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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 establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method to study the pharmacokinetics and distribution of ephedrine in the rat’s epimedium, a major active ingredient of Polygonum cuspidatum, The role of herbs in rats. Methods: LC-MS / MS method was used. The mobile phase consisted of 5 mmol·L-1 ammonium acetate solution-acetonitrile (1: 1, v / v) , Flow rate: 0.2 mL · min-1. ESI source, negative ion scan mode, multiple reaction detection mode: The m / z of precursor and daughter ions are 269.2 and 181.9, respectively, for the detection of emodin in biological samples. Results: The emodin concentration in the range of 0.03-6μg · mL-1 showed a good linearity with a linear correlation coefficient of 0.9989. The absolute recoveries of high, medium and low concentrations were 87.8% ~ 120.3% with relative recoveries of 95.9% ~ 117.2%. The emodin in brain tissue showed a good linearity in the range of 5.0-1000 ng · g-1, with a linear correlation coefficient of 0.9999. The absolute recoveries of high, middle and low concentrations were 94.1% -97.2% and the relative recoveries were 99.1% -103.1%. Emodin in rat pharmacokinetic model in line with two-compartment model. Conclusion: This method has good sensitivity, accuracy, precision and specificity for the determination of emodin, and is fully suitable for the determination of trace emodin in biological samples.