基于多指标综合评分法优化黄连工业化生产提取工艺

目的:本研究采用多指标综合评分法优化适合工业化生产的黄连提取浓缩与干燥工艺。方法:首先确定了以盐酸小檗碱为指标的黄连生物碱测定方法;考察了乙醇浓度、料液比和提取时间对黄连生物碱提取的影响,在单因素结果的基础上采用L9(3^4)正交试验设计法优化黄连提取工艺,以干膏率和黄连生物碱含量进行综合评分确定最优提取工艺。同时采用L9(3^4)正交试验的方法考察了真空干燥工艺对黄连生物碱的影响,确定最优干燥工艺条件,并进行验证。结果:建立了黄连生物碱HPLC测定方法,精密度和加标回收率良好,方法准确可行;确定了黄连提取浓缩与真空干燥的最佳工艺,加入8倍70%乙醇,提取1.5 h,提取2次;控制温度60℃,采用真空减压法进行浓缩,浓缩至密度为1.18,然后进行真空干燥,温度控制在60℃,提取液铺设厚度2 mm。提取物中黄连生物碱质量分数为33.18%,提取率为82.59%。结论:通过多指标综合评分法优化的黄连提取工艺稳定可靠,适合工业化生产,为黄连及其中药复方制剂的工业化生产提供实验依据。

Optimization of Industrial Extraction of Coptidis Rhizoma Based on Multi-index Integrated Evaluation Method

Objective:Multi-index integrated evaluation method will be adopted to optimize the industrial extraction,concentration and drying process of Coptidis Rhizoma.Methods:Firstly,the assay method of coptis alkaloids with the index of berberine hydrochloride was determined.The effects of ethanol concentration,solid-liquid ratio and extraction duration on the extraction of coptis alkaloids were investigated.Based on the univariate factor result,orthogonal test L9(3^4)was conducted for the optimization of extraction technology of Coptidis Rhizoma,dry extract yield and the content of coptis alkaloids were chosen as the index of evaluation to determine the optimum technology.At the same time,orthogonal test L9(3^4)was also conducted to investigate the effect of coptis alkaloids in vacuum drying process.The optimum drying processes were determined and verified by industrial production.Results:HPLC method of coptis alkaloids was set up,which has well accuracy and recovery rate.The method was accurate and feasible.The optimum technology of extraction,concentration and vacuum drying of Coptidis Rhizoma was as follows:adding 8 times amount of 70%ethanol and extracting twice,1.5 hours every time,controlling temperature at 60℃,concentrating by vacuum decompression method,concentrating to the density of 1.18,and then vacuum drying,controlling temperature at 60℃,laying thickness of extracting solution was 2 mm.The coptis alkaloids of extract was 33.18%,and the extraction rate was 82.59%.Conclusion:The extraction technology of Coptidis Rhizoma optimized by multi-index integrated evaluation is stable,reliable and suitable for industrial production.The research can provide experimental evidences for industrial production of Coptidis Rhizoma and its Chinese medicine compound preparations.