萃取-薄层色谱法检测克拉霉素注射液中的有关物质

Detection of the related substances in clarithromycin injection by extraction-TLC method

目的建立萃取-薄层色谱法(TLC)检查克拉霉素注射液中的有关物质及分解产物。方法用乙酸乙酯萃取,萃取液浓缩至干,氯仿定容,TLC法检查。TLC条件为氯仿—甲醇—氨溶液(120∶20∶0.2)作展开剂;硫酸铈2.0g与钼酸钠2.5g,加入10%硫酸溶液使成100ml为显色剂。结果对杂质的最小萃取量2.5μg,萃取率大于96%;所选展开剂对有关物质及分解产物均可实现清晰分离,显色剂的最低检出限2μg;平行萃取、检查三次的结果相同。结论本法对杂质萃取、分离、检出的效果良好,具有重复性,可有效地用于存在辅料干扰的克拉霉素注射液中的有关物质检查。

Objective The extraction- TLC method for the detection of the related substances in clarithromycin injection was established.Methods The samples were extracted by ethyl acetate and concentrated to dryness,and dissolved in chloroform,then subjected to TLC plate.The TLC conditions were as follows:The developing solvent was chloroform- methanol- ammonia solution(120∶ 20∶ 0.2); the chromogenic agent was a mixture containing 2.0g of cerium(IV) sulfate tetrahydrate and 2.5g of sodium molybdate in 100ml of 10% sulfuric acid.Results The limit of extraction was 2.5μ g;extraction rate was more than 96% ;the related substances were isolated,the detection limit was 2μ g.In the triplicate examination,results were consistent. Conclusion In this method, the results of extraction,isolation and detection were satisfied and reproducible.It could be used successfully to detect the related substances in clarithromycin injection.