Woolf E, Fu I, Matuszewski B
Department of Drug Metabolism, Merck Research Laboratories, West Point, PA 19486, USA.
J Chromatogr B Biomed Sci Appl. 1999 Jul 9;730(2):221-7. doi: 10.1016/s0378-4347(99)00215-7.
A method for the determination of rofecoxib in human plasma is described. After the addition of an internal standard, buffered (pH 5) plasma samples are extracted with hexane-methylene chloride (50:50, v/v). The extracts are evaporated to dryness and reconstituted in mobile phase. Upon exposure to UV light, the analyte was found to undergo a stilbene-phenanthrene-like photocyclization reaction with the resulting formation of a highly fluorescent species. Thus, the plasma extracts were analyzed via HPLC with post-column photochemical derivatization and fluorescence detection. The assay has been validated in the concentration range of 0.5-100 ng/ml using 1-ml samples. The method has been successfully utilized to support human clinical pharmacokinetic studies.
描述了一种测定人血浆中罗非昔布的方法。加入内标后，用己烷 - 二氯甲烷（50:50，v/v）萃取缓冲（pH 5）的血浆样品。提取物蒸发至干并在流动相中复溶。在紫外光照射下，发现分析物会发生类似芪 - 菲的光环化反应，生成一种高荧光物质。因此，通过柱后光化学衍生化和荧光检测的高效液相色谱法对血浆提取物进行分析。该测定法在使用1 ml样品时，在0.5 - 100 ng/ml的浓度范围内得到验证。该方法已成功用于支持人体临床药代动力学研究。
