高效液相色谱-质谱联用法测定人体内血浆中的阿奇霉素

High performance liquid chromatography-mass pectrometry determination of azithromycin in human plasma

目的:建立一种简便、快速的高效液相色谱质谱联用法测定人体内血浆中的阿奇霉素浓度的方法。方法:采用HyPurityC18柱(2.1mm×150mm,5μm),柱温40°C,流动相为10mmol·L-1醋酸铵(pH5.2)∶乙腈∶甲醇(50∶40∶10),流速为0.2mL·min-1,质谱条件采用正离子检测的电喷雾接口(ESI),其喷雾电压4.5kV,选择性监测质荷比(M/Z)为375(阿奇霉素),749(克拉霉素)带正电荷的分子离子峰。结果:阿奇霉素最低定量限为3.91μg·L-1,线性范围3.91～1000μg·L-1(r=0.9993),日内和日间RSD均低于12%。结论:该方法灵敏度高、快速、简便、无杂质干扰,适合于阿奇霉素浓度检测以及生物等效性研究。

AIM: To establish a simple and rapid high performance liquid chromatography-mass pec trometry(HPLC-MS) method for determina tion of azithromycin in human plasma. METHODS: Chromatographic column was HyPu ri ty C_(18) (2.1 mm×150 mm, 5 μm) and (40 ℃) of column temperature. The mo bil e phas e consisted of 10 mmol·L^(-1) ammonium acetate(pH 5.2)-acetonitrile-methan o l(50 ∶40 ∶10) with a flow rate of 0.2 mL·min^(-1). Using selected ion mass s pectral (M/Z) 375 (azithromycin), 749 (clarithromycin) for quantitation. The voltage of electrospray ionization was 4.5 kV. RESULTS: The lower limit of qualification was 3.91 μg·L^(-1). T he calibration curve was in good linearity over the range of 3.91-1 000 μg·L ~ (-1) (r=(0.999 3)). The intra-day and inter-day RSD were less than 12 %. CONCLUSION: HPLC-MS is sensitive, rapid and suitable for the study of pharmacokinetics and bioequivalence of azithromycin.