UPLC-MS/MS测定醒脑静口服制剂中3种环烯醚萜在大鼠脑中含量及其脑药动力学研究  

UPLC-MS /MS determination of content of three iridoids of Xingnaojing oral preparation in rat brains and study on their brain pharmacokinetics

作　　者：徐攀[1] 杜守颖[1] 陆洋[1] 白洁[1] 刘慧敏[1] 杜秋[1] 陈振振[1] 王振[1] 

机构地区：[1]北京中医药大学,北京100102

出　　处：《中国中药杂志》2014年第12期2351-2355,共5页China Journal of Chinese Materia Medica

基　　金：国家自然科学基金面上项目(81073057);北京中医药大学复方中药制药研究创新团队项目(2011-CXTD-13);北京中医药大学自主课题项目(2013-JYBZZ-XS-093)

摘　　要：为了建立UPLC-MS/MS同时测定大鼠脑中栀子苷、京尼平龙胆双糖苷、栀子苷酸灵敏可靠的分析方法，并对这3种环烯醚萜苷在脑中风大鼠口服醒脑静后的脑药动力学进行研究。该实验中脑浆样品沉淀蛋白2次；采用Acquity BEH C18柱，流动相为乙腈-1%甲酸-水梯度洗脱，质谱采用电喷雾电离源（ESI），多反应监测（MRM）进行负离子检测，样品分析时间为3.5 min。结果表明3种环烯醚萜苷成分在大鼠脑中的线性关系良好，提取回收率在99.6%~114.3%，日内、日间精密度和准确度良好，稳定性等均符合要求。各物质在中风大鼠脑中的t1/2和MRT相似，栀子苷与京尼平龙胆双糖苷有双峰现象，而栀子苷酸为单峰。表明该方法特异灵敏、准确可靠，可用于醒脑静口服制剂的脑药动力学研究。To establish a UPLC-MS/MS method for the simultaneous determination of geniposide, genipin 1-O-beta-D-gentiobioside and geniposidic acid in rat brains and study the brain pharmacokinetics of the three iridoid glycosides in stroke rat after the oral administration of Xingnaojing. In this experiment, brain samples were precipitated with protein for twice. Acquity BEH C18 column was adopted, with acetonitrile-0.1% formic acid-water as the mobile phase for gradient elution. ESI source was adopted for mass spectra; multiple reaction monitoring （MRM） was conducted to detect negative ions. The time for sample analysis was 3.5 min. the results showed good linear relations among the three iridoid glycosides, with the extraction recovery between 99.6% and 114.3%, good intra- and inter-day precisions and accuracies and stability in line with the requirements. The t1/2 and MRT in the three components were similar in brains of stroke rats. Geniposide and genipin 1-O-beta-D-gentiobioside showed double peaks; where as geniposidic acid showed a single peak. In conclusion, the method is so specific, sensitive, accurate and reliable that it can be used to study the brain pharmacokinetics of Xingnaojing oral preparation.

关 键 词：UPLC—MS MS 栀子苷 京尼平龙胆双糖苷 栀子苷酸 醒脑静 脑药动力学 脑中风 

分 类 号：R285.5[医药卫生—中药学] O657.63[医药卫生—中医学]