摘要
目的:对水飞蓟中七种黄酮木脂体类活性成分在电喷雾串联质谱碎裂机制进行了探讨。方法:利用超高效液相色谱-离子肼电喷雾串联质谱(UPLC-ESI-MS/MS)与诱导碰撞解离技术(CID)在负离子模式下选择合适碰撞能量对水飞蓟中七种黄酮木脂体类活性成分进行了分析,并对其二级质谱碎裂机制进行了探讨。超高效液相色谱条件ACQUITY UPLC C18色谱柱(2.1 mm×50 mm,1.7μm);流动相水-甲醇(0.1%甲酸)70∶30;流速0.25 mL.min-1;进样5μL。结果:超高效液相色谱可以很好地对此7种化合物进行分离,在二级质谱中异构体产生其特征碎片离子,呈现出一定的裂解规律,据此可以快速灵敏地区分此异构体。结论:本文为黄酮木脂体类化合物的快速检测提供了一种有效的方法。
A UPLC-ESIMS method was developed for simultaneous analysis of seven major bioactive flavonolignans in silymarin including silychristins A (1) and B (2), silydianin (3), silybins A (4) and B (5), and isosilybins A (6) and B (7). In this study, the seven major active flavonolignans including the diastereomers 1/2, 4/5, and 6/7 were completely separated using UPLC with an ACQUITY UPLC C18 column and MeOH-water (formic acid) mobile phase system. The collision-induced dissociation (CID) MS/MS spectra of these flavonolignans were studied systematically using ESI-MS. The results with the present methodology showed that UPLC-MS/MS can be used for general screening of active natural products from plant extracts and for the specific quality control of silymarin.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2011年第17期2361-2366,共6页
China Journal of Chinese Materia Medica
基金
国家自然科学基金项目(30973624)
浙江省自然科学基金项目(Y4090121)