摘要
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 determine human plasma by established HPLC the bicalutamide concentration in - MS/MS method. Methods The plasma was treated with protein precipitation, Bicalutamide -d4 was used as internal standard, chromatographic column： Agilent ZORBAX SB -Cls column （2. 1 mm xS0. 0 mm, 5 μm）, column temperature：20℃, mobile phase： methanol -0. 1% formic acid and 2 mmol · L-l ammonium formate, isocratic elution, flow rate ：0. 35 mL ·min - 1, mass concentration of the sample was measured with negative ion scan and multiple reaction monitoring mode. The specificity, lower limit of quantitation and standard curve, precision and recovery rate and stability as well as the matrix effect were investigated. Results The standard curve of bicalutamide was y = 6. 82 x 10-3 ＋ 1.33 x 10-2 （ r = 0. 999 1 ）, and has good linear relationship in 10 - 1500 ng·mL-1 , the lowest concentration was 10 ng ~ mL-1. Intra- day and inter- day RSD of blood samples were less than 15%, the average recovery was 〉 95%, and stability was good. Conclusion The method was simple, rapid, sensitive and accurate, specific, suitable for the determination of bicalutamide concentration in human plasma.
出处
《中国临床药理学杂志》
CAS
CSCD
北大核心
2017年第20期2065-2067,共3页
The Chinese Journal of Clinical Pharmacology
