HPLC-ELSD法测定注射用盐酸大观霉素的含量及有关物质  

Content determination of spectinomycin hydrochloride for injection by HPLC-ELSD

作　　者：巩丽萍[1] 杨娜[1] 刘琦[1] 谢元超[1] 

机构地区：[1]山东省食品药品检验所,济南250101

出　　处：《中国抗生素杂志》2013年第9期679-683,共5页Chinese Journal of Antibiotics

基　　金：国家药典委员会国家药品标准提高研究项目;项目编号:1015[国药综发(2010)35号文]

摘　　要：目的建立测定注射用盐酸大观霉素的含量及有关物质的方法。方法色谱柱：AgilentSBC18（250mm×4．6mm，5μm）；流动相：O．07mol／L七氟丁酸溶液-乙腈（83：17）；漂移管温度：105℃，载气流速为1．5L／min。结果大观霉素在0．0175～0．210mg／mL/mm内，进样量的对数值与峰面积对数值线性关系良好，r=0．9998，最低检测限5.3ng，供试品在溶液中稳定性差。平均加样回收率为分别为100．4％（n=9），RSD为1．6％。结论本方法准确、简便，重现性好，可用于注射用盐酸大观霉素的质量控制。Objective To establish an HPLC-ELSD method for the content analysis of spectinomycin hydrochloride for injection and its related substances. Methods The separation was performed on an Agilent C18 column AgilentSBC18（250mm×4.6mm,5μm）. The mobile phase consists of 0.07 mol/L hyptafluorobutyric-acetonitrile （83 ： 17）. The temperature of the drift tube was set at 105~C, and the gas flow is 1.5L/min. Results In the range of 0.0175-0.210 mg/mL, there was a good linear relationship between the log value of the inject quantities and the log value of the peak areas. The limit of detection is 53ng. Spectinomycin hydrochloride was instable in solution. The average recovery is 100.4%, with RSD 1.6 % （n=9）. Conclusion The method is simple, accurate and highly reproducible. This method is suitable for quality control of spectinomycin hydrochloride for injection.

关 键 词：大观霉素 高效液相色谱法 蒸发光散射检测 含量测定 有关物质 

分 类 号：R917[医药卫生—药物分析学]