Quantitative determination of tautomeric FK506 by reversed-phase liquid chromatography
Quantitative determination of tautomeric FK506 by reversed-phase liquid chromatography
复制标题
DOI：
10.1016/0731-7085(95)01605-8
复制
发表时间：
1996-01-01
影响因子：
3.4
通讯作者：
Hosoda, J
中科院分区：
文献类型：
--
作者：
Akashi, T;Nefuji, T;Hosoda, J
采用反相高效液相色谱法对器官移植免疫抑制剂FK 506的含量测定进行了研究。在水溶液色谱图上有三个峰对应于FK 506及其互变异构体化合物。由于差向异构化，这些化合物之间发生相互转化，然后在水溶液中达到平衡。水-溶剂溶液中的含水量增加，原因是FK 506和互变异构体I的峰面积减少，互变异构体II的峰面积增加。对于水溶液的定量分析，这产生了一个问题，因为平衡时混合物的组成随水含量而变化。一个简单的方法，使用聚氧乙烯月桂醇醚（Brij-35）的溶液作为稀释剂，已被开发，以提供一个恒定的平衡。通过用Brij-35稀释剂稀释样品，可以定量水溶液中的FK 506。从发酵液中提取的样品证实了所提出的方法的可靠性。
The quantitative determination of FK506, an immunosuppresant for organ transplants, was studied by using reversed-phase high performance liquid chromatography. There were three peaks corresponding to FK506 and its tautomeric compounds on the chromatogram obtained from aqueous solution. Interconversion among these compounds due to epimerization occurs and then reaches an equilibrium in aqueous solution. An increase in the water content in water-solvent solutions caused by the peak areas of FK506 and Tautomer I to decrease and that of Tautomer II to increase. For quantitative analyses of aqueous solutions this creates a problem because the composition of the mixture at equilibrium varies with the water content. A simple method, using a solution of polyoxyethylene lauryl alcohol ether (Brij-35) as a diluent, has been developed to provide a constant equilibrium. By diluting the sample with the Brij-35 diluent, it is possible to quantify FK506 in aqueous solutions. The reliability of the proposed method was confirmed with samples extracted from fermentation broth.