论文部分内容阅读
目的建立液相-质谱(LC-MS)联用方法,用于抗肿瘤药卢比替康在肿瘤患者血浆中的定量分析。方法血浆样品用0.2 mL盐酸(0.5 mol·L~(-1))酸化后,乙酸乙酯提取,上清液在40℃水浴条件下氮气流吹干,萃取物用流动相复溶后进LC-MS联用仪分析测定。采用反相C_(18)柱进行色谱分离,流动相为:乙腈:10 mmol·L~(-1)醋酸铵水溶液(90:10,V/V)。结果本方法在5～500μg·L~(-1)内线性良好,r=0.999 4(n=4),低、中、高3种浓度质控样品的批内及批间RSD均<5%,提取回收率分别为80.66%、88.47%、85.05%,最低定量限5μg·L~(-1)。结论本方法灵敏度高,操作简便易行,能够满足该药进行临床药动学研究的要求。
Objective To establish a liquid chromatography-mass spectrometry (LC-MS) method for the quantitative analysis of the antitumor drug lubitecan in the plasma of cancer patients. Methods The plasma was acidified with 0.2 mol hydrochloric acid (0.5 mol·L -1) and extracted with ethyl acetate. The supernatant was dried under a stream of water at 40 ° C under nitrogen flow. The extract was reconstituted with a mobile phase of LC- MS analyzer analysis and determination. Chromatographic separation was performed on an reversed-phase C_ (18) column with acetonitrile: 10 mmol·L -1 ammonium acetate aqueous solution (90:10, V / V). Results The method showed a good linearity within 5 ~ 500μg · L -1, r = 0.999 4 (n = 4). The intra-and inter-assay RSD of low, medium and high quality control samples were all less than 5% The recoveries were 80.66%, 88.47% and 85.05%, respectively. The lowest limit of quantification was 5μg · L -1. Conclusion The method is sensitive, easy to operate and can meet the requirement of clinical pharmacokinetics study.