摘要
采用LC-MS/MS法对醋制前后柴胡中的Ⅰ型柴胡皂苷a、c、d与Ⅱ型柴胡皂苷b2进行含量测定,色谱柱为KinetexTMC18(50 mm×4.6 mm,2.6μm),流动相为水-乙腈-甲醇三元梯度洗脱;检测系统为电喷雾离子源(ESI)-三重四级杆质谱仪,ESI负离子模式检测,待测成分与内标均采用负离子加合物作为选择性反应监测(SRM)的前体离子,以[M+HCOO]-/[M-H]-作为SRM检测离子对。方法学验证结果显示,所建立的方法灵敏度高、专属性好,可作为柴胡生品及醋炙品的质量控制方法。含量测定结果表明,醋制过程引发了由Ⅰ型柴胡皂苷向Ⅱ型的转化,醋制后柴胡皂苷b2的含量明显增加,对柴胡醋炙品的质量控制应同时考虑对Ⅰ、Ⅱ型柴胡皂苷柴胡皂苷进行测定。
A liquid chromatography tandem mass spectrometry （LC-MS/MS） method was developed for the simultaneous determination of the type Ⅰ saikosaponin a, c, d and the type Ⅱ saikosaponin b2 in crude radix bupleuri and radix bupleuri processed by vinegar. The analytes were well separated on a KinetexTM C18 column （50 mm ×4.6 mm, 2. 6 μm） using gradient elution. The analytes and the internal standard were analyzed by monitoring the fragmentation transition pair of anionic adducts to deprotonated molecules in negative electrospray mode. The validated method was proved to be sensitive, precise, accurate and selective, and could be applied for the quality control of crude and processed radix bupleuri by vinegar. The results of quantification indicates possible chemical transformation of the type I saikosaponin to their structural isomers of the type Ⅱ, and the quality control of radix bupleuri processed by vinegar should take consideration of both type I and Ⅱ saikosaponins.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2012年第4期334-340,共7页
Journal of China Pharmaceutical University
基金
国家自然科学基金资助项目(No.30873439)~~
