ABSTRACT
Objective: To investigate the chemical constituents of the leaves of Hydrangea macrophylla. Methods: The chemical constituents were separated and purified by various isolation methods (silica gel, ODS, and HPLC column chromatography), and their structures were determined by the analysis of spectral data (1H-NMR, 13C-NMR, and MS). Results: Eleven compounds were obtained and elucidated as following: secologanin ethyl methyl acetal (1), secologanin dimethyl acetal (2), secoxyloganin (3), 7-deoxyloganic acid (4), loganic acid (5), 8-epi-loganin (6), loganin (7), 7-dehydrologanin (8), sweroside (9), epi-vogeloside (10), and vogeloside (11). Conclusion: Compound 1 is a new compound, named as macrophyoside. Compounds 3 and 8 are isolated for the first time from the plants of Hydrangea Linn.
ABSTRACT
Objective To establish an HPLC method for simultaneous determination of loganin, chiratin, secoxyloganin, rosmarinic acid and calceolarioside B in Shuangxiangpaishi granules. Method HPLC colunmn was Alltima C18 column (4.6 mm×250 mm, 5 μm); mobile phase consisted of acetonitrile-methanol (1: 3) (A) -0.1% phosphate acid solution (B) with gradient elution; the column temperature was 35°C; the flow rate was 1.0 ml/min; all the injection volume was 20 μl; loganin, chiratin and secoxyloganin were detected at 240 nm, rosmarinic acid and calceolarioside B were detected at 330nm. Results The above mentioned five main ingredients had linearity in the given concentration range at 5.91-118.20 μg/ml (r=0.9995), 4.10-82.00 μg/ml (r=0.9991), 8.13-162.60 μg/ml (r=0.9993), 12.57-251.40 μg/ml (r=0.9998), 4.95-99.00μg/ml (r=0.9997), respectively. The average recoveries (n=6) and RSD were 96.88 (1.31), 99.09 (1.47%), 98.29 (1.59), 98.82 (1.42) and 97.51 (0.86), respectively. Conclusion This dual-wavelength HPLC method could simultaneously determine the contents of the five ingredients in Shuangxiangpaishi granules and can be used to evaluate their quality. The method is simple, accurate, sensitive and repeatable. It could be used as an efficient strategy for systematic quality evaluation of Shuangxiangpaishi granules.
ABSTRACT
To optimize the alcohol precipitation process for Lonicerae Flos and Artemisiae Annuae Herba (LA) in Reduning Injection and obtain the relationship equation of the key process parameters and quality attributes, which could provided a theoretical basis of the control automization in the alcohol precipitation process. With the transfer rates of neochlorogenic acid, chlorogenic acid, cryptochlorogenin acid, caffeic acid, secoxyloganin and solid content in precipitation liquid as evaluation indexes, the effect of the seven factors, such as relative density and the temperature of LA in liquid phase before alcohol precipitation, alcohol concentration in the end of alcohol precipitation, stirring speed in alcohol precipitation, adding alcohol speed, standing temperature, and standing time, on the alcohol precipitation process was investigated by the single factor experiment. By analysis of variance, the key factors that could influence the alcohol precipitation process were determined. Then the range of parameters of key factors was further studied and explored by Box-Behnken response surface methodology. The optimum preparation conditions of the alcohol precipitation process of LA were as follows: stirring speed was 550 r/min, adding alcohol speed was 4.0 mL/s, standing temperature was 30℃, standing time was 24 h, alcohol concentration was 75%, the relative density of LA was 1.10, and the temperature of LA was 25℃. Under these conditions, the transfer rates of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, and secoxyloganin were 94.8%, 97.6%, 97.4%, 97.2%, and 96.1%, and the solid content was 4.2%. The alcohol precipitation process of LA have been optimized by the response surface method, which could help to enhance the stability of the process.
ABSTRACT
Objective: To establish an HPLC method for simultaneously determining eight components such as neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, isochlorogenic acid A, isochlorogenic acid B, isochlorogenic acid C, and secoxyloganin in Lonicerae Japonicae Flos. Methods: A RP-HPLC method was established with Luna C18 column (250 mm × 4.6 mm, 5 μm) by a gradient elution using methanol (A) and 0.1% phosphoric acid (B): 0-20 min, 12%-30% A; 20-60 min, 30%-50% A; The flow rate was 1.0 mL/min with double wavelength (237 and 324 nm), and the column temperature was 30°C. Results: The eight components was separated to baseline; Each component had a wide linear range and a good linear relationship (r > 0.9998); The recoveries were 98.72% to 102.50%. Conclusion: The method is accurate, sensitive, reliable, and has a good reproducibility. It could be used for the quality control of Lonicerae Japonicae Flos.
ABSTRACT
Objective: To establish a quantitative analysis of multi-components with a single-marker (QAMS) method for the determination of the nine components in Reduning Injection (RI), comparing with the external standard method, and to evaluate the adaptation and application of QAMS method in the quality control of RI. Methods: Chlorogenic acid, isochlorogenic acid A, and gardenoside were used as the internal reference substances. The relative correlation factors (f) of neochlorogenic acid, cryptochlorogenic acid, and caffeic acid to chlorogenic acid, isochlorogenic acid B and isochlorogenic acid C to isochlorogenic acid A, and secoxyloganin to gardenoside were calculated and established. The results were compared with those obtained by the external standard method. Results: Within the linear ranges, the f values of chlorogenic acid to neochlorogenic acid, cryptochlorogenic acid, and caffeic acid were 0.965, 0.991, and 0.555, respectively; isochlorogenic acid A to isochlorogenic acid B and isochlorogenic acid C were 1.283 and 1.129, respectively; jasminoidin to secoxyloganin was 1.030. The two methods did not show the significant difference in assay results. Conclusion: The QAMS method is feasible and credible, and could be used to determine the multiple components in RI.