HPLC法测定甲磺酸左氧氟沙星氯化钠注射液中有关物质  

HPLC determination of related substances in levofloxacin mesylate sodium chloride injection

作　　者：刘杨 傅蓉 易大为 张亚杰 LIU Yang;FU Rong;YI Dawei;ZHANG Yajie(Liaoning Inspection,Examination and Certification Center,Liaoning Institute for Drug Control,Shengyang 110036,China)

机构地区：[1]辽宁省检验检测认证中心,辽宁省药品检验检测院,沈阳110036

出　　处：《中国药品标准》2023年第6期636-642,共7页Drug Standards of China

摘　　要：目的:建立高效液相色谱法测定甲磺酸左氧氟沙星氯化钠注射液中有关物质。方法:采用十八烷基硅烷键合硅胶(4.6 mm×250 mm,5μm)色谱柱,以醋酸铵高氯酸钠溶液-乙腈为流动相,梯度洗脱,流速1.0 mL·min^(-1),柱温40℃,检测波长为294 nm和238 nm。结果:在该色谱条件下,左氧氟沙星与各杂质均能有效分离,左氧氟沙星、杂质A的定量限分别为0.120 0μg·mL^(-1)、0.371 2μg·mL^(-1),左氧氟沙星和杂质A分别在0.600 1~4.801μg·mL^(-1)和0.742 5~5.940μg·mL^(-1)范围内与其峰面积呈良好线性关系(r=1.000),左氧氟沙星、杂质A回收率(n=9)分别在97.86%~101.22%和99.65%~101.82%之间,重复性、精密度、稳定性等均符合规定。5批甲磺酸左氧氟沙星氯化钠注射液样品测定结果显示,杂质A均未检出,其他最大杂质含量在0.02%~0.08%,杂质总量在0.02%~0.15%。结论:经方法学验证,本方法灵敏、快速、专属性强、准确度高,可用于甲磺酸左氧氟沙星氯化钠注射液有关物质的测定。Objective:An HPLC method for the determination of related substances in levofloxacin mesylate sodium chloride injection was established.Methods:The octadecylsilane bonded silica gel(4.6 mm×250 mm,5μm) column was used with ammonium acetate sodium perchlorate solution acetonitrile as the mobile phase.The flow rate was 1.0 mL·min~(-1),and the column temperature was 40 ℃.The detection wavelengths were 294 nm and 238 nm.Results:Under the chromatographic conditions,levofloxacin and all impurities can be effectively separated.The limits of quantitation of levofloxacin and impurity A were 0.120 0 μg·mL~(-1) and 0.371 2 μg·mL~(-1),respectively.Levofloxacin and impurity A showed a good linear relationship with their peak areas(r=1.000) in the range of 0.600 1-4.801 μg·mL~(-1) and 0.742 5-5.940 μg·mL~(-1),respectively.The recoveries of levofloxacin and impurity A(n=9) were 97.86%-101.22% and 99.65%-101.82%,respectively.The repeatability,precision and stability met the requirements.The results of 5 batches of levofloxacin mesylate sodium chloride injection samples showed that impurity A was not detected,the maximum impurity content of other impurities was 0.02%-0.08%,and the total impurity was 0.02%-0.15%.Conclusion:Through methodological verification,it is confirmed that this method is sensitive,rapid,exclusive and highly accurate,and can be used for the determination of related substances of levofloxacin mesylate sodium chloride injection.

关 键 词：HPLC 甲磺酸左氧氟沙星 有关物质 质量控制 梯度洗脱 

分 类 号：R921.2[医药卫生—药学]