ABSTRACT
Two undescribed terpene glycosides and two compounds were isolated from the n-butanol fraction of Alpiniae Oxyphyllae Fructus by using various chromatographic methods, including MCI Gel, Sephadex LH-20, ODS, silica gel and semi-preparative HPLC. The structures of the isolated compounds were identified by spectroscopy methods (1D, 2D NMR, UV, IR, MS, etc.), and the absolute configuration of the compound 1 was determined by ECD calculation and acid hydrolysis. Compounds 1 and 2 are new compound, and compounds 3 and 4 were isolated from Alpiniae Oxyphyllae Fructus for the first time.
ABSTRACT
Objective:To establish the Ultra-High Performance Liquid Chromatography (UPLC) characteristic chromatogram of different parts of Alpinia oxyphylla Miq., and to compare different parts of the chemical components based on multivariate statistical analysis. Methods:The UPLC was used to establish the fingerprint of Alpinia oxyphylla Miq. . The chromatograms were matched to generate the UPLC charactersistic chromatogram of different parts. Based on the variance analysis of single factor, combined with the Principal Component Analysis (PCA) ,Cluster Analysis (CA) and the Partial Orthogonal Least Square Discriminant Analysis (OPLS-DA) to analyze the differences of different medicinal parts of Alpinia oxyphylla Miq.. Results:16 common peaks of Alpinia oxyphylla Miq. were demarcated in crude drugs, compared with the medicinal materials of Alpinia oxyphylla Miq., the peak 13 (tectochhrysin) was lost in the decoction pieces, and the shell were missing peak 5 and peak 6. The results of PCA and CA showed that 15 batches of different medicinal parts of Alpinia oxyphylla Miq. can be broadly divided into 3 categories. The OPLS-DA result showed that the value of the peak area of peaks 14 (Nootkatone), 4, 7 and 12 were the main factors affecting the chemical composition of different parts of Alpinia oxyphylla Miq. .Conclusion:The fingerprint determination method established in this study is stable and controllable, which could distinguish the different parts of Alpinia oxyphylla Miq. .
ABSTRACT
Objective: To optimize the purification technology for flavone from Alpiniae Oxyphyllae Fructus (FAOF) with macroporous resins. Methods: Static and dynamic adsorption-desorption were used to select the best one from 15 different type macroporous resins; With the content of flavone as index, the purification technology parameters of flavone were optimized. Results: HP20 type resin showed the best purifying profile, its optimum technology conditions were as follows: sample injection concentration was 1.518 mg/mL, sample flow rate was 1.0 mL/min, quantity of adsorption was 50 mL, desorption rate was 1.0 mL/min, eluted by 6 BV 30% ethanol. Conclusion :The flavone could be isolated from Alpiniae Oxyphyllae Fructus by HP20 macroporous resins.
ABSTRACT
To establish the fingerprint of Alpiniae Oxyphyllae Fructus by UPLC. The chromatographic fingerprint was obtained with ACQUITY UPLC HSS T3 column (100 mm × 2.1 mm, 1.8 μm) and gradient eluted with acetonitrile and aqueous formic acid. The flow rate was 0.5 mL/min, the sample room temperature and the column temperature were maintained at 10℃ and 30℃, respectively. The detection wavelength was set at 254 nm. The injection volume was 2 μ L. The common mode of UPLC fingerprint of Alpiniae Oxyphyllae Fructus was set up firstly. There were 20 common peaks in the fingerprints. Protocatechuic acid, α-hydroxymethyl furfural, oxyphyllenodiol A, teuhetenone A, teuhetenone A, chrysin, kaempferide, tectochrysin, and nootkatone were identified by comparing the retention time and their ultraviolet spectra. The similarities of 15 Alpiniae Oxyphyllae Fructus among 19 batches of Alpiniae Oxyphyllae Fructus were above 0.970. The method is rapid and efficiency. It can be used for the quality evaluation of Alpiniae Oxyphyllae Fructus.