Gong Xiaobin, Yang Le, Zhang Feng, Liang Youtian, Gao Shouhong, Liu Ke, Chen Wansheng
Department of Pharmacy, Changzheng Hospital, Second Military Medical University, Shanghai, People's Republic of China.
Department of Oncology, Changzheng Hospital, Second Military Medical University, Shanghai, People's Republic of China.
Biomed Chromatogr. 2017 Nov;31(11). doi: 10.1002/bmc.3989. Epub 2017 Jun 15.
A fully valid UHPLC-MS/MS method was developed for the determination of etoposide, gemcitabine, vinorelbine and their metabolites (etoposide catechol, 2',2'-difluorodeoxyuridine and 4-O-deacetylvinorelbine) in human plasma. The multiple reaction monitoring mode was performed with an electrospray ionization interface operating in both the positive and negative ion modes per compound. The method required only 100 μL plasma with a one-step simple de-proteinization procedure, and a short run time of 7.5 min per sample. A Waters ACQUITY UPLC HSS T3 column (2.1 × 100 mm, 1.8 μm) provided chromatographic separation of analytes using a binary mobile phase gradient (A, 0.1% formic acid in acetonitrile, v/v; B, 0.1% formic acid in water, v/v). Linear coefficients of correlation were >0.995 for all analytes. The relative deviation of this method was <10% for intra- and inter-day assays and the accuracy ranged between 86.35% and 113.44%. The mean extraction recovery and matrix effect of all the analytes were 62.07-105.46% and 93.67-105.87%, respectively. This method was successfully applied to clinical samples from patients with lung cancer.
建立了一种完全有效的超高效液相色谱-串联质谱法（UHPLC-MS/MS），用于测定人血浆中依托泊苷、吉西他滨、长春瑞滨及其代谢物（依托泊苷儿茶酚、2',2'-二氟脱氧尿苷和4-O-去乙酰长春瑞滨）。采用多反应监测模式，每个化合物的电喷雾电离接口在正离子和负离子模式下运行。该方法仅需100μL血浆，采用一步简单的去蛋白程序，每个样品的运行时间短至7.5分钟。使用沃特世ACQUITY UPLC HSS T3色谱柱（2.1×100mm，1.8μm），采用二元流动相梯度（A，乙腈中0.1%甲酸，v/v；B，水中0.1%甲酸，v/v）对分析物进行色谱分离。所有分析物的线性相关系数均>0.995。该方法日内和日间测定的相对偏差<10%，准确度在86.35%至113.44%之间。所有分析物的平均提取回收率和基质效应分别为62.07 - 105.46%和93.67 - 105.87%。该方法已成功应用于肺癌患者的临床样本。
