Drug Metabolism and Bioanalysis Laboratory, College of Pharmacy, Wonkwang University, Iksan, Korea.
J Sep Sci. 2010 Mar;33(6-7):948-54. doi: 10.1002/jssc.200900674.
A rapid, selective and sensitive method for the determination of lamivudine in human plasma was developed using hydrophilic interaction chromatography-MS/MS. This method involved protein precipitation with acetonitrile as sample preparation procedure. Lamivudine and famotidine (internal standard) were analyzed on a Luna hydrophilic interaction chromatography column with the mobile phase of acetonitrile/10 mM ammonium formate (95:5, v/v) and detected using electrospray ionization mass spectrometry in the selected reaction monitoring mode. The standard curve was linear (r(2)=0.9985) over the concentration range of 50-3000 ng/mL. The lower limit of quantification was 50 ng/mL using 50 microL of plasma sample. The coefficient of variation and relative error for intra- and inter-assay at four quality control levels were 2.1-7.5 and -4.0 to 3.3%, respectively. The absolute and relative matrix effects for lamivudine and famotidine were practically absent. The present method was successfully applied to the pharmacokinetic study of lamivudine after oral dosing of lamivudine (100 mg tablet) to male healthy volunteers.
建立了一种快速、选择性和灵敏的人血浆中拉米夫定的亲水作用色谱-MS/MS 测定方法。该方法采用乙腈沉淀蛋白作为样品前处理方法。拉米夫定和法莫替丁（内标）在 Luna 亲水作用色谱柱上进行分析，流动相为乙腈/10 mM 甲酸铵（95:5，v/v），采用电喷雾电离质谱在选择反应监测模式下进行检测。标准曲线在 50-3000 ng/mL 浓度范围内呈线性（r(2)=0.9985）。使用 50 μL 血浆样品，定量下限为 50 ng/mL。四个质控水平的日内和日间精密度的变异系数和相对误差分别为 2.1-7.5%和-4.0 至 3.3%。拉米夫定和法莫替丁的绝对和相对基质效应实际上不存在。本方法成功应用于男性健康志愿者口服拉米夫定（100mg 片剂）后拉米夫定的药代动力学研究。
