基于响应面法的土茯苓中落新妇苷提取工艺研究
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摘要
以土茯苓为原料,采用超声法提取土茯苓中的落新妇苷,利用高效液相色谱法对提取液中的落新妇苷进行定量测定。在单因素实验的基础上,采用BOX-Behnken响应面法考察乙醇浓度、料液比和超声时间对土茯苓提取液中落新妇苷含量的影响,以此确定从土茯苓中提取落新妇苷的优化工艺。优化结果表明,当乙醇浓度为67. 7%,提取时间为87. 5 min,料液比为1∶10. 3(g∶mL)时,土茯苓提取液中的落新妇苷含量的预测值为0. 0621 mg/mL。验证实验结果显示,预测值与实测值之间的平均偏差为2. 0%,说明实验所建立的数学模型具有良好的预测性。最终确定土茯苓中落新妇苷提取工艺为:提取时间为90 min,乙醇浓度为70%,料液比为1∶10(g∶mL),实验测定土茯苓提取液中落新妇苷平均含量为0. 0611 mg/mL.
By using Smilacis glabra Rhizoma as the raw material,ultrasonic method was used to extract astilbin. High performance liquid chromatography(HPLC) was used for the quantitative determination of astilbin in the extract of Smilacis glabra Rhizoma. Based on the single-factor experiment,the BOXBehnken response surface method was used to investigate the effects of ethanol concentration,solidliquid ratio and ultrasonic time on the content of astilbin in the extraction liquid of Smilacis glabra Rhizoma,in order to determine the optimal extraction process of astilbin from Smilacis glabra Rhizoma. The results showed that when the concentration of ethanol was 67. 7%,the extraction time was 87. 5 min,and the ratio of material to liquid was 1∶ 10. 3 g: mL,the content of astilbin in the extract of Smilacis glabra Rhizoma was 0. 0621 mg/mL. The experimental results show that the average deviation between the predicted value and the measured value is 2. 0%,which indicates that the mathematical model established in this experiment has good predictability and the extraction process is accurate and feasible. Finally,the extraction process is determined to be: the extraction time is 90 min,the ethanol concentration is 70%,the matter-liquid ratio is 1∶ 10 g: mL,and the average content of astilbin in the extraction solution is 0. 0611 mg/mL.
By using Smilacis glabra Rhizoma as the raw material,ultrasonic method was used to extract astilbin. High performance liquid chromatography(HPLC) was used for the quantitative determination of astilbin in the extract of Smilacis glabra Rhizoma. Based on the single-factor experiment,the BOXBehnken response surface method was used to investigate the effects of ethanol concentration,solidliquid ratio and ultrasonic time on the content of astilbin in the extraction liquid of Smilacis glabra Rhizoma,in order to determine the optimal extraction process of astilbin from Smilacis glabra Rhizoma. The results showed that when the concentration of ethanol was 67. 7%,the extraction time was 87. 5 min,and the ratio of material to liquid was 1∶ 10. 3 g: mL,the content of astilbin in the extract of Smilacis glabra Rhizoma was 0. 0621 mg/mL. The experimental results show that the average deviation between the predicted value and the measured value is 2. 0%,which indicates that the mathematical model established in this experiment has good predictability and the extraction process is accurate and feasible. Finally,the extraction process is determined to be: the extraction time is 90 min,the ethanol concentration is 70%,the matter-liquid ratio is 1∶ 10 g: mL,and the average content of astilbin in the extraction solution is 0. 0611 mg/mL.
引文
[1]国家药典委员会．中华人民共和国药典[S]．北京:中国医药科技出版社，2015.
[2]方圆，王雪彦，晁若冰．土茯苓药材中落新妇苷和总黄酮的含量测定方法研究[J]．药物分析杂志，2010,30(9):1738-1741.
[3]隋欣，王人悦．落新妇苷稳定性的研究[J]．食品研究与开发，2015,36(8):10-12.
[4]方婧，付梅红，杨洪军，等．微波协助提取在中药饮片含量测定中的应用(3):微波法与药典法测定土茯苓中落新妇苷含量比较[J]．中国实验方剂学杂志，2011,17(24):43-45.
[5]林耿丰，梁伟杰，肖凤霞，等．正交设计法优选土茯苓中落新妇苷及总黄酮的提取工艺[J]．亚太传统医药，2011,7(6):39-42.
[6]温慧萍，肖建中，雷伟敏，等．HPLC结合响应面法优化柳叶蜡梅总黄酮提取工艺及其抑菌活性研究[J]．浙江农业学报，2018,30(2):298-306.
[7]张霞，康鑫，何先元，等．响应面法优化黄荆叶总黄酮提取工艺及月周期变化规律研究[J]．安徽农业科学，2019,47(3):158-162.
[8]王敏，胡梦梅，陈文龙，等．响应面法优化土茯苓总黄酮的提取工艺[J]．江西中医药，2014,45(11):60-63.
[2]方圆，王雪彦，晁若冰．土茯苓药材中落新妇苷和总黄酮的含量测定方法研究[J]．药物分析杂志，2010,30(9):1738-1741.
[3]隋欣，王人悦．落新妇苷稳定性的研究[J]．食品研究与开发，2015,36(8):10-12.
[4]方婧，付梅红，杨洪军，等．微波协助提取在中药饮片含量测定中的应用(3):微波法与药典法测定土茯苓中落新妇苷含量比较[J]．中国实验方剂学杂志，2011,17(24):43-45.
[5]林耿丰，梁伟杰，肖凤霞，等．正交设计法优选土茯苓中落新妇苷及总黄酮的提取工艺[J]．亚太传统医药，2011,7(6):39-42.
[6]温慧萍，肖建中，雷伟敏，等．HPLC结合响应面法优化柳叶蜡梅总黄酮提取工艺及其抑菌活性研究[J]．浙江农业学报，2018,30(2):298-306.
[7]张霞，康鑫，何先元，等．响应面法优化黄荆叶总黄酮提取工艺及月周期变化规律研究[J]．安徽农业科学，2019,47(3):158-162.
[8]王敏，胡梦梅，陈文龙，等．响应面法优化土茯苓总黄酮的提取工艺[J]．江西中医药，2014,45(11):60-63.