Kitani M, Miyamoto G, Odomi M
Tokushima Research Institute, Otsuka Pharmaceutical Co., Ltd., Japan.
J Chromatogr. 1993 Oct 22;620(1):97-104. doi: 10.1016/0378-4347(93)80056-a.
A high-performance liquid chromatographic assay method for the quantification of OPC-18790 enantiomers in human plasma and urine is described. A human plasma or urine was extracted with organic solvent under alkaline conditions following the addition of internal standard. The enantiomers and internal standard were then derivatized by reaction with the chiral reagent GITC (2,3,4,6-tetra-O-acetyl-beta-D-glucopyranosyl isothiocyanate), followed by octadecylsilica chromatographic separation of the diastereomeric products. The mobile phase consisted of acetonitrile-water (41:59). The fluorescence of the eluate was monitored at 355/405 nm. The lowest quantification limit of each enantiomer was 10 ng/ml in plasma and 0.1 micrograms/ml in urine. Both intra- and inter-day coefficients of variation were below 10%. The assay is sensitive, specific and applicable for stereoselective pharmacokinetic studies in human.
描述了一种用于定量人血浆和尿液中OPC-18790对映体的高效液相色谱分析方法。加入内标后，在碱性条件下用有机溶剂萃取人血浆或尿液。然后，对映体和内标与手性试剂GITC（2,3,4,6-四-O-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯）反应进行衍生化，接着对非对映体产物进行十八烷基硅胶色谱分离。流动相由乙腈-水（41:59）组成。在355/405nm处监测洗脱液的荧光。各对映体在血浆中的最低定量限为10ng/ml，在尿液中的最低定量限为0.1μg/ml。日内和日间变异系数均低于10%。该分析方法灵敏、特异，适用于人体立体选择性药代动力学研究。
