UFLC-MS/MS测定人胎盘灌流液中齐多夫定浓度

Determination of Zidovudine in Placental Perfusate Fluid by UFLC-MS/MS

关键词:  齐多夫定  超快速液相-串联质谱法  胎盘灌流液

Key words:  zidovudine  UFLC-MS/MS  placental perfusate fluid

摘要:

目的 建立UFLC-MS/MS法测定人胎盘灌流液中齐多夫定浓度。方法 以米氮平为内标，采用蛋白沉淀的前处理方法，使用Synergi 4u Hydro-RP 80A分析柱(50 mm×2.00 mm，4 μm)，流动相A为含0.1%甲酸的水溶液，流动相B为甲醇，采用梯度洗脱，流速0.6 mL·min^-1。质谱采用电喷雾离子源(ESI)以多反应监测(MRM)扫描模式，在正离子电离模式下进行测定，齐多夫定和米氮平的定量分析离子分别为m/z 268.1/127.1和266.2/195.0。结果 齐多夫定在25~5 000 ng·mL^-1内线性关系良好，平均方法回收率90.5%~96.7%，日内及日间精密度RSD均<15%，稳定性考察结果良好。结论 该方法可用于人胎盘灌流液中齐多夫定浓度的检测。

Abstract:

OBJECTIVE To establish an UFLC-MS/MS method for determining the concentration of zidovudine in placental perfusate fluid. METHODS Mirtazapine was used as the internal standard, and samples were precipitated with acetonitrile. Analysis of zidovudine and mitrazapine was carried out on a Synergi 4u Hydro-RP 80A column(50 mm×2.00 mm, 4 μm). Gradient elution occurred using 0.1% formic acid-methanol at a flow rate of 0.6 mL·min^-1. Detection was performed with multiple reaction monitoring using positive electrospray ionization: m/z 268.1/127.1 for zidovudine and 266.2/195.0 for mirtazapine. RESULTS Linearities were obtained from 25-5 000 ng·mL^-1. The recoveries were 90.5%-96.7%. The intra-day RSD and inter-day RSD were all <15%. And the analytes were proved to be stable. CONCLUSION This method can be used for the determination of zidovudine in placental perfusate fluid.