【摘要】 目的建立测定人血浆中长春氟宁(抗肿瘤药)浓度的高效液相色谱-质谱联用方法(LC-MS/MS)。方法以XB-CN柱(5μm,4.6 mm×100mm)为色谱柱,流动相为0.02mo·lL-1乙酸胺(pH=3.0)-乙腈=20∶80,流量为200μL·min-1,以液-液萃取方法提取血浆样品中的长春氟宁,样本经ESI源正离子化后,通过API2000三级四极杆串联质谱仪,用多反应离子监测方式(MRM)对长春氟宁(m/z:817.60/160.10)进行测定,并将此方法应用于测定中国肿瘤患者血中长春氟宁浓度。结果长春氟宁的血浆药物浓度在5～1000ng·mL-1线性良好,y=6.01-5.03×10-2x(γ=0.9958),低、中、高浓度(15,500,800ng·mL-1)的绝对回收率分别为81.08%,94.31%,88.06%,批内、批间精密度良好(RSD<10%)。结论该方法稳定、准确、灵敏、快速、特异性强,可用于该药临床药代动力学特征的研究。更多还原

【Abstract】 Objective To establish a HPLC-MS/MS method in order to determine vinflunine in human plasma.Methods The XB-CN(5 μm,4.6 mm×100 mm) was used as analytical column with a mobile phase consisted a mixture of ammonium acetate(0.02 mol·L-1,pH=3.0) and acetonitrile(20∶80),the flow rate was 200 μL·min-1.The plasma sample was wiped off protein with methyl tert-butyl ether(MTBE).Quantification was performed by a Perkin Elmer Sciex API 2000 tandem mass spectrometer with positive ion MS/MS employing a TurboIonSpray interface.Vinflunine was monitored using m/z 817.60 as the precursor ion and m/z 160.10 as the product ion.This method was used to measure vinflunine in plasma of Chinese cancer patients.Results The linear range was 5-1 000 ng·mL-1,y=6.01-5.03×10-2x(γ=0.9958) for vinflunine in human plasma.The absolute recovery of 15,500 and 800 ng·mL-1 was 81.08%,94.31%,88.06%,respectively.The intra-batch and inter-batch deviations were in high precision(RSD<10%).Conclusion The method is proved to be stable,sensitive,accurate,rapid,specific,and suitable for the clinical pharmacokinetics study.更多还原