摘要
目的采用高效液相色谱-脉冲安培检测(HPLC-PAD)法测定硫酸庆大霉素氯化钠注射液中的庆大霉素C组分及有关物质。方法采用Dionexics-5000+HPIC电化学检测器系统,AmG-3μm C18色谱柱,流动相为0.1 mol·L^(-1)三氟乙酸溶液-乙腈(98:2),流速1.0 mL·min^(-1),参比电极为Ag/AgCl,工作电极为常规金电极,柱后衍生剂为0.76 mol·L^(-1)氢氧化钠溶液,衍生剂流速0.3 mL·min^(-1),波形图选择Ag/AgCl,柱温35℃。结果庆大霉素C组分及有关物质各杂质均能达到有效分离。庆大霉素C1a、庆大霉素C2、庆大霉素C2a、庆大霉素C1及西索米星的线性范围分别为1.2~96.5、1.3~107.3、0.8~65.4、1.2~101.0、0.6~5.6μg·mL^(-1),r分别为0.9908、0.9927、0.9976、0.9980、0.9975;供试品溶液在室温(25℃)下放置12 h稳定。结论所用方法灵敏、准确、专属性强、重复性好,可用于测定硫酸庆大霉素氯化钠注射液中的庆大霉素C组分及有关物质。
OBJECTIVE To determine related substances and C substance in Gentamycin sulfate sodium chloride injection(GSSCI) by HPLC-PAD.METHODS The chromatographic separation was achieved on a AmG-3 μm C_(18) in a Dionexics-5000+HPIC electrochemical detector system.The mobile phases consisted of 0.1 mol·L^(-1) trifluoroacetic acid solution-acetonitrile( 98:2) with the flow rate of 1.0 mL·min^(-1),and thereference electrode was Ag/AgCl.Working electrode: conventional electrode gold.The post-column derivatization agent was 0.76 mol·L^(-1) sodium hydroxide solution with the flow rate of 0.3 mL·min^(-1).Waveform selection: Ag/AgCl, and the column temperature was 35 ℃.RESULTS Good separation between Gentamicin C component and impurities of related substances could be achieved.Good linear relationship was observed.The linear ranges of gentamicin C1 a,gentamicin C2,gentamicin C2 a,gentamicin C1 and sisomicin were 1.2-96.5 μg·mL^(-1)(r=0.9908),1.3-107.3 μg·mL^(-1)(r=0.9927),0.8-65.4 μg·mL^(-1)(r=0.9976),1.2-101.0 μg·mL^(-1)(r=0.9980) and 0.6-5.6 μg·mL^(-1)(r=0.9975),respectively.Sample solutions were stable at 25 ℃ within 12 hour.CONCLUSION The method is sensitive, accurate, specific and reproducible, which can be served as a reliable analytical method for the determination of related substances and C substance in GSSCI.
作者
熊雯
郑萍
袁宇琳
张静
XIONG Wen;ZHENG Ping;YUAN Yulin;ZHANG Jing(Drug Research Institute of Chengdu,Chengdu,Sichuan,610045 P.R.China)
出处
《华西药学杂志》
CAS
CSCD
2021年第5期558-562,共5页
West China Journal of Pharmaceutical Sciences
基金
符合国际规范的制剂分析与质量控制及标准研究公共服务平台项目(2018ZX09201018-023)。
