硫酸卡那霉素注射液杂质谱的HPLC-ELSD分析方法的评价与应用  

Evaluation and application of HPLC-ELSD in impurity profile detection of kanamycin sulfate injection

作　　者：赵敬丹[1] 刘浩[1] ZHAO Jing-dan;LIU Hao(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《药物分析杂志》2021年第1期117-123,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：2019年国家药品标准提高项目(No.2019H02)。

摘　　要：目的:优化并建立硫酸卡那霉素注射液杂质谱分析的高效液相色谱-蒸发光散射检测法(HPLCELSD法),同时将该方法应用于不同来源样品的分析,评价该方法对于氨基糖苷类抗生素质量分析的适用性。方法:采用Welch LP-C_(18)(4.6 mm×250 mm,5μm)色谱柱,以0.2 mol·L^(-1)三氟乙酸溶液-甲醇(98∶2)为流动相,柱温为30℃,流速0.3 mL·min^(-1),不分流型蒸发光散射检测器检测。结果:硫酸卡那霉素注射液的各工艺杂质之间、降解杂质之间、各杂质与卡那霉素及辅料之间均分离良好,专属性试验显示该方法可用于杂质谱的全面分析。结论:优化后的HPLC-ELSD法可用于卡那霉素原料及其注射液的快速质量评价;该方法的专属性良好,相对于其他方法具有分析速度快,成本低,易于推广等优势。Objective:To optimize and establish an HPLC-ELSD method,and determine the related substances in kanamycin sulfate injection from different sources in order to evaluate its suitability in the analysis of aminoglycoside antibiotics by a series of methodological studies,especially the specificity.Methods:A Welch LP-C18 column(4.6 mm×250 mm,5μm)was used,and the mobile phase was 0.2 mol·L^(-1) trifluoroacetic acid solution-methanol(98∶2)at a flow rate of 0.3 mL·min^(-1).ELSD detector was used on splitless mode.Results:Satisfied resolutions were obtained among different related process impurities,different degraded impurities,as well as kanamycin and different excipients.And mass balance was proved through the specificity tests.The method could be used for comprehensive analysis of the impurity profile of kanamycin sulfate injection.Conclusion:The optimized method will play an important role in fast quality evaluation of kanamycin and its injection.The ELSD method is proved with better specificity,more efficiency,lower costs and easier to be popularized than other methods.

关 键 词：硫酸卡那霉素注射液 杂质谱 2-脱氧链霉胺衍生物 氨基糖苷类抗生素 高效液相色谱-蒸发光散射检测 

分 类 号：R917[医药卫生—药物分析学]