八月瓜果皮中常春藤皂苷元水解工艺优化及图谱分析

Optimization of hydrolysis process and structure map analysis of hederagenin in Akebia trifoliata pericarp

以乙腈-0.1%磷酸(体积比20∶80)溶液为流动相,检测波长210 nm,建立了高效液相色谱法测定常春藤皂苷元的方法,并采用傅立叶红外光谱(Fourier transform infrared spectrometry,FTIR)、核磁共振对其结构进行分析。考察了HCl体积分数、温度和时间对常春藤皂苷元水解得率的影响。在单因素实验的基础上,采用响应面分析法对工艺进行优化,建立了各因子关于常春藤皂苷元水解得率的回归方程,得到该工艺的最佳条件。结果表明,HCl体积分数24%、温度82℃、水解时间3.1 h,在此条件下,常春藤皂苷元得率为61.423%;样品中常春藤皂苷元的含量为(11.55675±0.039221)mg/g;常春藤皂苷元的红外光谱分析与标准品的主要官能团基本一致;核磁共振分析与报道的常春藤皂苷元核磁数据基本一致。该研究可为八月瓜果皮中常春藤皂苷元的深加工提供一定参考。

In order to optimize the hydrolysis,content determination and structural analysis of the saponins in the extracted Akebia trifoliata pericarp,a method was developed for the determination of hederagenin,using acetonitrile-0.1%phosphoric acid(20∶80)solution as mobile phase and the detection wavelength was 210 nm.Its structure was analyzed by infrared spectroscopy(FTIR)and 1HNMR and 13 CNMR.The effects of volume fraction of hydrochloric acid,temperature and time on the hydrolysis yield of hederagenin were investigated.Based on the single factor experiment,using response surface analysis method to optimize the process,established the regression equation of each factor on hederagenin hydrolysis yield,and obtained the optimum conditions of the process.The results showed that the volume fraction of hydrochloric acid was 24%,the temperature was 82℃,and the hydrolysis time was 3.1 h.Under these conditions,the yield of hederagenin was 61.423%;the content of hederagenin in the sample was(11.55675±0.039221)mg/g;the infrared spectrum of hederagenin was basically consistent with the main functional groups of the hederagenin standard;the 1 HNMR and 13 CNMR analysis were basically consistent with the reported data of hederagenin.Therefore,this study can provide some reference for the deep processing of hederagenin in the Akebia trifoliata pericarp.