Inhibition of the succinic dehydrogenase of tetrahymena geleii S by a phosphono-substituted succinate analog.
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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.
In the title compound, C(6)H(18)N(2)(2+).C(4)H(4)O(4)(2-).C(4)H(6)O(4), the components lie on centres of symmetry in space group P-1, such that the asymmetric unit contains three half-molecules. Despite the different mode (with respect to other dicarboxylic acids) adopted by the intermolecular self-interaction of succinic acid derivatives, the overall structure of the title compound consists of anionic layers that are typical of the packing structures exhibited by other dicarboxylic acid analogues.
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