normasRESUMO
Two new lignan glycosides, 2'-hydroxyl asarinin 2'-O-ß-D-glucopyranoside (cuscutoside C, 1) and 2'-hydroxyl asarinin 2'-O-ß-D-apiofuranosyl-(1 â 2)-[ß-D-glucopyranosyl-(1 â 6)]-ß-D-glucopyranoside (cuscutoside D, 2), were isolated from the seeds of Cuscuta chinensis Lam., along with six known compounds, 2'-hydroxyl asarinin 2'-O-ß-D-glucopyranosyl-(1 â 6)-ß-D-glucopyranoside (3), 2'-hydroxyl asarinin 2'-O-ß-D-apiofuranosyl-(1 â 2)-ß-D-glucopyranoside (cuscutoside A, 4), kaempferol 3,7-di-O-ß-D-glucopyranoside (5), 5-caffeoyl quinic acid (6), 4-caffeoyl quinic acid (7), and cinnamic acid (8). Their structures were elucidated on the basis of spectroscopic analyses including HR-ESI-MS, ESI-MS/MS, (1)H and (13)C NMR, HSQC, HMBC, and TOCSY.
Assuntos
Cuscuta/química , Medicamentos de Ervas Chinesas/isolamento & purificação , Glicosídeos/isolamento & purificação , Lignanas/isolamento & purificação , Medicamentos de Ervas Chinesas/química , Glicosídeos/química , Lignanas/química , Estrutura Molecular , Ressonância Magnética Nuclear Biomolecular , Sementes/química , EstereoisomerismoRESUMO
Asiatic acid is a major pentacyclic triterpene isolated from Centella asiatica. It shows a variety of bioactivities. In order to obtain its derivatives, potentially useful for detailed pharmacological studies, the substrate was subjected to incubations with selected micro-organisms. In this work, asiatic acid was converted into three new compounds: 2α,3ß,23,30-tetrahydroxyurs-12-ene-28-oic acid (1), 2α,3ß,22ß,23-tetrahydroxyurs-12-ene-28-oic acid (2), and 2α,3ß,22ß,23,30-pentahydroxyurs-12-ene-28-oic acid (3) by the fungus Alternaria longipes AS 3.2875. The structures of the three metabolites were determined by 1D and 2D NMR spectral data.
Assuntos
Alternaria/metabolismo , Triterpenos Pentacíclicos/metabolismo , Biotransformação , Centella/química , Estrutura Molecular , Ressonância Magnética Nuclear Biomolecular , Triterpenos Pentacíclicos/química , Plantas Medicinais/química , EstereoisomerismoRESUMO
New TLC, HPLC and LC/MS methods were developed for the rapid separation, characterization and quantitation of thiophenes in Radix Echinopsis, a herbal medicine, which has been used in China for long history. Nineteen commercial batches of this herb were analyzed by TLC and HPLC. Only five batches were derived from correct species. The other 14 batches were identified as its adulterating species, Radix Rhapontici, as they did not contain characteristic thiophenes of Echinopsis species. By LC/MS, 16 thiophenes were identified from the methanol extracts of Radix Echinopsis and Radix Rhapontici according to their fragmentation behaviors in MS/MS. In addition, a fully validated HPLC method was established to determine the contents of alpha-terthienyl in Radix Echinopsis. The contents ranged from 2.7 to 5.2 mg/g for five tested samples. The methods in this paper were simple and reliable, and could be used for the comprehensive quality control of Radix Echinopsis.