目的建立分散固相萃取-高效液相色谱(DSPE-HPLC)联用技术应用于金银花及其相关中成药连花清瘟胶囊(LQC)中环烯醚萜苷类成分(马钱酸、莫诺苷、马钱苷、当药苷、断氧化马钱子苷、开联番木鳖苷二甲基乙缩醛)的快速提取、净化和测定的方法。方法分别采用超声提取法对金银花及相关中成药LQC进行提取,采用不同净化材料进行快速净化,采用HPLC法测定环烯醚萜苷类成分。结果采用硅藻土作为净化剂,金银花提取物净化效果较好;采用硅藻土-活性炭(80∶20)的复合净化剂时,LQC提取物净化效果较好;且该提取方法操作简单、快速、样品用量少、净化效率高,结合HPLC技术实现了金银花及相关中成药LQC中环烯醚萜苷类成分的快速提取、净化和测定。结论拓展了DSPE技术在复杂基质中药材及中成药中活性成分提取、净化中的应用,为复杂基质中药材及中成药中活性成分的提取净化及分析研究提供了方法和数据支持。
Objective To develop a new method based on dispersive solid phase extraction-high performance liquid chromatography (DSPE-HPLC) for the rapid extraction, cleansing, and determination of iridoid glycosides (loganic acid, morroniside, loganin, sweroside, secoxyloganin, and secologain dimethyl acetal) in Lonicerae Japonicae Flos (LJF) and the related traditional Chinese patent medicine (TCPM) Lianhua Qingwen Capsule (LQC). Methods Ultrasonic extraction was used for the extraction, different purification material was investigated for the rapid purification, and HPLC method was used for the determination of the content of iridoid glycosides. Results The purification effect of LJF extract was much better by using diatomite as the purification material; The purification of LQC extract was much better by using diatomite-active carbon 80 ; 20. This method was simple and rapid, and has high efficiency. It could be used for the extraction, cleaning, and determination of iridoid glycosides in LJF and related prescription combined with HPLC. Conclusion This study expands the application of DSPE in the extraction and purification of complex matrix traditional Chinese material medicine (TCMM) and TCPM, and supplies the new method and data support for the extraction and purification ofbioactive compounds from complex matrix TCMM and TCPM.