Simultaneous analysis of dextran-methylprednisolone succinate, methylprednisolone succinate, and methylprednisolone by size-exclusion chromatography.
Simultaneous analysis of dextran-methylprednisolone succinate, methylprednisolone succinate, and methylprednisolone by size-exclusion chromatography.
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DOI：
10.1016/s0731-7085(98)00308-2
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发表时间：
1999-04
影响因子：
3.4
通讯作者：
R. Mehvar
中科院分区：
文献类型：
--
作者：
R. Mehvar
本文报道了同时测定低浓度（1.0 ~ 100 μg ml−1）葡聚糖-琥珀酸甲基强的松龙（DEX-MPS）及其降解产物半琥珀酸甲基强的松龙（MPS）和甲基强的松龙（MP）的高效液相色谱分析方法。分离后，采用粒径隔离柱，流动相为KH2PO4(10 mM)：乙腈（3:1），流速为1 ml min - 1，在250 nm处进行检测。流动相的pH值对MPS和MPS峰的分辨率有较大影响；MP和MPS在pH 3.4时共洗脱，在pH≥5时基线溶解。检测器响应与分析物浓度（MP和MPS为1.0 ~ 100 μg ml - 1， DEX-MPS为2.5 ~ 100 μg ml - 1）呈线性关系（r≥0.997）。运行内和运行间误差（<13%）和精密度（CV≤6%）数据表明，该方法可以准确和精确地定量检测浓度范围内的所有三种成分。应用该方法测定了DEX-MPS的取代度、纯度和稳定性。
An analytical HPLC method is reported for simultaneous measurement of low (1.0–100 μg 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≥5. Linear relationships (r≥0.997) were found between the detector response and the concentrations of the analytes (1.0–100 μg ml−1for MP and MPS and 2.5–100 μg ml−1for DEX-MPS). Intra- and inter-run error (<13%) and precision (CV of ≤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.