RESUMEN
Objective: To establish an HPLC-MS method for the simultaneous quantitation of neomangiferin, mangiferin, timosaponin E1, timosaponin BII, timosaponin BIII, anemarrhenasaponin I, timosaponin AIII, and timosaponin AII in Anemarrhenae Rhizoma, and to analyze the content change before and after salt processing. Methods: Chromatography was performed on Agilent SB-C18 (50 mm × 2.1 mm, 1.8 μm) column by gradient elution using 0.05% formic acid in water (A)-acetonitrile (B) at the flow rate of 0.4 mL/min. The column temperature was kept at 30 ℃ and the inject volume was 10 μL. HPLC-MS was used for quantification in negative ion mode under ESI. Results: The eight components had good linearity (r ≥ 0.9997) within the linear range. The average recovery rate was 97.55%-103.01% with RSD < 2.80%. The contents of the eight components in Anemarrhenae Rhizoma varied according to the different habits. The contents of mangiferin, timosaponin BII, and timosaponin AIII were high. After salt processing, contents of timosaponin E1, timosaponin BII, and anemarrhenasaponin I were reduced, content of timosaponin BIII was increased and contents of neomangiferin, mangiferin, timosaponin AIII, and timosaponin AII had no obvious changes. Conclusion: The changes of components in Anemarrhenae Rhizoma before and after salt processing are proved by the method of HPLC-MS which is simple, sensitive, and accurate.
RESUMEN
Objective: To provide the HPLC-ELSD fingerprint analysis method of Anemarrhenae Rhizoma, and to reflect and comprehensively control the quality of Anemarrhenae Rhizoma. Methods: The HPLC-ELSD separation was performed on a C8 analytical column (4.6 mm × 250 mm, 5 μm) gradient eluted with a mixture consisting of acetonitrile (A) and 0.2% acetic acid-water (B) at a flow rate of 1 mL/min with ELSD detector. Using a linear gradient of 0 min, 5% A; 5 min, 7% A; 5-15 min, 15% A; 15-36 min, 22% A; 36-43 min, 35% A; 43 min, 40% A; 51 min, 50% A; 51-60 min, 100% A. The temperature of column was 25 ℃. The flow rate of ELSD detector atomizer (air) was 2.6 mL/min. The temperature of the drift tube was 100 ℃ and the injection volume was 20 μL. Results: The fingerprint with better separation effect by using gradient elution method within 60 min was established, and also the 12 peak which are common peak were determined. The most of chemical components of Anemarrhenae Rhizoma were chromatographic separated in this HPLC-ELSD fingerprint. Conclusion: The method is simple and reliable, and in this way for the steroidal saponins and flavonoids of Anemarrhenae Rhizoma can be identified at the same time. Moreover, it can fully reflect the characteristics of the chemical composition of Anemarrhenae Rhizoma, therefore it can be used as an effective quality control method for Anemarrhenae Rhizoma.
RESUMEN
Neomangiferin, a natural C-glucosyl xanthone, has recently received a great deal of attention due to its multiple biological activities. In this study, a rapid and sensitive ultra-high performance liquid chroma-tography tandem mass spectrometry (UHPLC–MS/MS) method for the quantification of neomangiferin in rat plasma was developed. Using chloramphenicol as an internal standard (IS), plasma samples were subjected to a direct protein precipitation process using methanol (containing 0.05% formic acid). Quan-tification was performed by multiple reactions monitoring (MRM) method, with the transitions of the parent ions to the product ions of m/z 583.1-330.9 for NG and m/z 321.1-151.9 for IS. The assay was shown to be linear over the range of 0.2–400 ng/mL, with a lower limit of quantification of 0.2 ng/mL. Mean recovery of neomangiferin in plasma was in the range of 97.76%–101.94%. Relative standard deviations (RSDs) of intra-day and inter-day precision were both o 10%. The accuracy of the method ranged from 94.20%to 108.72%. This method was successfully applied to pharmacokinetic study of neomangiferin after intravenous (2 mg/kg) and intragastric (10 mg/kg) administration for the first time. The oral absolute bioavailability of neomangiferin was estimated to be 0.53%7 0.08%with an elimination half-life (t1/2) value of 2.74 7 0.92 h, indicating its poor absorption and/or strong metabolism in vivo.
RESUMEN
Objective: To establish a UPLC-PDA-ELSD method for the fingerprint of Xiaokeqing Granules (XG) and to determine the contents of neomangiferin, mangiferin, timosaponin BII, palmatine, and berberine so as to provide the basis for the quality control of XG. Methods: The chromatographic fingerprints were determined by UPLC-PDA-ELSD using mangiferin and timosaponin BII peaks as the reference peaks, 23 PDA and 10 ELSD common peaks were selected, and the digital quantitative fingerprint of XG was established. Using the third systematic quantified fingerprint method, the quality levels of 28 batches of XG were assessed. The contents of neomangiferin, mangiferin, timosaponin BII, palmatine, and berberine in the 28 batches of samples were determined using external st andard method. Results: Twenty batches of XG were identified as qualified and eight batches were unqualified, in which there were differences in the five main consitituents. The quantitative results were consistent with the fingerprint. Conclusion: The method is accurate, stable, and simple, which could be applied to the quality control of XG.
RESUMEN
Objective:To determine the changes of mangiferin and neomangiferin contents in Rhizoma Anemarrhenae before and after processing.Methods: High performance liquid chromatography(HPLC) was used to determine the changes of mangiferin and neomangiferin contents in Rhizoma Anemarrhenae before and after processing.The mobile phase was ACN: 25 mmol/L KH_(2)PO_(4)(pH 3.0),gradient elution.The Similarity Evaluation System for Chromatographic Fingerprint of TCM(2004 A edition) was used to evaluate the similarity of the 3 batches of Rhizoma Anemarrhenae before and after processing.(Results:)Mangiferin in the 3 batches was upregulated and neomangiferin was downregulated afer prosessing.The similarity of the 3 batches was all decreased(