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用于正相液相色谱法测定前列腺素原料药和三醋精溶液中前列腺素及其5,6-反式异构体的银改性流动相。

Silver-modified mobile phase for normal-phase liquid chromatographic determination of prostaglandins and their 5,6-trans isomers in prostaglandin bulk drugs and triacetin solutions.

作者信息

Kissinger L D, Robins R H

出版信息

J Chromatogr. 1985 Mar 15;321(2):353-62. doi: 10.1016/s0021-9673(01)90453-4.

DOI:10.1016/s0021-9673(01)90453-4
PMID:3988843
Abstract

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].

摘要

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。

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