Shanghai Key Laboratory for Pharmaceutical Metabolite Research, School of Pharmacy, Second Military Medical University, No. 325 Guohe Road, Shanghai 200433, China.
Rapid Commun Mass Spectrom. 2010 Sep 15;24(17):2520-8. doi: 10.1002/rcm.4643.
A high-performance liquid chromatography-diode array detection/electrospray ionization mass spectrometry (HPLC-DAD/ESI-MS) method was applied to the characterization of ten iridoid glycosides in Gardenia jasminoides Ellis, a traditional Chinese medicine. During the process of structural elucidation, two groups of isomers including two epimers were structurally characterized and differentiated according to their distinctive fragmentation patterns which were closely related to their isomeric differentiations. Subsequently, the major compounds were purified by multi-dimensional chromatography and semi-preparative HPLC and the structure identification was confirmed with NMR techniques. The major fragmentation pathways of iridoid glycosides in Gardenia jasminoides Ellis obtained through the MS data were schemed systematically, which provided the best sensitivity and specificity for characterization of the iridoid glycosides especially the isomers so far. Based on the fragmentation patterns of iridoid glycosides concluded, seven major iridoid glycosides were characterized in rat plasma after intravenous administration of Gardenia jasminoides Ellis.
建立了高效液相色谱-二极管阵列检测/电喷雾电离质谱(HPLC-DAD/ESI-MS)联用方法,用于分析栀子中的 10 种环烯醚萜苷类成分。在结构鉴定过程中,根据其特征性裂解模式,对两组包括两个差向异构体在内的同分异构体进行了结构表征和区分,这些裂解模式与它们的异构化差异密切相关。随后,通过多维色谱和半制备高效液相色谱对主要化合物进行了纯化,并通过 NMR 技术确定了结构鉴定。通过 MS 数据系统地总结了栀子中环烯醚萜苷类化合物的主要裂解途径,为环烯醚萜苷类化合物,特别是异构体的特征化提供了最佳的灵敏度和特异性。基于总结的环烯醚萜苷类化合物的裂解模式,在栀子灌胃给药后的大鼠血浆中鉴定出 7 种主要的环烯醚萜苷类成分。