摘要
目的:建立液相色谱-串联质谱(LC-MS/MS)方法,对虎杖主要药效成分大黄素在大鼠体内的药代动力学及在脑组织分布的经时变化进行研究,以探讨虎杖药材在大鼠体内的作用规律。方法:采用LC-MS/MS方法,色谱柱:Eclipse Plus-C18柱(50mm×2.1mm,1.8μm);流动相:5mmol·L-1醋酸铵溶液-乙腈(1∶1,v/v),流速:0.2mL·min-1。ESI离子源,负离子扫描模式,多反应离子检测模式:母离子和子离子的m/z分别是269.2和181.9,检测生物样品中的大黄素含量。结果:血浆大黄素在0.03～6μg·mL-1范围内呈良好的线性,线性相关系数0.9989,高、中、低浓度绝对回收率87.8%～120.3%,相对回收率为95.9%～117.2%;脑组织大黄素在5.0～1000ng·g-1范围内呈良好的线性,线性相关系数0.9999,高、中、低浓度绝对回收率94.1%～97.2%,相对回收率99.1%～103.1%。大黄素在大鼠体内药代动力学模型符合二房室模型。结论:该方法对大黄素测定具有良好的灵敏度、准确度、精密度以及专属性,完全适应于生物样品中微量大黄素的浓度测定。
Objective：To develop an LC - MS/MS method based on liquid chromatography with tandem mass spectrometry detection for the determination of emodin of Rhizoma Polygoni Cuspidati in plasma and brain of rat. Method： The column was Eclipse Plus - C18 （50 mm × 2. 1 mm, 1.8 μg, mobile phase was 5 mmol · L^-1 NH4 Ac solution - acetonitrile （ 1 ： 1, v/v） at a flow rate of 0. 2 mL · min^-1. The analyte was detected using negative ionization by multiple reaction monitoring mode. The mass transition paires of m/z 269.2 and 181.9 was applied to detect emodin. Results ：The assay exhibited a good linearity in the concentration range from 0. 03 - 6 μg ·mL^-1 with a correlation coefficient of 0. 9989 from rat plasma. The method recoveries of emodin were from 95.9% to 117.2% and the extraction recoveries of emodin were from 87.8% to 120. 3% at three concentration levels from rat plasma samples. A good linearity in the concentration range from 5.0 - 1000 ng · g^-1 with a correlation coefficient of 0. 9999 from rat brain. The method recoveries of emodin were from 99. 1% to 103.1% and the extraction recoveries of emodin were from 94. 1% to 97.2% at three concentration levels from rat brain samples. Conclusion：This method is accurate, precise, sensitive and specific, and can be applied to the determination of emodin in biological specimen.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第6期926-930,共5页
Chinese Journal of Pharmaceutical Analysis
