ABSTRACT
Objective: To investigate the chemical constituents from the canes of Schisandra sphenanthera. Methods: The compounds were isolated and purified by chromatography on silica gel. Their structures were elucidated on the basis of spectroscopic methods, including MS, 1D, and 2D NMR spectral techniques. Results: Thirteen compounds were isolated from 95% ethanol extract in the canes of S. sphenanthera, including six lignans, six triterpenes, and one steroid and their structures were identified as sphendilactone (1), kadsulactone (2), schisanlactone E (3), 12-β-hydroxycoccinic acid (4), schizandronic acid (5), schisanbilactone A (6), β-sitosterol (7), meso-dihydroguaiaretic acid (8), deoxychizandrin (9), schizantherin A (10), schisanhenol B (11), γ-schizandrin (12), and R-(+)-angeloygomisin M1 (13). Conclusion: Among them, one new triterpene is named as sphendilactone (1). Schisanhenol B, deoxychizandrin, R-(+)-angeloygomisin M1, kadsulactone, schisanlactone E, 12β-hydroxycoccinic acid, and schisanbilactone A are isolated from this plant for the first time.
ABSTRACT
A qualitative analytical method of liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (HPLC-Q-TOF-MS) was developed for identification of multi-constituents and an analytical method was developed for simultaneously determining 4 major compounds (rutin, isoquercitrin, kaempferol-3-0-rutinoside, and astragalin) in Tetrastigma hemsleyanum Diels et Gilg. The HPLC-Q-TOF-MS assay was performed on a Welch Ultimate XB-C18 column (4.6 mm x 150 mm, 5 microm) with the mobile phase consisting of acetonitrile (A) and water containing 0.1% Formic acid (B) in gradient mode at a flow rate of 0.8 mL x min(-1). The column temperature was at 30 degrees C, and negative ion mode was used for TOF-MS. The UPLC-QqQ-MS assay was performed on a Waters CORTECS C18 (2.1 mm x 100 mm, 1.6 microm) with the mobile phase consisting of acetonitrile (A) and water containing 0.1% formic acid (B) in gradient mode at a flow rate of 0.25 mL x min(-1). The column temperature was at 45 degrees C, and MRM mode was used for QqQ-MS. Based on the retention time and MS spectra, 24 compounds were identified or tentatively characterized by comparing with reference substances or literatures. For quantitative the linear range of 4 detected compounds were good (r > 0.9966), and the overall recoveries ranged from 98.27% to 101.58%, with the RSD ranging from 3.15% to 5.88%. The results indicated that new approach conbined HPLC-Q-TOF-MS and UPLC-QqQ-MS was applicable in qualitative and quantitative quality control of Tetrastigma hemsleyanum.
Subject(s)
Acetonitriles , Chemistry , Chromatography, High Pressure Liquid , Methods , Formates , Chemistry , Tandem Mass Spectrometry , Methods , Vitaceae , Chemistry , Water , ChemistryABSTRACT
In this study, a rapid and sensitive analytical method was developed for the determination of 10 major compounds (procyanidin B1, catechin, procyanidin B2, rutin, isoquercitrin, kaempferol-3-O-rutinoside, astragalin, quercitrin, quercetin, and kaempferol) in Tetrastigma hemsleyanum by using ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (UPLC-MS/MS) in multiple-reaction monitoring (MRM) mode. UPLC-MS/MS assay with negative ion mode was performed on a Waters CORTECS C18 (2.1 mm x 100 mm, 1.6 μm) with the mobile phase consisting of acetonitrile (A) and 0.1% aqueous formic acid (B) in gradient elution at a flow rate of 0.25 mL · min(-1) and the column temperature was set at 45 °C. Under the optimized chromatographic conditions, good separation for 10 target compounds were obtained including chiral isomer procyanidins B1 and B2 were completely separated within 8.5 min. Satisfactory linearity was achieved with wide linear range and fine determination coefficient (r > 0.996 6), the overall recoveries were ranged from 95.44%-110.40% with the RSD ranging from 2.37%-8.69%. It is the first report about simultaneous analysis of 10 major flavonoids components in Tetrastigma hemsleyanum by using UPLC-MS/MS method, which affords highly sensitive, specific, speedy and efficient method for quality control of Tetrastigma hemsleyanum