摘要
目的:建立液相色谱(脉冲安培检测器)测定硫酸小诺霉素氯化钠注射液中小诺霉素组分含量的方法,为制定该类药的质量控制标准提供参考。方法:用十八烷基硅烷键合硅胶为填充剂(4.0 mm×150 mm,3μm),以1.25%(v/v)三氟乙酸溶液[含0.025%五氟丙酸,0.85%(v/v)的50%氢氧化钠溶液,用0.5 mol·L^(-1)的氢氧化钠溶液调节pH至2.6]-乙腈(97.5∶2.5)为流动相,柱温为30℃,流速为0.7 mL·min^(-1);柱后衍生氢氧化钠溶液浓度为0.5 mol·L^(-1)(含0.005 mol·L^(-1)乙二胺四乙酸溶液),以流速0.3 mL·min^(-1)等度淋洗。结果:小诺霉素在19.93～59.80μg·mL^(-1)浓度范围内线性关系良好(r=0.999 6),小诺霉素精密度(RSD)为0.55%,检测下限为23.9 ng,平均回收率为99.1%。6批样品测定结果分别为90.7%、91.1%、90.6%、91.2%、90.7%、88.6%,与2015年版《中华人民共和国药典》方法结果无明显差异。结论:经方法学验证,本法适用于硫酸小诺霉素氯化钠注射液中小诺霉素组分含量的控制。
Objective:To establish a new method to analyze micronomicin content in micronomicin sulfate and sodium chloride injection using a liquid chromatographic method with pulsed electrochemical detection(LC-PED), to evaluate the quality of the drug. Methods:The seperation was performed on a C18 column(4. 0 mm×150 mm, 3 μm). The mobile phase was 1.25%(v/v)trifluoroacetic acid[containing 0.025% pentafluoropropionic acid and 0.85%(v/v)of 50% sodium hydroxide,adjusting the pH to 2.6 with 0.5 mol·L^-1 NaOH]-acetonitrile(97.5∶2.5) at a flow rate of 0.7 mL·min^-1. The temperature of the column was set at 30 ℃. 0.5 mol·L^-1 NaOH(containing 0.5 mol·L^-1 EDTA)was added post column at a flow rate of 0.3 mL·min^-1 to raise the pH of detection to at least 12. Results:The linearity of micronomicin ranges from 19.93 to 59.80 μg·mL^-1 with a correlation coefficient of 0.999 6. The precision(RSD)of micronomicin was 0.55%. The LOD of micronomicin was 5.98 μg·mL^-1(23.9 ng injected). The average recovery rate was 99.1%. The results of six samples were 90.7%,91.1%,90.6%, 91.2%,90.7%,88.6%,respectivey. Conclusion:The method is proved to be applicable to the control of the content of micronomicin component in micronomicin sulfate and sodium chloride injection.
作者
易巧
刘绪平
韩春霞
熊骏
YI Qiao;LIU Xu-ping;HAN Chun-xia;XIONG Jun(Jiangxi Institute for Drug Control,Jiangxi Provincial Engineering Research Center for Drug and Medical Device Quality, Nanchang 330029,China;Thermo Fisher Scientific(China)Co., Ltd.,Shanghai 201206,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第12期2200-2203,共4页
Chinese Journal of Pharmaceutical Analysis
关键词
液相色谱-脉冲安培检测器
硫酸小诺霉素氯化钠注射液
小诺霉素组分
liquid chromatography-pulsed electrochemical detection
micronomicin sulfate and sodium chlorideinjection
micronomicin component
