亚临界水提取固相分散萃取净化测定人参中皂苷含量

Effects of Extraction and Drying Methods on Effective Components of Cistanche Deserticola Extracts

为建立一种人参及其制品中人参皂苷的提取方法和检测方法,优化亚临界水提取条件,固相分散萃取填料种类、材料的使用条件。以400 kPa、240℃亚临界水提取,得到提取液后,利用聚乙烯吡咯烷酮(PLS)填料以固相分散萃取的方式富集其中的皂苷类化合物,以5 mL甲醇洗脱目标物,进入液相色谱检测。结果显示,在添加质量分数分别为0.2,0.5和1.0 g/kg时,亚临界水提取,仅耗时5 min,能将样品中人参皂苷完全提取。加标回收率为90.59%~99.06%,精密度(SRSD)为0.92%~2.53%,小于3%。待测液质量浓度在5~500μg/mL,即人参皂苷含量0.02~4.0 g/kg范围内,线性关系良好,R^(2)大于0.9990。方法检出限在5.68~8.08μg/g,满足微量检测和常量检测的要求。利用亚临界水提取人参样品中的人参皂苷,并结合PLS填料固相分散萃取净化富集样品,液相色谱检测,是一种快捷、高效、准确、稳定、绿色环保的检测方法。

To establish a method and determination for extraction of ginsenoside and its products,the conditions of subcritical water extraction and solid-phase dispersive extraction(SPE)were optimized.After extraction with 400 kPa and 240℃subcritical water,the saponins were enriched with PLS packing by solid-phase dispersion extraction,and the target was eluted with 5 mL methanol and detected by liquid chromatography.The results showed the subcritical water extraction took only 5 minutes and could completely extract ginsenoside from the subcritical water at 0.2,0.5 and 1.0 g/kg,respectively.The recoveries were 90.59%-99.06%and the precision SRSD was 0.92%-2.53%,less than 3%.When the concentration of ginsenoside was in the range of 5-500μg/mL,it meant that the content of ginsenoside was in the range of 0.02-4.0 g/kg,the linearity was good,and R^(2) was greater than 0.9990.The detection limit was 5.68-8.08μg/g,which met the requirements of trace and constant detection.The ginsenosides were extracted by subcritical water,and were treated by PLS solidphase dispersion extraction and detected by liquid chromatography,which was a fast,efficient,accurate,stable,green and environmentally friendly detection method.