Department of Hospital and Clinical Pharmacy, University Medical Center Groningen, University of Groningen, PO Box 30.001, 9700 RB Groningen, The Netherlands.
Talanta. 2012 Jan 15;88:385-90. doi: 10.1016/j.talanta.2011.11.004. Epub 2011 Nov 6.
A method has been developed for the determination of ribavirin in human serum for therapeutic drug monitoring purposes, using liquid chromatography electrospray ionization mass spectrometry. Separation was obtained with a mobile phase gradient starting and ending in 100% aqueous conditions using a Waters Atlantis® T3 column (100×2mm, 3μm). The entire sample preparation consisted of dilution, followed by ultrafiltration. From the clear ultrafiltrate 5μL was injected on the LC-MS/MS system. The calibration curves were linear in the range of 0.2-10mg/L with within-run and between-run precisions (CVs) in the range of 0-10%. The method was validated with respect to specificity, selectivity, linearity, accuracy, precision, recovery and stability and meets the requirements of the FDA. The method was extensively tested for matrix effects by determining the variation of the slopes of calibration curves in different sources of serum and plasma. This method is suitable for the determination of ribavirin in human serum for therapeutic drug monitoring.
建立了一种用于治疗药物监测目的的人血清中利巴韦林的测定方法,采用液相色谱-电喷雾电离质谱法。使用 Waters Atlantis® T3 柱(100×2mm,3μm),以 100%水条件开始和结束的流动相梯度实现分离。整个样品制备包括稀释,然后进行超滤。从澄清的超滤物中取 5μL 注入 LC-MS/MS 系统。校准曲线在 0.2-10mg/L 范围内呈线性,批内和批间精密度(CV)在 0-10%范围内。该方法经过特异性、选择性、线性、准确性、精密度、回收率和稳定性验证,符合 FDA 的要求。通过确定不同来源的血清和血浆中校准曲线斜率的变化,对基质效应进行了广泛的测试。该方法适用于治疗药物监测中测定人血清中的利巴韦林。