摘要
目的:建立天麻中总多酚的含量测定方法,并对其大孔树脂的纯化工艺进行优化。方法:采用福林酚比色法测定天麻中总多酚的含量。以吸附、解吸性能为考察指标,采用静态吸附和解吸试验对4种大孔树脂进行筛选,采用动态吸附和解吸试验对上样液流速、上样液质量浓度、洗脱溶剂体积分数、洗脱流速、洗脱液体积进行考察,从而对其纯化工艺进行优化。结果:没食子酸检测质量浓度的线性范围为4~32μg/mL(r=0.9999);精密度、稳定性、重复性试验的RSD均小于2%;加样回收率为95.51%~102.94%(RSD=2.54%,n=6)。D301型大孔树脂对天麻中总多酚的静态吸附和解吸能力相对较强;最优纯化工艺为上样液流速2倍柱体积/h,上样液质量浓度4mg/mL,洗脱溶剂(乙醇)体积分数70%,洗脱流速3BV/h,洗脱溶剂体积5BV。按最优纯化工艺优化后的天麻中总多酚含量为0.381 mg/g。结论:所建含量测定方法灵敏度高、稳定性好;优化的纯化工艺稳定、可行。
OBJECTIVE:To establish a method for content determination of total polyphenols from Gastrodia elata,and to optimize the purification technology of macroporous resin. METHODS:The content of total polyphenols from G. elata was determined by Folin-ciocaileu colorimetry. Using the absorption and desorption performance as index,4 kinds of macroporous adsorption resins were selected by static adsorption and desorption tests. The flow rate and mass concentration of the sampling solution,volume fraction of eluent,eluent flow rate and eluent volume were investigated by dynamic adsorption and desorption tests. The purification technology of macroporous resin was optimized. RESULTS:The linear range of gallic acid was 4-32 μg/mL (r=0.999 9). RSDs of precision,stability and repeatability tests were all less than 2%. The recovery rate of the sample was 95.51%-102.94%(RSD=2.54%,n=6). D301 macroporous resin had strong static adsorption and desorption ability from G. elata polyphenols. The optimal purification technology included that the sample solution flow rate 2 BV/h;the sample solution mass concentration 4 mg/mL;the elution solvent 70% ethanol;the elution flow rate was 3 BV/h,and the eluent volume 5 BV. The content of total polyphenols from G. elata optimized by the optimal purification technology was 0.381 mg/g. CONCLUSIONS: Established method is sensitive and stable. The optimized purification technology is stable and feasible.
作者
蔺蓓蓓
郑红星
刘祥
周天华
胡红忠
陈琛
LIN Beibei;ZHENG Hongxing;LIU Xiang;ZHOU Tianhua;HU Hongzhong;CHEN Chen(Chinese-German Joint Institute for Natural Product Research,Shaanxi University of Technology/Shaanxi Provincial Engineering Research Center of Gastrodia elata and Cornus officinalis/College of Biological Science and Engineering, Shaanxi University of Technology, Shaanxi Hanzhong 723000, China;Shaanxi Baisheng Biological Engineering Co.,Ltd,Shaanxi Lueyang 724300,China)
出处
《中国药房》
CAS
北大核心
2019年第14期1965-1969,共5页
China Pharmacy
基金
国家高端外国专家项目(No.GDT20186100426)
国家教科文卫重点引智项目(No.W20166100045)
陕西省重点研发计划项目(No.2017NY-070)
陕西理工大学教育厅专项项目(No.18JK0156)
陕西省创新能力支撑计划项目(No.2019XY-04)
关键词
天麻
总多酚
大孔树脂
福林酚比色法
纯化工艺
Gastrodia elata
Total polyphenols
Macroporous resin
Folin-ciocaileu colorimetry
Purification technology