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目的建立测定人血浆中阿奇霉素浓度的高效液相色谱电化学(HPLC-ECD)检测法。方法采用ZORBAX XDB-C18柱(Agilent 150 mm×4.6 mm,5μm)进行分离;以乙腈-50 mmol.L-1KH2PO4-K2HPO4缓冲液(pH=7.0)(70∶30,V/V)为流动相;流速为1.0 mL.min-1;柱温为45.0℃;ESA CoulochemⅢ型电化学检测器检测,电压650 mV。以克拉霉素为内标,待测血浆经乙腈沉淀后,上清液氮气吹干,用定量流动相溶解后进样。结果本法线性关系良好(r=0.999 9),线性范围10~1 000μg.L-1,定量下限为10μg.L-1,回归方程ρ=6.132 8Ai/As-0.019 5;相对回收率均在85%~115%内,绝对回收率>75%;日间、日内精密度RSD均<10%。结论该法简便、灵敏、特异,适用于人体药动学及治疗药物检测的研究。
OBJECTIVE To establish a high performance liquid chromatography-electrochemical (HPLC-ECD) method for the determination of azithromycin in human plasma. Methods The separation was performed on a ZORBAX XDB-C18 column (Agilent 150 mm × 4.6 mm, 5 μm). The mobile phase was acetonitrile-50 mmol.L-1 KH2PO4-K2HPO4 buffer (pH = 7.0) ; Flow rate of 1.0 mL.min-1; column temperature of 45.0 ℃; ESA Coulochem Ⅲ electrochemical detector detection voltage of 650 mV. To clarithromycin as the internal standard, the plasma was measured after precipitation by acetonitrile, the supernatant was dried with nitrogen, dissolved with a quantitative mobile phase injection. Results The linear relationship was good (r = 0.999 9), the linear range was 10-1 000 μg.L-1, the lower limit of quantification was 10 μg.L-1, the regression equation ρ = 6.132 8Ai / As-0.019 5; 85% ~ 115%, the absolute recovery rate> 75%; intraday, intraday precision RSD <10%. Conclusion The method is simple, sensitive and specific, suitable for human pharmacokinetics and therapeutic drug testing.