HPLC-MS法测定人血浆中克拉霉素

HPLC-MS determination of clarithromycin in the human plasma

目的建立HPLC-MS测定人血浆中克拉霉素的方法，并用于药物动力学研究。方法采用Thermo C18柱（150mm×2．1mm，5μm），柱温45℃，流动相为乙腈-15mmol·L^-1醋酸铵水溶液（含0．5％甲酸，0．1％三氟乙酸）（42：58），流速0．35mL·min^-1；以罗红霉素为内标，采用电喷雾电离正源，选择性离子方式检测。克拉霉素及内标用于定量分析的离子分别为m／z 748．6、m／z 837．8。血浆样品用甲醇沉淀蛋白后进样。结果克拉霉素在12．1～3400．0ng·mL^-1线性关系良好，相关系数为0．9999，最低检测限为2．0ng·mL^-1.萃取回收率〉83．0％，方法回收率103．7％～106．7％，日内日间精密度均〈7．9％。结论该方法结果准确、灵敏度高，适用于克拉霉素药物动力学和生物等效性研究。

Objective To establish an HPLC-MS method for the and to study the pharmacokinetics of clarithromycin. Methods determination of clarithromycin in the human plasma The analytes were determined by HPLC-MS method using Thermo C18 column （150 mm× 2.1 mm, 5 μm）, acetonitrile-15 mmol · L^-1 ammonium acetate solution with 0.5% formic acid and 0.1% trifluoroacetic acid （ 42 ： 58） as the mobile phase at 0.35 mL · min^-1 , with positive ion SIM detection of clarithromycin （m/z=748.6）, using roxithromycin （m/z=837.8） the internal standard. The column temperature was 45℃. The plasma was deposited by methanol directly. Results The calibration curve was linear within 12.1-3 400.0 ng · mL^-1 （r =0. 999 9）. The limit of quantitation was 2. 0 ng · mL^-1. The extraction recovery was 〉83.0% and the method recovery was 103.7%-106.7%. The relative standard deviations for the intra-day and inter-day were 〈7.9%. Conclusion The method is simple, accurate, fast and sensitive and suitable for the pharmacokinetics and bioequivalence study of clarithromycin.