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目的建立超快速液相色谱-串联质谱(UPLC-MS/MS)法检测胎盘灌流液中拉米夫定的浓度。方法以法莫替丁为内标,胎盘灌流液样本用乙腈沉淀蛋白处理,采用Shim-pack XR-ODS II C18柱(2.0 mm×75 mm,2.2μm)为分析柱,以甲醇和10mmol·L-1醋酸铵溶液为流动相进行梯度洗脱,流速为0.4 mL·min-1,采用离子选择性电极离子源正离子模式,多反应监测进行定量分析。结果本法在1~2 500 ng·mL-1间线性良好,日内日间精密度<10%,绝对回收率≥72%。结论本方法快速可靠,结果准确,适用于生物样本中拉米夫定浓度的测定。
Objective To establish a method for the determination of lamivudine in placental perfusate by ultra-fast liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods Famotidine was used as an internal standard. The samples of placental perfusate were treated with acetonitrile-precipitated protein and analyzed by Shim-pack XR-ODS II C18 column (2.0 mm × 75 mm, 2.2 μm) with methanol and 10 mmol·L -1 ammonium acetate solution was used as the mobile phase. The flow rate was 0.4 mL · min-1, and the ion-selective ion source positive ion mode was used. The multi-reaction monitoring was used for quantitative analysis. Results The method was linear in the range of 1-2 500 ng · mL-1 with a precision of <10% within days and days and an absolute recovery of ≥72%. Conclusion The method is rapid and reliable with accurate results and is suitable for the determination of lamivudine in biological samples.