碱水超声法提取二醇型人参皂苷工艺研究

Study on Ultrasonic Alkaline Water Extraction of Panoxadiol Saponins

目的:比较超声碱水提取人参皂苷方法与传统用蒸馏水和甲醇提取人参皂苷方法的不同,研究超声碱水提取人参皂苷的优势,寻找最佳实验条件,从而得到能获取最高提取率的超声碱水提取方法。方法:提取时采用超声碱水提取方法,实验分为五个变量,分别为提取温度、碱水pH值、提取时间、超声功率、料液比;每个变量设置三个梯度,设置单因素试验分别考察,共11组实验。实验以提取温度35℃,提取时间40 min,提取功率120 W,pH值13,料液比1∶10为对照组。提取时采用超声波清洗器,通过单因素实验分别获得五个最佳实验条件,从而确定最佳工艺方案。确定最佳工艺方案后,按最佳工艺方案里的实验条件进行试验。超声甲醇提取和蒸馏水提取时,除提取所用溶剂不同外,提取时间、料液比、pH值、温度、提取功率均与超声碱水提取人参皂苷方法的对照组一致。分析时采用高效液相色谱法(HPLC法)。色谱条件:色谱柱选用Hypersil Gold C_(18)(250 mm×4.6 mm,5μm)测定13组实验的人参皂苷的含量,流动相为乙腈(A)-0.05%磷酸水(B),流速为1 mL/min,检测波长为203 nm。结果:十一组超声碱水提取人参皂苷总提取率分别为:当料液比1∶10时,0.363%;1∶15时,0.303%;1∶20时,0.339%。提取温度20℃时,0.374%;35℃时,0.303%;50℃时,0.309%。提取时间20 min时,0.338%;60 min时,303%;50 min时,0.338%。超声功率80 W时,0.284%;120 W时,0.303%;160 W时,0.312%。溶剂pH值9时,0.316%;pH值11时,0.303%;pH值13时,0.627%。超声蒸馏水提取的总提取率为167%;超声甲醇提取的总提取率为0.196%。结论:通过进行单因素考察实验,设置十一组实验,运用超声波清洗器提取,高效液相进行分析,通过计算提取率,可以得出超声碱水提取人参皂苷的最佳实验条件为20℃、pH值13、160 W、20 min、料液比1∶10。通过超声碱水提取人参皂苷与传统提取人参皂苷提取率相比,超声碱水提取法提取率高,具有显著的优势,能够较大的提高提取Rb1,Rb2,Rc,Rd四种人参皂苷的提取率,增加人参的利用率,减少浪费。

Objective:In comparison with the traditional method of extracting ginsenoside,ultrasonic extraction of ginsenoside was studied.The optimal extraction conditions of ginsenoside were studied by ultrasonic method.The ultrasonic extraction method was obtained.Method:The extraction temperature,alkaline water pH,extraction time,ultrasonic power,ratio of material to liquid were compared with each other.Three variables were set for each variable,and single factor test was carried out.In a total of 11 experiments.The extraction temperature was 35℃,the extraction time was 40 min,the extraction power was 120 W,pH 13 and the ratio of solid to liquid was 1∶10.At the time of extraction,five best experimental conditions were obtained by single factor experiment,and the optimum technological scheme was determined.After determining the optimum process plan,test was carried out according to the experimental conditions in the optimum process plan.The extraction time,ratio of material to liquid,pH,temperature and extraction power were all consistent with the control group of ginsenoside extracted by ultrasonic water in the extraction process.The analysis was carried out using high performance liquid chromatography(HPLC).The mobile phase consisted of acetonitrile(A)-0.05%phosphoric acid(B)at a flow rate of 1 mL/min,and the content of ginsenoside was determined by using Hypersil Gold C_(18)(250 mm×4.6 mm,5μm).The wavelength is 203 nm.Conclusion:The total extraction rates of ginsenosides extracted by ultrasonication were as follows:when the ratio of material to liquid was 1∶10,0.363%,0.303%at 1∶15;0.339%at 1∶20 and 0.374%at 20℃;0.303%at 35℃,0.309%at 50℃,0.338%at 20 min,303%at 60 min,0.338%at 50 min;0.284%for ultrasonic power;0.303%for 120 W;0.312%for 160 W;0.316%for solvent pH 9,0.303%for pH 11 and 0.627%for pH 13.The total extraction rate of ultrasonic distilled water extraction was 167%.The total extraction rate of ultrasonic methanol extraction was 0.196%.