【摘要】 目的:建立犬血浆中冬凌草甲素浓度的LC-MS测定方法,为深入研究冬凌草甲素在犬体内的药代动力学特征提供有效、可靠的检测手段。方法:采用Shim-pack VP-ODS(150 mm×2.0 mm,5μm)色谱柱,以乙腈-水(50∶50)为流动相,HPLC/电喷雾离子源质谱检测(HPLC/ESI-MS),乙酸乙酯作为萃取剂,检测犬血浆中冬凌草甲素的含量,并评价方法的稳定性和重现性。结果:本方法在0.0125~6.4μg.mL-1浓度范围内线性关系良好(R2=0.9994),定量限为0.0125μg.mL-1,平均回收率为71.18%~76.99%,日内精密度为2.4%~5.0%,日间精密度为1.2%~6.3%。室温放置30 min,样品预处理后放置24 h、-24℃贮存14 d及反复冻融3次稳定性良好。其RSD均小于15%。结论:该分析方法可行性高,重现性好,可用于研究冬凌草甲素在犬体内药代动力学特征。更多还原

【Abstract】 Objective:To establish an LC-MS method for quantitative determination of oridonin in dog plasma and provide a reliable method to evaluate the pharmacokinetics profile of oridonin in dogs.Methods:Shim-pack VP-ODS(150 mm×2.0 mm,5 μm) column,acetonitrile-water(50∶50)mobile phase system,HPLC/electrospray ionization mass spectrometric detection(HPLC/ESI-MS),and acetic ether were developed to quantitatively determine oridonin in dog plasma.The stability and repeatability of the method were evaluated.Results:The assay was found to be linear for oridonin concentration in the range 0.0125 μg·mL-1 to 6.4 μg·mL-1,with a lower limit of quantification of 0.0125 μg·mL-1.The extractive recovery was 71.18%-76.99%.The intra-day and inter-day precision of the method were 2.4%-5.0% and 1.2%-6.3% respectively.Stability studies indicated that oridonin in dog plasma was stable for 30 min at room temperature,24 h after sample pretreatment process,store at-24 ℃ for 14 days and was also stable over three freeze–thaw cycles.All of the relative standard deviation were less than 15% respectively.Conclusions:This method is highly feasible and reproducible.It may be a reliable technology to study pharmacokineties of oridonin in dogs.更多还原