RESUMEN
OBJECTIVE：To establish a method for sim ultaneous determination of 7-hydroxycoumarin，6，7-dimethoxy- coumarin，5，7-dimethoxycoumarin，imperatorin and bergaptene in Shugan hewei pills. METHODS ：Samples were extracted by Soxhlet extraction and separated by using D 101 macroporous adsorption resin ；HPLC method was used to determine the contents of above 5 components. The determination was performed on Venusil MP C 18 column with mobile phase consisted of methanol- 0.1％ phosphoric acid water solution （gradient elution ）at the flow rate of 1.0 mL/min. The detection wavelength was 270 nm and the column temperature was 30 ℃ . The sample size was 10 μ L. RESULTS：The linear ranges were 1.875-187.5 μ g/mL for 7-hydroxycoumarin（r＝0.999 9），1.075-107.5 μg/mL for 6，7-dimethoxycoumarin（r＝0.999 9），1.261-126.1 μg/mL for 5， 7-dimethoxycoumarin（r＝0.999 9），0.875-87.5 μg/mL for imperatorin（r＝0.999 9），2.033-203.3 μg/mL for bergaptene（r＝0.999 8）， respectively. RSDs of precision ，stability（24 h），reproducibility and durability tests were lower than 2.0％. Average recoveries were 95.18％ -98.44％ （RSD＝1.27％ ，n＝6）， 95.35％ -98.14％ （RSD＝1.16％ ，n＝6），95.21％ -97.32％ （RSD＝0.83％ ，n＝6）， 95.43％-97.14％（RSD＝0.76％，n＝6），95.12％-98.75％（RSD＝1.35％，n＝6），respectively. The average contents of the above five components in 3 batches of shugan hewei pills were 0.424，0.239，0.305，0.180，0.459 mg/g（n＝2）.CONCLUSIONS：A method for simultaneous determination of five components in Shugan hewei pills was established.
RESUMEN
Objective: To establish an HPLC method for simultaneous determination of 7-hydroxycoumarin, narirutin, naringin, hesperidin, neohesperidin, nobiletin, 3,5,6,7,8,(3,4)-heptamethoxyflavone, tangeretin, and auraptene from Aurantii Fructus, determinate and compare the content of various chemical components from Aurantii Fructus with different perimeters. Methods: The HPLC system consisted of a diamon C18 (250 mm × 4.6 mm, 5 μm), the mobile phase was methanol (A)-water (adjusted pH 3.0 with phosphorous acid). The gradient elution conditions: 0-25 min, 30%-50% A; 25-35 min, 50%-70% A; 35-40 min, 70%-75% A; 40-55 min, 75%-100% A. The flow rate was 1.0 mL/min and the column temperature was 30 ℃. The detection wavelength was 320 nm and the injection volume was 20 μL. Results: The calibration curves of 7-hydroxycoumarin, narirutin, naringin, hesperidin, neohesperidin, 3,5,6,7,8,(3,4)-heptamethoxyflavone, nobiletin, tangeretin, and auraptene had good linear relationship in the ranges of 0.002 18-0.07 μg (r = 0.999 8), 0.021 8-0.70 μg (r = 0.999 9), 0.242 5-7.76 μg (r = 0.999 8), 0.024 38-0.78 μg (r = 0.999 4), 0.523 76-16.76 μg (r = 0.999 3), 0.003 13-0.10 μg (r = 0.999 3), 0.004 13-0.132 μg (r = 0.999 6), 0.002 75-0.088 μg (r = 0.999 6), and 0.000 93-0.03 μg (r = 0.999 3); And the average recoveries (n = 6) of the nine components were 98.50%, 98.80%, 99.51%, 98.43%, 99.64%, 99.21%, 100.03%, 98.75%, and 101.11%, respectively. Conclusion: This method can be applied to determinating the components from Aurantii Fructus, including 7-hydroxycoumarin and 3,5,6,7,8,(3,4)-heptamethoxyflavone, etc.
RESUMEN
Objective: To investigate the chemical constituents from the petroleum ether and ethyl acetate extract of Guizhi Fuling Capsule (GFC). Methods: The compounds were separated with chromatography on silica gel and polydextran gel columns, and prep-HPLC, and their chemical structures were identified by NMR and MS spectral methods, respectively. Results: Eight compounds were isolated from the petroleun ether extract and were identified as coumarin (1), 7-hydroxycoumarin (2), cinnamic alcohol (3), ergosterol (4), ergosta-4, 6, 8 (14), 22-tetraen-3-one (5), β-amyrin acetate (6), campesterol (7), and α-amyrin acetate (8). Thirteen compounds were isolated from the ethyl acetate extract and were identified as apingenin (9), kaemferol (10), quercetin (11), kaempferol-3-O-glucopyranoside (12), catechin (13), epicatechin (14), syringic acid (15), hyperin (16), eicosanoids (17), syringaresinol (18), mudanpioside A (19), mudanpioside C (20), and galloylpaeoniflorin (21). Conclusion: Compounds 1-21 are isolated from GFC for the first time.