UPLC-MS/MS法同时测定家兔血浆中6个黄酮类成分及其药代动力学研究  

UPLC-MS/MS simultaneous determination and pharmacokinetic of six flavonoids in rabbit plasma

作　　者：黄勇[1] 何峰[1] 郑林[1] 张治蓉[1] 兰燕宇[1] 王永林[1] 

机构地区：[1]贵阳医学院药学院,贵阳550004

出　　处：《药物分析杂志》2012年第1期1-6,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金(No.30860366);国家科技重大专项课题(No.2008ZX09101-021);贵州省科技计划重大专项项目(No.黔科合重大专项字[2007]6010号)

摘　　要：目的:建立UPLC-MS/MS同时测定家兔血浆中注射用复方荭草冻干粉针的6个黄酮类化合物(异荭草素,荭草素,牡荆素,灯盏乙素,木犀草苷,槲皮苷)的分析方法,并计算其在家兔体内的药动学参数。方法:血浆样品酸化后以甲醇沉淀蛋白;色谱采用Waters BEH C18(2.1 mm×50 mm,1.7μm)色谱柱,流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,质谱采用多反应监测(MRM)进行正离子检测,样品分析时间为3.5 min。结果:6个黄酮类成分在家兔血浆中呈良好线性关系,提取回收率在79.4%～105.9%之间,日内、日间精密度和准确度良好,各检测成分的方法回收率分别为异荭草素96.8%～110.1%,荭草素85.8%～98.8%,牡荆素86.0%～110.6%,灯盏乙素86.7%～102.5%,木犀草苷84.1%～93.8%,槲皮苷96.5%～112.2%。6个黄酮类成分在家兔体内的平均滞留时间均较短,在16 min以内。结论:该方法特异、快速、灵敏,可用于注射用复方荭草冻干粉针的药代动力学研究。Objective ： To develop an UPLC - MS/MS method for simultaneous determination of six flavonoids （ isoorientin, orientin, vitexin, scutellarin, cynaroside, quercitrin） after intravenous administration of compound Hongcao freeze dried powder for injection and acqire the pharmacokinetic parameters in rabbit plasma. Methods ：Following a protein precipitation with acidified methanol for plasma samples. The whole analysis was achieved within 3.5 rain by gradient elution on an Waters BEH C18 （2. 1 mm × 50 mm, 1.7 μm） column and the mobile phase consisting of aeetonitrile and water（ containing 0. 1% formic acid）. Detection was carried out by the multiple reaction monitoring（MRM） positive ion mode. Results：Good linearity was achieved for the six compounds, the extraction recovery was between 79. 4% to 105.9%, the intra - and inter - day precisions and the accuracy were good ,the method recoveries of the six flavonoids were 96. 8% - 110. 1% for isoorientin, 85.8% - 98.8% for orientin, 86. 0% - 110. 6% for vitexin, 86. 7% - 102. 5% for scutellarin, 84. 1% - 93.8% for cynaroside, 96. 5% - 112. 2% for quercitrin, respectively. The MRT of the six flavonoids in rabbit was all blow 16 min. Conclusion：The above mentioned method is specific, sensitive and suitable for the pharmacokinetic studies of compound Hongcao freeze dried powder for injection.

关 键 词：生物样品 中药复方注射剂 黄酮 异荭草素 荭草素 牡荆素 灯盏乙素 木犀草苷 槲皮苷 药代动力学 超高效液相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]