HPLC-ELSD法测定注射用阿奇霉素含量及有关物质

Determination of Azithromycin for Injection and Its Related Substances by HPLC-ELSD

目的:研究分析HPLC-ELSD法测定注射用阿奇霉素含量及有关物质。方法:精密选取适量的阿奇霉素对照品,将样品分为4份。将它制作成酸降解产物、碱降解产物、氧化降解产物以及高温破坏降解产物。精密根据:“1.3.1”的对照品储存液中的0.5ml、1.0ml、1.5ml、2.5ml以及5.0ml的溶液分别放于10ml的容量瓶内,加入稀释液进行摇匀制作成对照品溶液。精密量取进行相关物质测试的供试品溶液中的0.5ml、1.0ml、1.5ml、2.5ml以及5.0ml的溶液分别放于100ml的容量瓶内,使用稀释液进行稀释并摇晃均匀得到供试品的0.5%、1.0%、1.5%、2.5%以及4.0%的对照品溶液。精密选择6份相同编号的样品,根据以上的实验方式制作成供试品溶液。结果:阿奇霉素和酸降解产物、碱降解产物、氧化降解产物以及高温破坏降解产物所出现的降解产物可以很好的进行分离、分解,降解产物以及主成分自身的鉴定不出现混淆,扰乱等情况。阿奇霉素在0.51124-5.10229ug的范围内表示其线性的关系优好。相关物质在进行检测时在0.7509-6.5989ug的范围内表示峰面积的对数与样品原本的浓度相比,质量对数显示有良好的线性关系。阿奇霉素的平均含量在标示量的99.4%左右。结论:本实验方法简单方便、操作手续轻松并且准确可靠,运用其测定注射用阿奇霉素含量及有关物质以及质量控制,具有较高的应用价值,值得推广。

Objective:To study and analyze the determination of azithromycin for injection and its related substances by HPLC-ELSD.Methods:Accurately select appropriate azithromycin reference substance,and divide the sample into 4 parts,then make them into acid degradation products,alkali degradation products,oxidation degradation products and high temperature destruction degradation products.Precision basis:0.5 ml,1.0 ml,1.5 ml,2.5 ml and 5.0 ml of the reference substance storage solution in"1.3.1"are respectively put into a 10ml volumetric flask,and diluted solution is added and shaken evenly to prepare the reference substance solution.Accurately measure 0.5 ml,1.0 ml,1.5 ml,2.5 ml and 5.0 ml of the test solution for testing related substances,put them in a 100ml volumetric flask,dilute them with diluent and shake them evenly to obtain 0.5%,1.0%,1.5%,2.5%and 4.0%reference solutions of the test solution.Accurately select 6 samples with the same number,and prepare the test solution according to the above experimental method.Results:the degradation products in azithromycin,acid degradation products,alkali degradation products,oxidative degradation products and high-temperature destruction of degradation products can be well separated and decomposed,and the identification of degradation products and principal components themselves is not confused or disturbed.Azithromycin has a good linear relationship in the range of 0.51124-5.10229ug.The logarithm of peak area in the range of 0.7509-6.5989ug when detecting related substances shows a good linear relationship with the original concentration of the sample.The average content of azithromycin is about 99.4%of the labeled amount.Conclusion:The experimental method is simple,convenient,easy to operate,accurate and reliable.The method for determination of azithromycin for injection and its related substances and quality control has high application value and is worth popularizing.