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目的应用高效液相色谱-串联质谱联用(LC-MS/MS)法建立大鼠尿液中朝藿定A、B、C及淫羊藿苷的同时测定方法,初步探讨淫羊藿提取物在大鼠体内的排泄规律。方法以人参皂苷Rg1为内标,选用Agilent Eclipse XDB-C_(18)色谱柱(2.1 mm×150 mm,5μm);流动相:乙腈-0.1%乙酸水(30∶70);流速:0.3 m L·min~(-1);柱温:40℃;采用电喷雾离子源(ESI)负离子多反应检测(MRM)模式测定。结果朝藿定A、B、C以及淫羊藿苷在1~500 ng·m L~(-1)浓度范围内线性关系良好,日内精密度(RSD)均小于7.4%,日间精密度(RSD)均小于12.7%。大鼠口服灌胃给予淫羊藿提取物36 h后朝藿定A、B、C及淫羊藿苷的平均尿累积排泄量/给药量比值不超过0.27‰,0.20‰,0.30‰和0.43‰。结论本研究建立的LC-MS/MS方法简便灵敏快速,适用于尿液中朝藿定A、B、C以及淫羊藿苷的同时测定及淫羊藿提取物尿排泄动力学研究的应用,研究结果显示淫羊藿提取物原形药物基本不经尿液排泄,提示肾排泄不是其主要消除途径。
OBJECTIVE To establish a method for the simultaneous determination of Buyouding A, B, C and icariin in rat urine by high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) Excretion rules in rats. Methods Ginsenoside Rg1 was used as an internal standard and Agilent Eclipse XDB-C 18 column (2.1 mm × 150 mm, 5 μm) was used. The mobile phase consisted of acetonitrile and 0.1% acetic acid (30:70). The flow rate was 0.3 m L · Min ~ (-1); column temperature: 40 ℃; determined by electrospray ionization (ESI) negative ion multiple reaction detection (MRM) mode. Results The concentrations of A, B, C and Icariin in the concentration range of 1 ~ 500 ng · m L -1 were good. The intra-day precision (RSD) was less than 7.4%. The intra-day precision RSD) were less than 12.7%. The mean urine excretion / administration dose of epimedin A, B, C and icariin after oral gavage of epimedium extract in rats for 36 h did not exceed 0.27 ‰, 0.20 ‰, 0.30 ‰ and 0.43 ‰. Conclusion The LC-MS / MS method established in this study is simple, sensitive and rapid and is suitable for the simultaneous determination of somatostatin A, B, C and icariin in urine and urinary excretion dynamics of Epimedium extract. The results show that the essential oil of Epimedium extract is essentially excreted without urine, suggesting that renal excretion is not the main way to eliminate it.