Matin S B, Amos B
J Pharm Sci. 1978 Jul;67(7):923-6. doi: 10.1002/jps.2600670713.
A method for the quantitative determination of prednisolone and prednisone in human plasma utilizing GLC and chemical-ionization mass spectrometry is described. Corticosteroids are extracted from plasma into ether, and the extract is purified either by passing through a magnesium silicate column or by solvent partitioning. Interference from endogenous hydrocortisone is removed by selective derivatization with Girard Reagent T. Following derivatization, prednisolone can be quantitatively separated from the water-soluble hydrocortisone derivative by simple solvent partitioning. The extracted prednisone and prednisolone are converted to their corresponding methoxyimino trimethylsilyl derivatives, and subjected to GLC-mass spectrometry. Prednisone and prednisolone plasma profiles following a 15-mg oral dose of prednisone in a human volunteer are presented. The method can measure prednisone and prednisolone in plasma at the nanogram per milliliter level.
本文描述了一种利用气相色谱法（GLC）和化学电离质谱法对人血浆中泼尼松龙和泼尼松进行定量测定的方法。皮质类固醇从血浆中萃取到乙醚中，提取物通过硅酸镁柱或溶剂分配进行纯化。通过用吉拉德试剂T进行选择性衍生化来消除内源性氢化可的松的干扰。衍生化后，泼尼松龙可通过简单的溶剂分配从水溶性氢化可的松衍生物中定量分离出来。萃取的泼尼松和泼尼松龙转化为相应的甲氧基亚氨基三甲基硅烷基衍生物，然后进行气相色谱 - 质谱分析。给出了一名人类志愿者口服15毫克泼尼松后的泼尼松和泼尼松龙血浆浓度曲线。该方法可测量血浆中纳克/毫升水平的泼尼松和泼尼松龙。
