基于伴随标志物在线控制技术绞股蓝总皂苷纯化工艺及成分鉴定研究.docVIP

基于伴随标志物在线控制技术绞股蓝总皂苷纯化工艺及成分鉴定研究 　　[摘要] 基于“伴随标志物”紫外在线检测技术以绞股蓝总皂苷（GPS）为目标，优化绞股蓝中GPS的纯化工艺，采用UPLCQTOFMS技术对GPS进行定性。“伴随标志物”紫外在线检测研究表明，上样终点为流出液吸光度为原药液的1/2时，洗脱终点为洗脱流出液吸光度基本稳定。UPLCQTOFMS鉴定出GPS提取物中的16个皂苷，其中新皂苷3个。该研究优选出的纯化工艺简单、检测方便、易于在线测定、实时记录，能较好的运用到大生产或生产的自动化中。质谱定性鉴定结果表明，基于“伴随标志物”紫外在线检测技术能很好地保留药材中的主要药效成分，为过程控制和质量溯源提供了分析工具。 　　[关键词] 绞股蓝总皂苷； 纯化； 大孔吸附树脂； 伴随标志物； 在线检测； UPLCQTOFMS 　　Purifying process of gynostemma pentaphyllum saponins based on 　　adjoint marker online control technology and identification of 　　their compositions by UPLCQTOFMS 　　FAN Dongdong1，2， KUANG Yanhui3， DONG Lihua 2， YE Xiao 1，2， CHEN Liangmian2， ZHANG Dong 2， 　　MA Zhenshan2， WANG Jinyu2， ZHU Jingjing2*， WANG Zhimin2*， WANG Deqin3， LI Chuyuan3 　　（1. Shaanxi University of Chinese Medicine， Xi′an 712046， China； 　　2. National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines， Institute of 　　Chinese Materia Medica， China Academy of Chinese Medical Sciences， Beijing 100700， China； 　　3. Hutchison Whampoa Guangzhou Baiyunshan Chinese Medicine Co.， Ltd.， Guangzhou 510515， China） 　　[Abstract] To optimize the purification process of gynostemma pentaphyllum saponins （GPS） based on adjoint marker online control technology with GPS as the testing index. UPLCQTOFMS technology was used for qualitative analysis. Adjoint marker online control results showed that the end point of load sample was that the UV absorbance of effluent liquid was equal to half of that of load sample solution， and the absorbance was basically stable when the end point was stable. In UPLCQTOFMS qualitative analysis， 16 saponins were identified from GPS， including 13 known gynostemma saponins and 3 new saponins. This optimized method was proved to be simple， scientific， reasonable， easy for online determination， realtime record， and can be better applied to the mass production and automation of production. The results of qualitative analysis indicated that the adjoint marker online control technology can well