高效液相色谱-串联质谱法测定中国肿瘤患者血浆中长春氟宁的浓度  

Determination of vinflunine concentration in Chinese cancer patients by LC-MS/MS

作　　者：詹靖[1,2] 李苏[1,3] 廖海[1,4] 邓丽婷[1,4] 

机构地区：[1]华南肿瘤学国家重点实验室,广州510060 [2]中山大学肿学肿瘤防治中心,广州510060 [3]中山大瘤防治中心,广州510060 [4]中山大学肿瘤防治中心,广州510060

出　　处：《中国临床药理学杂志》2010年第6期450-453,共4页The Chinese Journal of Clinical Pharmacology

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。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 （ MT- BE）. Quantification was performed by a Perkin Elmer Sciex API 2000 tandem mass spectrometer with positive ion MS/MS employing a TurboI- onSpray 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.

关 键 词：高效液相色谱-质谱联用法 长春氟宁 血浆药物浓度 

分 类 号：R969.1[医药卫生—药理学] R979.1[医药卫生—药学]