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目的建立高效液相色谱-串联质谱法同时测定人血浆中阿米卡星、地塞米松和利巴韦林浓度的分析方法。方法血浆样品经甲醇沉淀蛋白,以卡那霉素为内标,采用Inertsil HILIC柱(2.1 mm×150 mm,3.5μm)分离,流动相组成包括乙腈(含体积分数0.1%甲酸)和水(含体积分数0.1%甲酸),梯度洗脱,流速0.4 m L·min~(-1)。通过电喷雾离子化,采用正离子检测。结果阿米卡星、地塞米松和利巴韦林的线性范围分别为1.038~1 038,1.063~1 063,1.029~1 029 ng·m L~(-1),相关系数(r≥0.99),定量下限分别为1.038,1.063,1.029 ng·m L~(-1)。日内及日间精密度小于13.7%,准确度的相对误差(RE)在-9.2%~10.9%。结论该方法高效、灵敏、特异性强,准确度、精密度好,适用于阿米卡星、地塞米松和利巴韦林药物动力学分析实验。
Objective To establish a method for simultaneous determination of amikacin, dexamethasone and ribavirin in human plasma by high performance liquid chromatography-tandem mass spectrometry. Methods Plasma samples were precipitated with methanol and kanamycin was used as an internal standard. The separated samples were separated on an Inertsil HILIC column (2.1 mm × 150 mm, 3.5 μm). The mobile phase consisted of acetonitrile (containing 0.1% formic acid by volume) and water Volume fraction of 0.1% formic acid), gradient elution, flow rate 0.4 m L · min -1. Electrospray ionization, positive ion detection. Results The linear ranges of amikacin, dexamethasone and ribavirin were 1.038 ~ 1.038, 1.063 ~ 1063 and 1.029 ~ 1029 ng · m L -1, respectively. The correlation coefficient (r ≥ 0.99) , Lower limit of quantitation were 1.038, 1.063 and 1.029 ng · m L -1, respectively. The intra- and inter-day precision was less than 13.7% and the relative accuracy (RE) was -9.2% -10.9%. Conclusion The method is efficient, sensitive, specific, accurate and precise and suitable for pharmacokinetic analysis of amikacin, dexamethasone and ribavirin.