多指标综合考察巴中产栀子提取工艺

Multi-index evaluation on the optimization of extraction process in Fructus Gardeniae from Bazhong

目的:多指标综合考察巴中产栀子提取工艺。方法:采用正交设计实验,考察料液比、提取次数、提取时间以及超声频率对巴中产栀子主要有效成分得率的影响,用高效液相色谱仪结合紫外检测器测定栀子提取液中栀子苷、西红花苷Ⅰ的含量,用高效液相色谱仪结合蒸发光散射检测器测定熊果酸含量。结果:用水提取巴中产栀子主要有效成分栀子苷最佳提取方案为料液比1∶15,提取3次,每次提取15 min,100 kHz频率超声提取;熊果酸的最佳提取方案为栀子原粉按栀子苷最佳得率方案提取后的药渣,用乙醇超声提取,料液比为1∶10,提取2次,每次提取60 min,100 kHz频率超声提取。应用统计软件,建立提取次数、提取时间、超声频率与Z总分之间多元非线性拟合回归方程如下Y=2.871 864 X12+0.002 283 X22-0.824 94X32+0.035 945 X1X2+0.702 867 X1X3-0.126 25 X2X3-13.271 6 X1+0.017 6 X2+8.144 655 X3,R=0.999 9。结论:采用多指标综合考察巴中产栀子提取工艺,指标全面,方法客观,通过验证性试验证明工艺稳定,值得推广。

OBJECTIVE To inspect the extraction process of Fructus Gardeniae from Bazhong by multi-index evaluatiorL METHODS To study the factors that play an important role on the active ingredients of Fructus Gardeniae by orthogonal de- sign, such as material-liquid ratio, extraction times, extraction time and ultrasonic frequency. With HPLC along with ELSD to detect the content of geniposide,crocin I,ursolic acid. RESULTS The outcome confirmed that the yield of main active ingredi- ents in Fructus Gardeniae extracted by water was high,the best extraction parameters of geniposide were as follows： material- liquid 1 ： 15, extracted 3 times, extracting 15 min, with the ultrasonic frequency of 100 kHz; and the extraction method of ursolic acid was to select ethanol as the solvent to draw the Fructus Gardeniae dregs extracted by water, the best extraction indexes were as follows： material liquid 1：10, extracted 2 times, extracting 60 min,with the ultrasonic frequency of 100 kHz. Combined with statistical software, established multiple nonlinear regression equation between Z-score and extraction times, extraction time, frequency ultrasonic, got the following equation： Y=2.871864X1 2＋0.002283X2 2-0.82494X3 2＋0.035945X1X2＋0.702867X1X3-0.12625X2X3-13.2716X1＋0.0176X2＋8.144655X3,R=0.9999. CONCLUSION Multi-index evalua- tion on the extraction process of Fructus Gardeniae from Bazhong is more comprehensive and objective. Validation experiments confirmed that the process is stable,worthy of popularizing.