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目的建立HPLC-MS/MS方法定量测定人血浆中阿比朵尔浓度。方法用蛋白沉淀处理血浆,以阿比朵尔-d_6为内标,色谱柱:Agilent Eclipse XDB-C_(18)柱(2.1 mm×150 mm,5μm),柱温:30℃,流动相:甲醇-0.1%甲酸水溶液,梯度洗脱,流速:0.25 mL·min~(-1)。用正离子扫描,多反应监测方式(MRM)测定样品中药物的质量浓度。考察该方法的专属性、标准曲线与定量下限、精密度与回收率、基质效应和稳定性。结果血浆样品中阿比朵尔回归方程为y=1.52×10~(-1)x-1.38×10~(-3)(r=0.999 7),阿比朵尔在10~1000 ng·mL~(-1)内线性关系良好,定量下限为10 ng·mL~(-1)。日内、日间精密度的RSD均<15%,平均回收率>95%,稳定性较好。结论本方法简便快速、特异性强、灵敏准确,适用于人体血浆中阿比朵尔浓度的测定。
Objective To establish a HPLC-MS / MS method for the quantitative determination of abidol in human plasma. Methods Serum was precipitated with protein and treated with abidol-d 6 as the internal standard. The column was Agilent Eclipse XDB-C 18 column (2.1 mm × 150 mm, 5 μm). The column temperature was 30 ℃ and the mobile phase was methanol -0.1% aqueous formic acid, gradient elution, flow rate: 0.25 mL · min ~ (-1). The mass concentration of the drug in the sample was determined by positive ion scanning and multiple reaction monitoring (MRM). Investigate the specificity of this method, the standard curve and lower limit of quantitation, precision and recovery, matrix effect and stability. Results The Abbott regression equation for plasma samples was y = 1.52 × 10 ~ (-1) x-1.38 × 10 ~ (-3) (r = 0.999 7) (-1). The lower limit of quantification was 10 ng · mL -1. The intra-day and inter-day precision RSD were <15%, the average recovery rate> 95%, good stability. Conclusion The method is simple, rapid, specific, sensitive and accurate and suitable for the determination of abidol in human plasma.