A uniform experimental design procedure was used to investigate the effects of some operating parameters on the extraction of emodin from Polygonum cuspidatum Sieb. et Zucc. products. Variables tested were volume rati...A uniform experimental design procedure was used to investigate the effects of some operating parameters on the extraction of emodin from Polygonum cuspidatum Sieb. et Zucc. products. Variables tested were volume ratio of material to solvent, size of material, extraction time and temperature and composition of extraction solvent （mixtures of acetone-water）. Each variable was tested at seven levels; 7 experiments were performed in random order. Analyses of the extracts were performed by high-performance liquid chromatography with diode array detection（HPLC-DAD）. Analytical responses were processed by using a forward regression analysis, in order to find polynomial function describing the relationship between variables and responses. For all the analytes the experimental conditions for providing the highest extraction yield inside the experimental domain considered were found. Finally, a simple, rapid and accurate analytical method was developed for the determination of emodin by high performance liquid chromatography. The separation is achieved within 25 rain on an ODS column using methanol and water as gradient mobiles. Emodin can be quantified by using external standard method detecting at 436 nm. Good linearity is obtained with correlation coefficient exceeding 0.9986 and the detection limit and the quantification limit are 1.53 and 3.23 mg/L respectively. This method shows good reproducibility for the quantification of the emodin with intra-day and inter-day relative standard deviation less than 2.3% and 5.6% respectively. Under optimized extraction conditions, the recovery of the standard is 96.5%. The validated method is successfully applied to quantify the emodin in seven Polygonum cuspidatum sieb. Et zucc. products, which provided an idea for the pre-treatment of determination of active compounds in traditional Chinese medicines.展开更多
基金Project (04JJ3081) supported by Hunan Province Natural Science Foundation of China
文摘A uniform experimental design procedure was used to investigate the effects of some operating parameters on the extraction of emodin from Polygonum cuspidatum Sieb. et Zucc. products. Variables tested were volume ratio of material to solvent, size of material, extraction time and temperature and composition of extraction solvent （mixtures of acetone-water）. Each variable was tested at seven levels; 7 experiments were performed in random order. Analyses of the extracts were performed by high-performance liquid chromatography with diode array detection（HPLC-DAD）. Analytical responses were processed by using a forward regression analysis, in order to find polynomial function describing the relationship between variables and responses. For all the analytes the experimental conditions for providing the highest extraction yield inside the experimental domain considered were found. Finally, a simple, rapid and accurate analytical method was developed for the determination of emodin by high performance liquid chromatography. The separation is achieved within 25 rain on an ODS column using methanol and water as gradient mobiles. Emodin can be quantified by using external standard method detecting at 436 nm. Good linearity is obtained with correlation coefficient exceeding 0.9986 and the detection limit and the quantification limit are 1.53 and 3.23 mg/L respectively. This method shows good reproducibility for the quantification of the emodin with intra-day and inter-day relative standard deviation less than 2.3% and 5.6% respectively. Under optimized extraction conditions, the recovery of the standard is 96.5%. The validated method is successfully applied to quantify the emodin in seven Polygonum cuspidatum sieb. Et zucc. products, which provided an idea for the pre-treatment of determination of active compounds in traditional Chinese medicines.
文摘以大黄素为指标对虎杖中的有效成分进行超临界流体CO2萃取。用正交设计法考察了最优萃取条件。影响超临界流体萃取率的主要因素依次是:动态流量、温度、压力、时间;确定了大黄素的最佳萃取条件是:萃取压力25 MPa,萃取温度55℃,动态流量8 kg/h,萃取时间30 m in。超临界流体萃取大黄素的提取率达0.36%。
