Kissinger L D, Robins R H
J Chromatogr. 1985 Mar 15;321(2):353-62. doi: 10.1016/s0021-9673(01)90453-4.
A silver-modified, normal-phase, high-performance liquid chromatographic system has been developed for prostaglanding bulk drugs and triacetin solutions. Silver nitrate present in the mobile phase results in high selectivity for cis/trans isomers with conventional silica columns. Prostaglandins were esterified with alpha-bromo-2'-acetonaphthone prior to chromatography to provide high detectability at 254 nm. For dilute triacetin solutions, a sample preparation scheme based on gravity-flow chromatography with silica columns was developed to isolate the prostaglandin from triacetin prior to derivatization. The analytical technique was applied to triacetin solutions containing as little as 10 micrograms/ml arbaprostil [15-(R)-methyl-PGE2].
已开发出一种银改性的正相高效液相色谱系统,用于前列腺素原料药和三醋精溶液的分析。流动相中存在的硝酸银可使常规硅胶柱对顺式/反式异构体具有高选择性。前列腺素在色谱分析前用α-溴-2'-乙酰萘进行酯化,以在254nm处提供高检测灵敏度。对于稀三醋精溶液,开发了一种基于硅胶柱重力流色谱的样品制备方案,以便在衍生化前从三醋精中分离出前列腺素。该分析技术应用于含有低至10微克/毫升阿巴前列素[15-(R)-甲基-PGE2]的三醋精溶液。