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目的RP-HPLC内标法建立大鼠血清中红景天苷浓度的测定方法。方法健康♂SD大鼠尾静脉注射红景天苷(60mg·kg-1)后,分别于不同时间点眼眶静脉丛取血0.5mL,高氯酸沉淀血清蛋白,离心取上清液进样分析。色谱柱为SHIMADZU C18柱(4.6mm×250mm,5μm),流动相为乙腈-水-三乙胺-冰醋酸(10∶90∶0.011∶0.016),流速为1.5mL·min-1,检测波长为277nm,柱温为50℃,进样量10μL,内标为咖啡因。结果红景天苷质量浓度在0.56~70mg·L-1内线性关系良好(r=0.9975),以信号/噪音=3∶1计算,红景天苷最低检测浓度为0.15mg·L-1,日内、日间精密度分别≤4.5%,≤5.4%,血清样品的平均回收率为(99.27±4.38)%。结论建立的RP-HPLC内标法方法简便、快速、准确,适合于红景天苷的血药浓度测定及药动学研究。
Objective To establish a method for the determination of salidroside in rat serum by RP-HPLC internal standard method. METHODS: After healthy rats were injected with salidroside (60 mg·kg-1) via tail vein, 0.5 mL blood was taken from the orbital venous plexus at different time points. Serum albumin was perchloric acid precipitated, and the supernatant was centrifuged for analysis. . The column was SHIMADZU C18 column (4.6mm×250mm, 5μm), the mobile phase was acetonitrile-water-triethylamine-glacial acetic acid (10∶90∶0.011∶0.016), the flow rate was 1.5mL·min-1, and the detection wavelength was At 277 nm, the column temperature was 50°C, the injection volume was 10 μL, and the internal standard was caffeine. Results The linear relationship between the mass concentration of salidroside was between 0.56 and 70 mg·L-1 (r=0.9975), the signal/noise ratio was 3:1, and the lowest concentration of salidroside was 0.15 mg·L-1. The intra-day and inter-day precisions were ≤4.5% and ≤5.4%, respectively. The average recovery rate of serum samples was (99.27±4.38)%. Conclusion The established RP-HPLC internal standard method is simple, rapid and accurate. It is suitable for the determination of plasma concentration and the pharmacokinetics of salidroside.