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目的建立高效液相色谱-质谱联用法(HPLC-MS/MS)定量测定人血浆中比卡鲁胺的浓度。方法用蛋白沉淀处理血浆,以比卡鲁胺-d4为内标,色谱柱:Agilent ZORBAX SB-C18柱(2.1 mm×50.0 mm,3.5μm),柱温:20℃,流动相:甲醇-0.1%甲酸+2 mmol·L-1甲酸铵水溶液,等度洗脱,流速:0.35m L·min~(-1)。用负离子扫描模式,多反应监测方式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。结果血浆样品中比卡鲁胺回归方程为y=6.82×10~(-3)x+1.33×10~(-2)(r=0.999 1)。比卡鲁胺在10~1500 ng·mL~(-1)内线性关系良好,定量下限为10ng·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,适用于人体血浆中比卡鲁胺浓度的测定。
Objective To establish a method for the quantitative determination of bicalutamide in human plasma by high performance liquid chromatography-mass spectrometry (HPLC-MS / MS). Methods The plasma was treated with protein precipitation and the internal standard was bicalutamide-d4. The column was Agilent ZORBAX SB-C18 column (2.1 mm × 50.0 mm, 3.5 μm). The column temperature was 20 ℃ and the mobile phase was methanol-0.1 % Formic acid +2 mmol·L-1 ammonium formate solution, isocratic elution, flow rate: 0.35m L · min -1. Negative ion scan mode, multi-reaction monitoring method to determine the sample mass concentration of the drug. Investigate the specificity of this method, the standard curve and lower limit of quantitation, precision and recovery, matrix effect and stability. Results The regression equation of bicalutamide in plasma was y = 6.82 × 10 ~ (-3) x + 1.33 × 10 ~ (-2) (r = 0.999 1). The linearity of bicalutamide in 10 ~ 1500 ng · mL ~ (-1) was good, and 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 bicalutamide in human plasma.