Venkatesh Gantala, Majid M I A, Ramanathan S, Mansor S M, Nair N K, Croft Simon L, Navaratnam V
Centre for Drug Research, Universiti Sains Malaysia, 11800 Penang, Malaysia.
Biomed Chromatogr. 2008 May;22(5):535-41. doi: 10.1002/bmc.965.
A simple, sensitive and specific reversed-phase high-performance liquid chromatographic method with UV detection at 251 nm was developed for quantitation of buparvaquone (BPQ) in human and rabbit plasma. The method utilizes 250 microL of plasma and sample preparation involves protein precipitation followed by solid-phase extraction. The method was validated on a C18 column with mobile phase consisting of ammonium acetate buffer (0.02 m, pH 3.0) and acetonitrile in the ratio of 18:82 (v/v) at a flow rate of 1.1 mL/min. The calibration curves were linear (correlation coefficient>or=0.998) in the selected range. The method is specific and sensitive with limit of quantitation of 50 ng/mL for BPQ. The validated method was found to be accurate and precise in the working calibration range. Stability studies were carried out at different storage conditions and BPQ was found to be stable. Partial validation studies were carried out using rabbit plasma and intra- and inter-day precision and accuracy were within 7%. This method is simple, reliable and can be routinely used for preclinical pharmacokinetic studies for BPQ.
建立了一种简单、灵敏且特异的反相高效液相色谱法，用于在251 nm处进行紫外检测，以定量人血浆和兔血浆中的布帕喹酮（BPQ）。该方法使用250微升血浆，样品制备包括蛋白质沉淀，然后进行固相萃取。该方法在C18柱上进行验证，流动相由醋酸铵缓冲液（0.02 m，pH 3.0）和乙腈按18:82（v/v）的比例组成，流速为1.1 mL/min。在选定范围内，校准曲线呈线性（相关系数≥0.998）。该方法特异且灵敏，BPQ的定量限为50 ng/mL。验证后的方法在工作校准范围内准确且精密。在不同储存条件下进行了稳定性研究，发现BPQ是稳定的。使用兔血浆进行了部分验证研究，日内和日间精密度及准确度均在7%以内。该方法简单、可靠，可常规用于BPQ的临床前药代动力学研究。
