高效液相色谱法测定盐酸替马沙星中的微量杂质

Determination of minor impurities in temafloxacin hydrochloride by high-performance liquid chromatography.

作者信息

Elrod L, Linton C L, Shelat B P, Wong C F

机构信息

PPD Analytical Research Department, Abbott Laboratories, North Chicago, IL 60064.

出版信息

J Chromatogr. 1990 Oct 19;519(1):125-36. doi: 10.1016/0021-9673(90)85141-h.

DOI:10.1016/0021-9673(90)85141-h

PMID:2077043

Abstract

Minor impurities in the antibacterial agent temafloxacin hydrochloride were determined using high-performance liquid chromatography. Manufacturing impurities and degradation products were separated using a reversed-phase system with gradient elution. Detector response was linear for the individual impurities to approximately 50 micrograms/ml which represents 2.5% of the drug concentration. The procedure provides quantitation of impurities to approximately the 0.05% level with precision (relative standard deviations) of 4.7% to 29% in typical bulk drug lots. A variety of reversed-phase columns were evaluated for the assay method with optimum resolution achieved using a 5-microns Nucleosil C18 packing.

摘要

采用高效液相色谱法测定了盐酸替马沙星抗菌剂中的微量杂质。使用具有梯度洗脱的反相系统分离生产过程中产生的杂质和降解产物。各杂质的检测器响应在约50微克/毫升范围内呈线性，这相当于药物浓度的2.5%。该方法可对杂质进行定量，在典型的原料药批次中，定量下限约为0.05%，精密度（相对标准偏差）为4.7%至29%。对多种反相柱进行了该测定方法的评估，使用5微米的Nucleosil C18填料可实现最佳分离度。