两种用于合成前列腺素卡前列素的高效液相色谱分析方法的比较。

Comparison of two high-pressure liquid chromatographic assays for carboprost, a synthetic prostaglandin.

作者信息

Brown L W, Carpenter B E

出版信息

J Pharm Sci. 1980 Dec;69(12):1396-9. doi: 10.1002/jps.2600691211.

Abstract

A high-pressure liquid chromatographic assay for carboprost tromethamine as the bulk drug and in a sterile solution formulation is described. The procedure involves derivatization of the prostaglandin to form the UV-absorbing naphthacyl ester, which then is chromatographed on a silica gel column using methylene chloride-1,3-butanediol-water (496:4:0.25) as the mobile phase. This procedure is compared with a nonderivatization procedure with refractive index detection. Both procedures separate the 15R-epimer of carboprost from carboprost, but only the derivatization procedure separates the 5-trans-isomer of carboprost. Possible reasons for the better separation using the derivatization procedure are discussed. Both procedures gave a coefficient of variation of approximately 1% for carboprost. The derivatization procedure gave a coefficient of variation of approximately 7% for the 15R-epimer and 5-trans-isomer when present at 2% of the carboprost level.

摘要

描述了一种用于测定原料药卡前列甲酯以及无菌溶液制剂中卡前列甲酯的高压液相色谱法。该方法包括将前列腺素衍生化以形成具有紫外吸收的萘甲酰酯，然后以二氯甲烷 - 1,3 - 丁二醇 - 水（496:4:0.25）作为流动相在硅胶柱上进行色谱分离。该方法与采用折光率检测的非衍生化方法进行了比较。两种方法都能将卡前列素的15R - 差向异构体与卡前列素分离，但只有衍生化方法能分离卡前列素的5 - 反式异构体。讨论了使用衍生化方法获得更好分离效果的可能原因。两种方法对卡前列素的变异系数约为1%。当15R - 差向异构体和5 - 反式异构体含量为卡前列素水平的2%时，衍生化方法对它们的变异系数约为7%。