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目的:建立高效液相色谱-质谱联用法测定人血浆中拉米夫定的浓度,并研究拉米夫定胶囊在健康人体的药动学。方法:血浆样品以法莫替丁作为内标,经1mol·L-1碳酸钠溶液碱化,异丙醇-醋酸乙酯(20∶80)萃取,以LC-MS法进行分析。色谱条件为Kromasil C18柱(150mm×4.6mm,5μm),甲醇-甲酸水(0.2%)为流动相,进行梯度洗脱。以电喷雾离子源(ESI源),正离子方式检测:扫描方式为选择离子监测(SIM),用于定量分析的离子分别为m/z230.05(拉米夫定)和m/z338.05(法莫替丁)。结果:测定血浆中拉米夫定在10～2500μg·L-1范围内线性关系良好,定量下限(LLOQ)为10μg·L-1,日内、日间精密度(RSD)均小于10.0%,拉米夫定提取回收率在73.8%～84.4%,RSD均小于10.0%。结论:该方法灵敏度高、专属性强,适用于人血浆中拉米夫定浓度的测定。
Objective: To establish a method for the determination of lamivudine in human plasma by high performance liquid chromatography-mass spectrometry (HPLC-MS) and to study the pharmacokinetics of lamivudine in healthy volunteers. Methods: Plasma samples were treated with famotidine as internal standard and alkalified in 1mol·L-1 sodium carbonate solution and extracted with isopropanol-ethyl acetate (20:80). The plasma samples were analyzed by LC-MS. The chromatographic conditions were Kromasil C18 column (150 mm × 4.6 mm, 5 μm) and methanol-formic acid water (0.2%) as the mobile phase, gradient elution. Electrospray ionization (ESI source), positive ion detection: The scanning mode was selected ion monitoring (SIM), and the ions for quantitative analysis were m / z 230.05 (lamivudine) and m / z 338.05 (Famotidine). Results: The linearity of lamivudine in plasma ranged from 10 to 2500 μg · L-1, the LLOQ was 10 μg · L-1, and the intra-day and inter-day precision was less than 10.0% The recovery of mifuding was between 73.8% and 84.4% with RSD less than 10.0%. Conclusion: This method has high sensitivity and specificity and is suitable for the determination of lamivudine concentration in human plasma.