土霉素和强力霉素的薄层色谱分析及纯度控制——与液相色谱法的比较

Assay and purity control of oxytetracycline and doxycycline by thin-layer chromatography--a comparison with liquid chromatography.

作者信息

Geelen S, Roets E, Hoogmartens J

机构信息

Katholieke Universiteit Leuven, Instituut voor Farmaceutische Wetenschappen, Belgium.

出版信息

J Pharm Biomed Anal. 1990;8(8-12):891-8. doi: 10.1016/0731-7085(90)80138-f.

DOI:10.1016/0731-7085(90)80138-f

PMID:2100638

Abstract

A thin-layer chromatographic (TLC) method using densitometry is described for the assay and purity control of oxytetracycline and doxycycline. With a mobile phase of dichloromethane-methanol-water (59:35:6, v/v/v) and a silica gel thin-layer, previously sprayed with 10% sodium edetate solution adjusted to pH 9.0, all the potential impurities of oxytetracycline or doxycycline are well separated from the main components and from each other. Results obtained with TLC are compared with those obtained by previously established liquid chromatography (LC) methods using poly(styrene-divinylbenzene) stationary phases. A good correlation was obtained (r greater than 0.9999). For TLC the relative standard deviation (RSD) for the assay of the main component was less than 2%, for LC the RSD was less than 1%.

摘要

本文描述了一种采用密度测定法的薄层色谱（TLC）方法，用于土霉素和强力霉素的含量测定及纯度控制。以二氯甲烷 - 甲醇 - 水（59:35:6，v/v/v）为流动相，硅胶薄层预先喷有pH值调至9.0的10%依地酸钠溶液，土霉素或强力霉素的所有潜在杂质与主要成分以及彼此之间均能良好分离。将TLC得到的结果与先前建立的使用聚（苯乙烯 - 二乙烯基苯）固定相的液相色谱（LC）方法得到的结果进行比较。获得了良好的相关性（r大于0.9999）。对于TLC，主要成分含量测定的相对标准偏差（RSD）小于2%，对于LC，RSD小于1%。