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Objective:To establish the quality standard for Xiao'er Hanting granule. Methods:Astragali Radix,Rhizoma Atrac-tylodis Macrocephalae (baked) and Saposhnikoviae Radix were qualitatively identified by a TLC method. The contents of calycosin-7-O-β-D-glycoside in the preparation were determined by an HPLC method. The chromatographic column was Cosmosil C18(250 mm× 4.6 mm,5 μm);the mobile phase was acetonitrile-0.2% methanoicacid(16 :84); the flow rate was 1.0 ml·min-1; the detection wavelength was 260 nm. Results:Astragaloside A in Astragali Radix was detected by the TLC method,and Rhizoma Atractylodis Mac-rocephalae (baked),Saposhnikoviae Radix and saposhnkoviae standard crude drug had the same clear spots without any negative inter-ference. The linear range of calycosin- 7-O-β-D-glycoside was 0.061-0.613 μg(r =0.999 9). The average recovery was 99.4% (RSD=1.29%,n=6). Conclusion:The method is accurate,rapid,stable and reliable with good reproducibility,which is suitable for the quality control of Xiao'er Hanting granule.
RESUMEN
Objective: To establish a UPLC fingerprint of Compound Qima Capsule (CQC), to determine the eight contents in CQC (gastrodin, 5-hydroxymethylfurfura(5-HF), calycosin-7-O-β-D-glycoside(CG), rhoifolin, naringin, formononetin-7-O-β-D-glucoside (FG), calycosin, and formononetin), and to provide the basis for the evaluation of CQC. Methods: The Agilent Eclipse C18 (100 mm × 4.6 mm, 3.5 μm) column was used with a mobile phase of methyl acetonitrile-0.05% phosphoric acid gradient elution, the flow rate was 0.3 mL/min, the column temperature was 25℃, and the detection wavelength was 265 nm. Results: The fingerprint chromatography with good resolution and reproducibility included 22 mutual peaks, and the similarity was more than 0.98. Gastrodin, 5-HF, CG, rhoifolin, naringin, FG, calycosin, and formononetin were baseline seperated with good linearity relationships between concentration and peak areas over the linear ranges, within 0.976-29.880, 10.596-52.980, 2.697-13.485, 2.262-11.309, 40.768-203.840, 5.825-29.126, 0.372-1.858, and 1.888-9.440 μg/mL (r > 0.999 9), whose average recoveries were 1.04%, 1.30%, 1.81%, 1.41%, 1.29%, 1.01%, 1.48%, and 1.29%. The contents of 10 batches of gastrodin, 5-HF, CG, rhoifolin, naringin, FG, calycosin, and formononetin were 2.883-3.491, 1.710-3.791, 0.107-0.286, 0.157-0.346, 8.853-10.726, 0.282-0.692, 0.097-0.135, and 0.041-0.063 mg/g, respectively. Conclusion: The method is rapid, simple, and accurate, and can be used for the quality control of CQC.
RESUMEN
Objective: To study a method of chemical constituents of Astragali Radix by HPLC-DAD-MS. Methods: The compounds were separated by using Thermo Hypersil-Hypurity C18 (150 mmx2.1 mm, 5 μm) analytical column. The oven temperature was adjusted at 40 °C. Mobile phase consisted of methanol and water using a gradient elution. The flow rate was set at 0.25 mL/min. UV spectra were obtained by scanning from 200 to 370 nm. The APCI-MS spectra were obtained in the positive ion mode scanning from m/z 100 to 650. Results: The peaks can be identified by comparing their UV spectra, the molecular weights and retention behaviors with data reported in the literature. At least five compounds were tentatively identified as calycosin-7-O-β-D-glycoside, ononin, calycosin, formononetin, and (3R)-7,2′-dihydroxy-3′, 4′-dimethoxyisoflavan. Conclusion: Because of providing UV and molecular mass as well as retention time, HPLC-DAD-MS is a powerful tool for chemical analysis of traditional Chinese material medica.