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Objective: To establish HPLC-DAD method for the simultaneous determination of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside in Shenqi Shiyiwei Granule (SSG). Methods: The chromatographic separation was achieved on an Waters XBridge-C18 (250 mm × 4.6 mm, 5.0 μm) column with methanol-acetonitrile-water (15:80:5) and methanol-0.1% phosphoric acid (10:90) as mobile phases for gradient elution, at the flow rate of 1.0 mL/min; The column temperature was 35℃. Results: The linear ranges of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside were 0.4-8.0 μg/mL (r = 0.999 2), 0.2-4.0 μg/mL (r = 0.999 5), 0.2-4.0 μg/mL (r = 0.999 5), 0.1-2.0 μg/mL (r = 0.999 6), 0.1-2.0 μg/mL (r = 0.999 7), 0.1-2.0 μg/mL (r = 0.999 4), 0.5-10 μg/mL (r = 0.999 2), 0.6-12 μg/mL (r = 0.999 2), 0.4-8.0 μg/mL (r = 0.999 4), 1.0-20 μg/mL (r = 0.999 6), and 0.8-16 μg/mL (r = 0.9993). The average recoveries (n = 6) were 98.1% (RSD = 0.9%), 98.1% (RSD = 1.6%), 99.1% (RSD = 1.6%), 98.3% (RSD = 1.8%), 99.5% (RSD = 1.5%), 99.9% (RSD = 0.6%), 98.5% (RSD = 0.7%), 100.4 (RSD = 0.8%), 101.6% (RSD = 0.4%), 99.7% (RSD = 0.9%), and 101.2% (RSD = 1.1%), respectively. The contents of nine batches of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside were 0.081-0.089, 0.261-0.269, 0.060-0.069, 0.038-0.047, 0.030-0.037, 0.042-0.049, 0.420-0.428, 0.141-0.151, 0.178-0.189, 0.107-0.117, and 0.069-0.078 mg/g. The results showed that there was little difference among the batches. Conclusion: The method is accurate, sensitive, credible, and repeatable. It can be applied to the quality control of SSG.
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Objective: To establish a method of HPLC for thesimultaneous determination of eleven ingredients (tanshinone IIA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin, and 23-acetate alisol B) in Xinnaokang Tablets. Methods: The contents of tanshinone IIA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin, and 23-acetate alisol B were determinedby HPLC. Separation was performed on an InertSustain C18column (250 mm × 4.6 mm, 5 μm); Mobile phase was methanol-acetonitrile (1∶1, A)-0.1% phosphoric acid (B), gradient elution: 0-10.0 min, 80% B; 10.0-20.0 min, 80%-70% B; 20.0-35.0 min, 70%-50% B; and 35.0-50.0 min, 50%-30% B; Flow rate was 0.9 mL/min; Column temperature was 40 ℃; Injection volume was 10 μL. Results: The separations of tanshinone IIA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin, and 23-acetate alisol B were good.The linear ranges were good,28.24-282.42, 15.89-158.90, 20.53-205.26, 4.09-40.94, 12.08-120.76,40.03-404.30, 4.08-40.75, 2.13-21.25, 7.91-79.14, 20.30-202.96, and 4.10-40.96μg/mL for tanshinone IIA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin,and 23-acetate alisol B, respectively, with the correlation r> 0.999 0. The extraction recoveries varied from 98.15% to 101.84% (RSD varied from 0.62% to 1.71%). The contents of tanshinone IIA, puerarin, β-ecdysone, liquiritin, paeoniflorin, spinosin, ferulic acid, kaempferide, emodin, tenuifolin,and 23-acetate alisol Bwere 0.870-0.887, 6.321-6.329, 0.857-0.866, 0.171-0.179, 0.369-0.377, 2.128-2.136, 0.088-0.099, 0.148-0.155, 0.113-0.121,0.371-1.380, and 0.101-0.109 mg/gin six batches of samples, respectively. Conclusion: This method is rapid and has high sensitivity, high accuracy, and good specificity,which can provide the basis for the quality control of Xinnaokang Tablets.
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Objective To compare the chemical components among Rhizoma Alismatis of different specifications. Methods Rhizoma Alismatis of 8 different weights were chosen, and then contents of 23-acetate alisol B were determined by HPLC, and infrared spectrometry fingerprint was determined by Fourier transform infrared spectroscopy. Results The contents of 23-acetate alisol B in Rhizoma Alismatis of 8 different specifications were over 0.06%, and had no relation with specification of Rhizoma Alismatis (P>0.05). The similarities of infrared spectrometry fingerprint were above 0.9. Conclusion The chemical components among Rhizoma Alismatis of different specifications were basically the same. Contents of 23-acetate alisol B of Rhizoma Alismatis of 8 different specifications conformed to regulation of China Pharmacopoeia.
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Objective:To establish a method for the determination of 23-acetate alisol B in Longdan Xiegan honey pills by HPLC. Methods:The analysis was performed on a Waters Symmetry C18 (250 mm × 4. 6 mm,5μm) column with the mobile phase of acetonitrile-0. 1% phosphoric acid (62 ∶ 38). The flow rate was 1. 0 ml·min-1, the column temperature was 35℃ and the detection wavelength was set at 208nm. Results: The linear range of 23-acetyl alisol B was 19. 999 5- 1 999. 9500 ng(r =0. 999 9), and the average recovery was 95. 56%(RSD = 0. 7%, n = 6). Conclusion: The method is simple, rapid and accurate, and can be used to control the quality of Longdan Xiegan honey pills with good repeatability and recovery.
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Objective: To study the chemical constituents in Alisma orientalis extracts with hypoglycemic effect. Methods: To study the in vivo hypoglycemic effects of A. orientalis extracts, high fat diet (HFD)-induced insulin resistance male C57BL/6J mice were treated with water and ethanol extracts of A. orientalis in diet, and glucose tolerance test was carried out following the intervention. Silica gel, ODS, and preparative HPLC were used to isolate the compounds. Their chemical structures were elucidated on the basis of NMR and MS spectral data. Results: Sixteen compounds were identified as sitosterol (1), palmitic acid (2), heptadecanoic acid (3), eicosanoic acid (4), 11-deoxy-alisol B (5), 23-acetate alisol B (6), 23-acetate alisol C (7), alisol B (8), 24-acetate alisol A (9), alisol G (10), 24-acetate alisol F (11), alisol L (12), alisol C (13), alisol F (14), alisol A (15), and 16-oxo-24-acetate alisol A (16), and nine of the triterpenes could improve glucose uptake in HepG2 cells. Conclusion: Compounds 3 and 4 are isolated from A. orientalis for the first time. The water and ethanol extracts of A. orientalis could improve glucose tolerance test. Triterpenes may be one of the therapeutic material basis in hypoglycemic activities in A. orientalis.
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Objective: To develop an effective and rapid method for the preparation of 23-acetate alisol B from Alisma orientalis. Methods: The SFE-CO2 extract from A. orientalis was injected into high speed counter current chromatography (HSCCC) directly, and eluted with difierent solvent systems. The crystalline purity was detected by HPLC. The structure of the target compound was identified by UV, IR, MS, and NMR. Results: The solvent system composed of n-hexane-ethylacetate- methanol-water (3∶2∶3∶2) was the best. The lower phase was used as the mobile phase and performed at a flow rate of 2 m/min, while the apparatus rotated at 800 r/min, and detected at 254 nm. The prepared alisol B 23-acetate was identified with infrared spectrometry (IR), mass spectrometry (MS), and nuclear magnetic resonance (NMR) detection, and its purity was 99.8% analyzed by HPLC. Conclusion: The established method is relatively simple, fast, and suitable for the fast isolation and separation of alisol B 23-acetate.
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Object To optimize the preparation procedure for Zhixuan Granula (ZXG). Methods The optimum extracting conditions of ZXG were selected by orthogonal test with the active components: 23-acetate alisol B, atractylenolide I, and dried extract as the index, it mice sedation of ZXG was clarified by pharmacodynamics. Results The optimum preparation procedure was as follows: Rhizoma Alismatis and Rhizoma Atractylodis Macrocephalae were extracted with alcohol first, adding 12-fold 70% alcohol by refluxing, extracting twice, 2 h once, then extracted with water, adding 14-fold water, extracting twice, 2 h once. The extract showed the obvious effect on sedation of mice. Conclusion The optimum preparation procedure is reliable, with higher extracting ratio of the active components.