Ishigai M, Asoh Y, Kumaki K
Drug Metabolism and Pharmacokinetic Laboratory, Chugai Pharmaceutical, Tokyo, Japan.
J Chromatogr B Biomed Sci Appl. 1998 Mar 20;706(2):261-7. doi: 10.1016/s0378-4347(97)00553-7.
A sensitive and specific liquid chromatographic-mass spectrometric assay has been developed for the determination of 22-oxacalcitriol (OCT), which is a new analog of 1alpha,25-dihydroxyvitamin D3. The analyte was isolated from serum by two solid-phase extraction steps on a C18 cartridge and NH2 cartridge. The recovery of OCT through two extraction steps was more than 90%. A related substance (ED-94), i.e. OCT with the side-chain shortened by one carbon, was used as an internal standard. Extracts were chromatographed on a C18 reversed-phase column interfaced to the electrospray ionization source. The mass spectrometer was operated in the positive-ion mode of selected reaction monitoring. The chromatographic run-time for one injection was less than 6 min. The intra- and inter-assay coefficients of variation for the lowest concentration examined (30 pg ml[-1]) were 9.83 and 10.67, respectively. And the analytical recovery of OCT added to serum was quantitative. Assay linearity was obtained in the range of 20-640 pg ml(-1).
已开发出一种灵敏且特异的液相色谱 - 质谱分析法，用于测定22 - 氧杂骨化三醇（OCT），它是1α,25 - 二羟基维生素D3的一种新类似物。通过在C18柱和NH2柱上进行两步固相萃取从血清中分离出分析物。两步萃取过程中OCT的回收率超过90%。一种相关物质（ED - 94），即侧链缩短一个碳原子的OCT，用作内标。提取物在与电喷雾电离源相连的C18反相柱上进行色谱分析。质谱仪在选择反应监测的正离子模式下运行。一次进样的色谱运行时间少于6分钟。所检测的最低浓度（30 pg ml⁻¹）的批内和批间变异系数分别为9.83和10.67。添加到血清中的OCT的分析回收率是定量的。在20 - 640 pg ml⁻¹范围内获得了分析线性。
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