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目的:优化烟叶中茄尼醇的超声提取及纯化工艺。方法:分别以茄尼醇提取率和转移率为指标,采用单因素试验对提取工艺中的料液比、超声提取温度、超声提取时间、超声功率、提取次数,以及纯化工艺中的皂化液用量(皂化液与提取液体积比)、酸化液用量(酸化液与皂化后提取液体积比)、萃取次数等因素水平进行考察,对优化后工艺进行验证,计算茄尼醇纯度;另将本法与传统浸提法(耗时30 h)和溶剂连续循环浸提法(耗时5~6 h)比较茄尼醇的提取量。结果:优化的提取工艺为料液比1∶14、超声提取温度70℃、超声提取时间60 min、超声功率120 W、提取3次,纯化工艺为皂化液与提取液体积比2∶35、酸化液与皂化后提取液体积比2∶14、萃取4次;验证试验中提取率、转移率和纯度均值分别为92.45%、79.88%、55.86%(RSD分别为0.46%、0.30%、0.40%,n=3);3种提取方法茄尼醇的提取量分别为52.22、45.22、26.10 mg/g。结论:优化工艺操作简单、稳定,提取耗时更短,更节约能源,且提取量和纯度均较高,适合用于烟叶中茄尼醇的生产提取及纯化。
Objective: To optimize the ultrasonic extraction and purification technology of solanesol in tobacco leaves. Methods: The extraction rate of solanesol and the rate of transfer were used as indexes. The ratio of solid to liquid, ultrasonic extraction temperature, ultrasonic extraction time, ultrasonic power, extraction times and the amount of saponification liquid in the purification process (Volume ratio of saponification liquid to extract liquid), the amount of acidified liquid (the volume ratio of acidified liquid to saponified liquid), the number of times of extraction and so on. The optimized technology was verified and the purity of solanesol was calculated. The extraction of solanesol was compared with traditional extraction (30 h) and continuous solvent extraction (5 ~ 6 h). Results: The optimal extraction process was solid-liquid ratio 1:14, ultrasonic extraction temperature 70 ℃, ultrasonic extraction time 60 min, ultrasonic power 120 W, extracted three times. The purification process was the volume ratio of saponification solution to extract was 2:35, The volume ratio of liquid to saponified extract was 2:14, extracted four times. The average extraction rate, transfer rate and purity in the validation test were 92.45%, 79.88%, 55.86% (RSD 0.46%, 0.30%, 0.40% n = 3). The extraction rates of solanesol of three extraction methods were 52.22, 45.22 and 26.10 mg / g, respectively. Conclusion: The optimized process is simple, stable, extraction time is shorter, more energy saving, and the extraction yield and purity are higher, so it is suitable for the extraction and purification of solanesol in tobacco leaves.