目的:优化通关藤中总皂苷的超声提取工艺及纯化工艺,制备纯化的通关藤总皂苷。方法:以通关藤总皂苷提取率为指标,以乙醇体积分数、液料比和提取温度等为因素,采用单因素试验和Box-Behnken响应面法优化通关藤总皂苷的超声提取工艺;以洗脱液中总皂苷含量为指标,考察乙醇洗脱体积分数对总皂苷经D101型大孔吸附树脂吸附纯化工艺的影响。结果:最优超声提取工艺条件为乙醇体积分数85%、液料比18.5∶1(ml/g)、提取温度80℃;验证试验中通关藤总皂苷平均提取率为4.80%(RSD=1.06%,n=3),与预测值4.89%接近,偏差为1.84%。最优纯化工艺条件为以45%乙醇为洗脱溶剂除杂,再用90%乙醇进行纯化;验证试验表明通关藤总皂苷含量实测平均值为62.45%(RSD=0.88%,n=3)。结论:优化后的工艺可较好地提取、纯化通关藤中的总皂苷,且工艺稳定、可靠。
OBJECTIVE: To optimize the ultrasonic extraction and purification technology of total saponins from Marsdenia te- nacissima, and to prepare purified total saponins from M. tenacissima. METHODS: Using the extraction rate of total saponins from M. tenacissima as index, ethanol volume fraction, solvent-solid ratio and extraction temperature as factors, ultrasonic extraction technology of total saponins from M. tenacissima was optimized by single factor test and Box-Behnken response surface design. Us- ing the content of total saponins in elution, the effects of ethanol elution volume fraction on purification technology of total sapo- nins by D101 type macroporous adsorption resin was investigated. RESULTS: The optimal ultrasonic extraction technology was as follows as ethanol volume fraction of 85%, solvent-solid ratio of 18.5 : 1 (ml/g), extraction temperature of 80 ℃. In verification test, the average extraction rate of total saponins from M. tenacissima was 4.80% (RSD= 1.06%, n=3); it was close to predicted value 4.89%, and the deviation was 1.84%. The optimal purification technology was as follows as 45% ethanol as eluant, 90% ethanol for purification. Verification test showed that the average content of total saponins from M. tenacissima was 62.45% (RSD= 0.88%, n=3). CONCLUSIONS: The optimized technology can be used for the extraction and purification of total saponins from M. tenacissima. The technology is stable and reliable.