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目的建立LC-MS/MS方法测定芫花素在大鼠体内的血药浓度,并研究其药物动力学。方法大鼠灌胃芫花提取物,眼眶采血,离心,以蛋白沉淀法处理血浆样品,芒柄花素为内标,电喷雾离子化,多反应检测方式进行负离子检测,检测离子质荷比(m/z)分别为283.2/267.9,267.0/251.9。使用Phenomenex Gemini 110 C18色谱柱(50 mm×2.0 mm,5μL);以甲醇-0.1%甲酸水(85∶15)为流动相,等度洗脱;柱温:40℃;流速:0.3mL·min-1。结果大鼠灌胃芫花提取物后的药-时曲线符合二房室模型,芫花素血药浓度在5~1000 ng·mL-1范围内线性关系良好(r2=0.998),最低检测限(LOQ)为0.5 ng·mL-1,日内及日间精密度(RSD)为2.42%~10.71%,日内及日间准确度为95.67%~112.15%,血浆中无内源性基质干扰,稳定性良好。结论本研究所建立的方法简便、灵敏、重复性好、分析速度快,可用于血浆样品中芫花素的血药浓度测定和大鼠体内药物动力学研究。
Objective To establish a LC-MS / MS method for the determination of genkwanin in rats plasma concentration and study its pharmacokinetics. Methods After the rats were inoculated with the extract of Daphne genkwa, orbital blood was collected and centrifuged, the plasma samples were treated with protein precipitation method, and the anion was detected by electrospray ionization and multi-reaction method. The ionization mass-to- m / z) were 283.2 / 267.9 and 267.0 / 251.9, respectively. A Phenomenex Gemini 110 C18 column (50 mm × 2.0 mm, 5 μL) was used. The mobile phase consisted of methanol-0.1% formic acid water (85:15) with isocratic elution. The column temperature was 40 ℃ and the flow rate was 0.3 mL · min -1. Results The pharmacokinetic-time curve of Daphne genkwa extract in rats was in accordance with the two-compartment model. The linear range of the range of 5-1000 ng · mL-1 was for rhamnothionine (r2 = 0.998) and the lowest detection limit was LOQ was 0.5 ng · mL-1, the intra-and inter-day precision was 2.42% -10.71%, intra-day and inter-day accuracy was 95.67% -112.15%, and no endogenous matrix interference and stability good. Conclusion The method established in this study is simple, sensitive, reproducible and rapid in analysis. It can be used to determine the plasma concentration of genkwanin and pharmacokinetics in rats.