HPLC-ELSD法在硫酸庆大霉素及其制剂质量控制中的影响因素考察  

The influencing factors of quality analysis of gentamycin sulfate and its preparations by HPLC-ELSD

作　　者：王立萍[1] 姚永青[1] 刘英[1] Wang Li-ping;Yao Yong-qing;Liu Ying(Henan Provincial Institute of Food and Drug Control,Zhengzhou 450018)

机构地区：[1]河南省食品药品检验所,郑州450018

出　　处：《中国抗生素杂志》2020年第5期448-454,共7页Chinese Journal of Antibiotics

摘　　要：目的以硫酸庆大霉素片为研究对象,分析HPLC-ELSD法在质量控制中的影响因素,探讨氨基糖苷类抗生素质量控制方法的发展趋势。方法采用Apollo C18色谱柱(250mm×4.6mm,5μm),流动相为0.2mol/L三氟乙酸溶液:甲醇(96:4,V/V),柱温35℃。ELSD检测:漂移管温度110℃,载气流速2.5L/min,增益1。结果方法存在溶剂效应,应优先选择流动相做溶剂;溶液浓度超载从而使色谱峰平顶,对组分测定结果有影响;采用西索米星对照品外标法测定有关物质,对照品溶液浓度的高低对测定结果无影响;采用随行标准曲线,色谱峰保留时间的改变对组分和有关物质测定无影响。结论HPLC-ELSD法虽然影响因素较多,但是实验过程注意这些影响因素,HPLC-ELSD法仍为一种简单、通用、价廉的控制硫酸庆大霉素等氨基糖苷类抗生素质量的方法。Objective Taking gentamicin sulfate tablets as the research object,the influencing factors of quality control by HPLC-ELSD were analyzed,and the development trend of quality control methods for aminoglycoside antibiotics was discussed.Methods Apollo C18 column(250 mm×4.6 mm,5μm)was used.The mobile phase was 0.2 mol/L trifluoroacetic acid solution:methanol(96:4,V/V),and the column temperature was 35℃.The ELSD detection conditions were:Drift tube temperature of 110℃,carrier gas velocity of 2.5 L/min,and gain of 1.Results The solvent should be chosen as the mobile phase in the presence of solvent effect;the concentration overload of solution made the chromatographic peak flat and had an effect on the determination results of components;in the the determination of related substances by the external standard method of sisomicin reference,the substance concentration had no effects on the determination results;the change of retention time of chromatographic peak had no effects on the determination of components and related substances by the follow-up standard curve.Conclusion Although there are many factors affecting the detection of aminoglycoside antibiotics,attention should be paid to these factors in the experimental process.The method of HPLC-ELSD is still a simple,universal and inexpensive method to control the quality of aminoglycoside antibiotics such as gentamicin sulfate.

关 键 词：氨基糖苷类 HPLC-ELSD 影响因素 硫酸庆大霉素片 

分 类 号：R917[医药卫生—药物分析学]