Kubo Masanori, Mizooku Yasuo, Hirao Yukihiro, Osumi Takahiko
Clinical Pharmacology, Department of Clinical Research & Development, Otsuka Pharmaceutical Co., Ltd., 3-2-27, Otedori, Chuo-ku, Osaka 540-0021, Japan.
J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Aug 5;822(1-2):294-9. doi: 10.1016/j.jchromb.2005.06.023.
An accurate, sensitive, reproducible, and selective liquid chromatography/tandem mass spectrometry (LC-MS/MS) method for determination of aripiprazole and its main metabolite, OPC-14857, in human plasma was developed and validated. Chromatographic separation was achieved isocratically on a C18 reversed-phase column within 7.5 min. The calibration curve, ranging from 0.1 to 100 ng/ml, was fitted to a 1/y2-weighted linear regression model. The assay showed no significant interference. Lower limit of quantitation (LLOQ) for both analytes was 0.1 ng/ml using 0.4 ml of plasma. Intra- and inter-assay precision and accuracy values for aripiprazole and OPC-14857 were within regulatory limits.
建立并验证了一种准确、灵敏、可重现且具选择性的液相色谱/串联质谱（LC-MS/MS）法，用于测定人血浆中阿立哌唑及其主要代谢物OPC-14857。在C18反相柱上以等度洗脱方式于7.5分钟内实现色谱分离。校准曲线范围为0.1至100 ng/ml，采用1/y2加权线性回归模型拟合。该测定法无显著干扰。使用0.4 ml血浆时，两种分析物的定量下限（LLOQ）均为0.1 ng/ml。阿立哌唑和OPC-14857的批内和批间精密度及准确度值均在规定范围内。
