Khan N H, Roets E, Hoogmartens J, Vanderhaeghe H
Katholieke Universiteit Leuven, Instituut voor Farmaceutische Wetenschappen, Belgium.
J Chromatogr. 1987 Sep 18;405:229-45. doi: 10.1016/s0021-9673(01)81765-9.
Isocratic high-performance liquid chromatography on PLRP-S 8-microns poly(styrene-divinylbenzene) copolymer allows complete separation of oxytetracycline, 4-epioxytetracycline, tetracycline, anhydrooxytetracycline, alpha- and beta-apooxytetracycline. The mobile phase was tert.-butanol-0.2 M phosphate buffer pH 8.0-0.02 M tetrabutylammonium sulphate pH 8-0.0001 M sodium ethylenediaminetetraacetate pH 8.0-water (5.9:10:5:10:78.1, m/v/v/v/v). With this isocratic method, 2-acetyl-2-decarboxamidooxytetracycline is only partly resolved from oxytetracycline. The separation and the detection limits can be improved by the use of gradient elution. Gradient elution was used for the comparison of official standards and for the analysis of a number of commercial samples, and to monitor the stability of oxytetracycline hydrochloride during storage in the solid state for about 6 years at various temperatures.
在PLRP - S 8微米聚(苯乙烯 - 二乙烯基苯)共聚物上进行等度高效液相色谱法,可实现土霉素、4 - 表氧化土霉素、四环素、脱水土霉素、α - 和β - 去氧土霉素的完全分离。流动相为叔丁醇 - 0.2 M pH 8.0的磷酸盐缓冲液 - 0.02 M pH 8的硫酸四丁铵 - 0.0001 M pH 8.0的乙二胺四乙酸钠 - 水(5.9:10:5:10:78.1,m/v/v/v/v)。采用这种等度方法,2 - 乙酰 - 2 - 脱羧酰胺基土霉素仅部分与土霉素分离。通过使用梯度洗脱可提高分离度和检测限。梯度洗脱用于官方标准品的比较以及多个商业样品的分析,并用于监测盐酸土霉素在不同温度下固态储存约6年期间的稳定性。