Mehvar R
College of Pharmacy and Health Sciences, Drake University, Des Moines, IA 50311, USA.
J Pharm Biomed Anal. 1999 Apr;19(5):785-92. doi: 10.1016/s0731-7085(98)00308-2.
An analytical HPLC method is reported for simultaneous measurement of low (1.0-100 microg ml(-1)) concentrations of dextran-methylprednisolone succinate (DEX-MPS) and its degradation products methylprednisolone hemisuccinate (MPS) and methylprednisolone (MP). The analytes were detected at 250 nm after resolution using a size exclusion column with a mobile phase of KH2PO4 (10 mM): acetonitrile (3:1) and a flow rate of 1 ml min(-1). The resolution of MP and MPS peaks was substantially affected by the pH of the mobile phase; while MP and MPS co-eluted at pH 3.4, they were baseline-resolved at pH > or = 5. Linear relationships (r > or = 0.997) were found between the detector response and the concentrations of the analytes (1.0-100 microg ml(-1) for MP and MPS and 2.5-100 microg ml(-1) for DEX-MPS). Intra- and inter-run error (< 13%) and precision (CV of < or = 6%) data indicated that the assay could accurately and precisely quantitate all three components in the examined concentration range. The application of the assay to determination of degree of substitution, purity, and stability of DEX-MPS was also demonstrated.
报道了一种反相高效液相色谱法，用于同时测定低浓度（1.0 - 100 μg ml⁻¹）的右旋糖酐 - 甲泼尼龙琥珀酸酯（DEX - MPS）及其降解产物半琥珀酸甲泼尼龙（MPS）和甲泼尼龙（MP）。使用尺寸排阻柱，以KH₂PO₄（10 mM）：乙腈（3:1）为流动相，流速为1 ml min⁻¹，在250 nm处检测分析物。MP和MPS峰的分离度受流动相pH值的显著影响；在pH 3.4时MP和MPS共洗脱，而在pH≥5时基线分离。在分析物浓度（MP和MPS为1.0 - 100 μg ml⁻¹，DEX - MPS为2.5 - 100 μg ml⁻¹）与检测器响应之间发现了线性关系（r≥0.997）。批内和批间误差（<13%）以及精密度（CV≤6%）数据表明，该测定法能够在检测浓度范围内准确、精确地定量所有三种成分。还证明了该测定法在测定DEX - MPS的取代度、纯度和稳定性方面的应用。
