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优化六味地黄方醇沉工艺,获得最优的醇沉工艺,为醇沉过程苷类控制提供理论依据。采用P-B试验设计,以莫诺苷、马钱苷、芍药苷为指标,考察醇沉前液密度、醇沉温度、搅拌速度、加醇浓度、静置温度、静置时间、醇含量、加醇方式、离心、醇洗10个参数对醇沉工艺的影响,得出六味地黄方浸膏苷类醇沉关键工艺参数。并采用Box-Behnken响应面法对关键工艺参数与醇沉效果的影响进行研究与探讨,得出关键工艺参数之间的交互影响以及与指标成分的相关性方程。通过对各个指标结果建立二次回归模型,并对二次回归方程求解得到六味地黄方苷类醇沉的最优工艺参数:醇沉前浸膏密度为1.13 g·m L-1,加入95%乙醇醇沉至含醇量为34%,580 r·min-1搅拌15 min,静置17 h,离心得到醇沉上清液,验证实验结果与模型预测值接近。采用响应面法优化六味地黄方苷类醇沉工艺确定工艺参数的方法合理可行。
Optimize Liuweidihuang alcohol precipitation process, to obtain the best alcohol precipitation process, to provide a theoretical basis for alcohol precipitation process glycosides control. Adopting the PB experimental design, taking morroniside, loganin and paeoniflorin as indexes, the effects of alcohol concentration, alcohol precipitation temperature, stirring speed, alcohol concentration, standing temperature, standing time, alcohol content and alcohol addition Method, centrifugation, alcohol wash 10 parameters on the alcohol precipitation process, draw Liu Wei Dihuang extract glycosides alcohol precipitation key process parameters. The influence of key process parameters and alcohol sink effect by Box-Behnken response surface method was studied and discussed. The interaction between key process parameters and the correlation equation with index components were obtained. Through establishing the quadratic regression model for each index result and solving the quadratic regression equation, the optimal technological parameters of the Liu Weihuang yellow glycoside alcohol precipitation were obtained: the density of the alcohol precipitation before precipitation was 1.13 g · m L-1, 95% The ethanol was precipitated to 34% alcohol content and stirred at 580 r · min-1 for 15 min. After standing for 17 h, the alcohol supernatant was obtained by centrifugation. The experimental results were in good agreement with the model predictions. The method of response surface method to optimize the method of determining process parameters of Liuwei Dihuang glycoside alcohol precipitation process is reasonable and feasible.