金橘中金橘苷的纯化工艺

The Purification Technology of Fortunellin from Fortunella margarita

采用硅胶柱色谱法进行纯化,以金橘苷提取率和纯度为考察指标计算综合评分,以脱剂比例、上样量、硅胶量、柱直径为因素,运用单因素试验和Box-Behnken响应面法优化金橘苷的纯化工艺。结果表明,响应面法确定的最佳纯化工艺为:洗脱剂氯仿-甲醇-水的体积比为4︰1︰0.1、上样量2.1 mL、硅胶量10.6 g、柱直径1 cm;验证试验中金橘苷取率和纯度的综合评分为1.0005(RSD=1.09%,n=3),与预测值1.0234接近,偏差为2.24%。优化后的工艺能较好地纯化金橘苷,且工艺稳定、可靠,可为金橘的深度研究及产业化应用提供技术参考和依据。

Silica gel column chromatography was used for purification.Using the extraction rate and purity of fortunellin from Fortunella margarita as index to calculate the comprehensive score,the ratio of eluting agent,the amount of sample,the amount of silica gel and the diameter of column as factors,the purification technology of fortunellin from Fortunella margarita was optimized by single factor test and Box-Behnken response surface methodology.It was determined that the optimum purification technology of fortunellin from Fortunella margarita was as follows:the eluting agent chloroform-methanol-water 4︰1︰0.1,the amount of sample 2.1 mL,the amount of silica gel 10.6 g,the diameter of column 1 cm.In validation test,the comprehensive score of the extraction rate and purity of fortunellin from Fortunella margarita was 1.0005(RSD=1.09%,n=3);It was close to predicted value 1.0234,and the deviation was 2.24%.The optimized technology could be used for the purification of fortunellin.The technology was stable and reliable,which could provide technical reference and basis for the in-depth study and industrial application of Fortunella margarita.