Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences, Beijing 100700, PR China.
J Pharm Biomed Anal. 2012 Dec;71:152-6. doi: 10.1016/j.jpba.2012.07.018. Epub 2012 Aug 8.
The identification and quantification of saponins in crude extracts are challenging because of their similar structures and weak ultraviolet absorption. In this study, a rapid resolution liquid chromatography coupled with triple quadruple electrospray tandem mass spectrometric method was established to identify and quantify steroid saponins in the rhizomes of Dioscorea panthaica Prain et Burk, a traditional Chinese medicine. Six steroid saponins were simultaneously determined and quantified within 9min. All analytes were subjected to a RP-18e (50mm×2mm) monolithic column using a gradient elution program with a final detection using electrospray ionization tandem mass spectrometry in the negative ionization mode. The rapid resolution liquid chromatography/tandem mass spectrometry method achieved a limit of detection ranging from 0.52 to 20.40ngmL(-1) and a limit of quantification ranging from 1.20 to 75.20ngmL(-1) for the six studied steroidal saponins. The intra-day and inter-day precision (RSD) were less than 5.34%, and the recovery (RSD) was 1.50-3.51%. The highly sensitive and rapid method is suitable for the quantification of steroidal saponins in D. panthaica rhizomes.
由于结构相似且紫外吸收较弱,粗提取物中甾体皂苷的鉴定和定量具有一定挑战性。本研究建立了一种快速分辨液相色谱-三重四极杆电喷雾串联质谱法,用于鉴定和定量分析传统中药穿龙薯蓣根茎中的甾体皂苷。该方法在 9min 内同时测定和定量了 6 种甾体皂苷。所有分析物均在 RP-18e(50mm×2mm)整体柱上进行梯度洗脱程序,最终采用电喷雾电离串联质谱法在负离子模式下进行检测。该快速分辨液相色谱/串联质谱法对 6 种甾体皂苷的检测限范围为 0.52-20.40ngmL(-1),定量限范围为 1.20-75.20ngmL(-1)。日内和日间精密度(RSD)小于 5.34%,回收率(RSD)为 1.50-3.51%。该高灵敏度、快速的方法适用于穿龙薯蓣根茎中甾体皂苷的定量分析。