超快速液相色谱-串联质谱法测定胎盘灌流液中拉米夫定的浓度

Determination of Lamivudine in Placental Perfusate by Employing Ultra Fast Liquid Chromatography with Tandem Mass Spectrometry

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-packXR—ODSIICIs柱（2．0mm×75mm，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0．4mL·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1～2500ng·mL-1间线性良好，日内日间精密度〈10％，绝对回收率I〉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 develop a method for determining the concentration of lamivudine in placental perfusate by emplo- ying ultra fast liquid chromatography with tandem mass spectrometry （UFLC-MS/MS）. METHODS Famotidine was used as the in- ternal standard. After protein precipitation with acetonitrile, the chromatography was performed on a Shim-pack XR-ODS II Cis column （2. 0 mm ×75 mm,2. 2μm） with mobile phase consisting of methanol and 10 mmol · L-1 ammonium acetate, gradient elution was used, and the flow rate was 0. 4 mL · min-1. Tandem mass spectrometric detection was conducted by using multiple reaction monito- ring （MRM） in positive ionization mode with an electrospray ionization interface. RESULTS The calibration curve of lamivudine was linear in the range of 1 -2 500 ng · mL-I. The intra- and inter-batch RSDs were less than 10%. The method recovery was more than 72%. CONCLUSION The method is rapid and accurate, which is suitable for the determination of lamivudine in placental perfusate.