荭草素和异荭草素、牡荆素和异牡荆素2对碳苷化合物的快速检测与鉴定

Rapid detectionand identification of two isomeric C-glycosides,orientin/isoorientin and vitexin/isovitexin

目的:建立利用超高效液相色谱-电喷雾电离质谱(UPLC-ESI/MS)快速检测和鉴定荭草素(orientin)和异荭草素(isoorientin)、牡荆素(vitexin)和异牡荆素(isovitexin)2对碳苷化合物的方法,并将其应用于荭草中上述2对碳苷化合物的分析鉴定。方法:采用BEH C18(2.1 mm×150 mm,1.7μm)色谱柱,柱温45℃,以甲醇(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱,流速0.3 mL.min-1;通过电喷雾电离源(ESI),考察了以正离子多反应监测(MRM)与不同能量下碰撞诱导解离(CID)对标准对照品中这2对碳苷化合物的检测和鉴定的可行性,利用所建立的方法筛选并鉴定了荭草粗提物中的这2对异构体。结果:建立了MRM筛选分析和CID快速鉴定荭草素和异荭草素、牡荆素和异牡荆素2对碳苷化合物的方法。应用这一方法,完成了荭草中这2对碳苷异构体的快速分析鉴定。结论:该方法简便、快速、可靠,可以用于荭草等含荭草素和异荭草素、牡荆素和异牡荆素2对异构体的药材及其相关产品中这些化合物的快速分析鉴定。

Objective：To develop a rapid method for the detection and identification of two isomeric C-glycosides,orientin/isoorientin and vitexin/isovitexin,by ultra performance liquid chromatography-electrospray ionization-mass spectrometry（UPLC-ESI/MS） and to evaluate its application in the analysis of the four glycosides in Polygonum orientale.Methods：The samples were separated on a BEH C18 column（2.1 mm×150 mm,1.7 μm） at 45 ℃ with gradient mobile phase of methanol（A） and 0.1% formic acid in water（B） at the flow rate of 0.3 mL·min-1;Multi-reaction monitoring（MRM） and collision-induced dissociation（CID） at different collision energy in the positive electrospray ionization（ESI） mode was evaluated,respectively,for the rapid detection and identification of the two isomeric C-glycosides in the standards and crude extracts.Results：A method of MRM and CID in the positive ESI was developed for the rapid detection and identification of the two isomeric C-glycosides.Orientin/isoorientin and vitexin/isovitexin were rapidly detected and identified in P.orientale.Conclusion：The method is simple,rapid and reliable and can be used in the rapid detection and identification of the two isomeric C-glycosides in their enriched plants and products.