柴胡皂苷提取物灌胃给予大鼠后肺组织中移形成分的LC-MS分析  

LC-MS analysis of saikosaponins in rat lung tissues after oral administration of bupleurum saikosaponin extract

作　　者：乔亚荣 张峰[1,2] 方媛[1] 贾金萍[3] 闫艳[1] 田俊生[1] 秦雪梅[1] 高晓霞[1] 

机构地区：[1]山西大学中医药现代研究中心,太原030006 [2]山西大学化学化工学院 [3]山西大学大型科学仪器中心

出　　处：《山西医科大学学报》2016年第3期264-269,共6页Journal of Shanxi Medical University

基　　金：国家自然科学基金项目(81001688;81473415);国际科技合作资助项目(2011DFA32630);"重大新药创制"科技重大专项资助项目(2012ZX09103201-035);山西省振东制药研究生教育创新中心硕士研究生实践教学模式探索项目

摘　　要：目的初步探讨柴胡皂苷类成分在大鼠肺组织的代谢,为更好地揭示柴胡皂苷类成分在体内过程提供依据。方法采用液相质谱联用仪分析柴胡皂苷提取物灌胃给药后大鼠肺组织中的成分,得到各成分的总离子流图和二级质谱图,结合文献与对照品对照对各色谱峰进行鉴定。色谱条件:采用BEH-C18色谱柱(2.1 mm×100 mm,1.7μm),流动相为乙腈(A)-水(B),梯度洗脱(0-4 min,25%A→37%A;4-10 min,37%A;10-18 min,37%A→50%A;18-22 min,50%A→90%A;22-25 min,90%A→90%A;25-26 min,90%A→25%A),流速0.4 ml/min。质谱条件:电喷雾电离离子源;正负离子扫描模式;温度450℃,质量扫描范围:m/z 150-1 500。结果以柴胡皂苷类化合物的质谱裂解规律为指导,共鉴定出15种化合物。其中10种药材原型成分,分别为柴胡皂苷(SS)a,SSc,SSf,SSd,SSb2,SSe,3″-O-乙酰化柴胡皂苷a,6″-O-乙酰化柴胡皂苷a,3″-O-乙酰化柴胡皂苷d,6″-O-乙酰化柴胡皂苷d;5种代谢物分别为柴胡次皂苷F,柴胡次皂苷D,柴胡次皂苷G,去糖氧化柴胡皂苷a,去糖氧化柴胡皂苷d。结论通过柴胡皂苷提取物肺中成分分析,初步确认了柴胡皂苷提取物在肺中的柴胡皂苷类成分以及代谢产物,为柴胡发挥解热镇痛作用的物质基础提供依据。Objective To explore the metabolic profile of saikosaponins in rat lung tissues,and provide evidences for the profile of saikosaponins in vivo. Methods A rapid,sensitive LC-MS was developed to explore the components of bupleurum saikosaponin extract in rat lung tissues after oral administration. The LC-MS full scan and MS / MS were established to identify the components in rat lung tissues. The separation was performed on an BEH C18（ 2. 1 mm × 100 mm,1. 7 μm）,with acetonitrile-water as the mobile phase. The gradient profile was as follows： 0- 4 min,25% A→37% A; 4- 10 min,37% A; 10- 18 min,37% A→50% A; 18- 22 min,50% A→90% A; 22- 25 min,90% A→90% A; 25- 26 min,90% A→25% A. The flow rate was maintained at 0. 4 ml / min. MS method was set with ESI ion,positive and negative ions mode and temperature of 450 ℃,and the full mass range was from 150 to 1 500. Results Based on the MS pattern of saikosaponins,15 compounds were identified in rat lung tissues,including saikosaponin a（ SSa）,SSc,SSf,SSd,SSb2,SSe,3″-O-acetylsaikosaponin a,6″-O-acetylsaikosaponin a,3″-O-acetylsaikosaponin d,6″-O-acetylsaikosaponin d,prosaikogenin F,prosaikogenin D,prosaikogenin G. Conclusion LC-MS results indicate that the active constituents in bupleurum saikosaponin extract in lung are confirmed,and provide an evidence for the antipyretic effects of saikosaponins in vivo.

关 键 词：LC-MS 柴胡皂苷类 代谢产物 体内分析 

分 类 号：R284[医药卫生—中药学]