HPLC法测定盐酸莫西沙星的有关物质  

Related substances analysis for moxifloxacin hydrochloride by HPLC

作　　者：王夕静 常春[1] 温秀红 傅强[1] WANG Xi-jing;CHANG Chun;WEN Xiu-hong;FU Qiang(School of Pharmacy,Xi′an Jiaotong University,Xi’an 710061,China;Xi′an Xintong Pharmaceutical Research Co.,Ltd.,Xi’an 710077,China)

机构地区：[1]西安交通大学药学院,西安710061 [2]西安新通药物研究有限公司,西安710077

出　　处：《药物分析杂志》2020年第11期2048-2055,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立高效液相色谱法测定盐酸莫西沙星原料药的有关物质。方法:采用Boston苯基键合硅胶(4.6 mm×250 mm,5μm)色谱柱,以四丁基硫酸氢铵缓冲溶液-甲醇为流动相,梯度洗脱,流速1.3mL·min-1,柱温45℃,检测波长293 nm。结果:盐酸莫西沙星与8个已知杂质A^L色谱峰均能良好分离,并分别在0.483~1.932μg·mL^-1(r=0.9994)、0.521~2.084μg·mL^-1(r=0.9992)、0.496~1.985μg·mL^-1(r=0.9986)、0.463~1.850μg·mL^-1(r=0.9994)、0.403~1.614μg·mL^-1(r=0.9991)、0.414~1.656μg·mL^-1(r=0.9978)、0.451~1.805μg·mL^-1(r=0.9988)、0.534~2.137μg·mL^-1(r=0.9998)、0.471~1.882μg·mL^-1(r=0.9994)范围内线性关系良好(n=6)。盐酸莫西沙星、杂质A、B、C、D、E、F、I、L的定量下限分别为0.18、0.31、0.42、0.40、0.38、2.0、0.3、1.0、2.8 ng;各杂质平均回收率(n=9)分别为92.8%、94.8%、103.6%、97.5%、101.0%、94.9%、96.6%、104.0%。6批盐酸莫西沙星样品测定结果显示,已知杂质及其他最大单个杂质含量均小于0.10%,杂质总含量小于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,可用于盐酸莫西沙星原料药有关物质的测定。Objective:To establish an HPLC method for the determination of the related substances in moxifloxacin hydrochloride.Methods:The determination was performed on a phenysilyl column(4.6 mm×250 mm,5μm).The mobile phase consisted of tetrabutyl ammonium bisulfate buffer solutition and methanol with gradient elution.The flow rate was 1.3 mL·min-1,and the column temperature was maintained at 45℃,the detection wavelength was set at 293 nm.Results:The resolutions between the peaks of moxifloxacin hydrochloride and eight known impurities(including impurities A-L)were good.The calibration curves of moxifloxacin hydrochloride and the known impurities were linear in their respective weight ranges of 0.483-1.932μg·mL^-1(r=0.9994)、0.521-2.084μg·mL^-1(r=0.9992)、0.496-1.985μg·mL^-1(r=0.9986)、0.463-1.850μg·mL^-1(r=0.9994)、0.403-1.614μg·mL^-1(r=0.9991)、0.414-1.656μg·mL^-1(r=0.9978)、0.451-1.805μg·mL^-1(r=0.9988)、0.534-2.137μg·mL^-1(r=0.9998)、0.471-1.882μg·mL^-1(r=0.9994).The limits of quantitation were 0.18,0.31,0.42,0.40,0.38,2.0,0.3,1.0,2.8 ng,and the recoveries(n=9)were 92.8%,94.8%,103.6%,97.5%,101.0%,94.9%,96.6%,104.0%for the above impurities,respectively.The determination results of the six batches of moxifloxacin hydrochloride samples showed that the known impurities were less than 0.10%,the maximum single unknown impurity was less than 0.10%,and the total impurity was less than 0.15%.Conclusion:The method is proved to be simple,rapid and accurate,and could be used for the determination of related substances in moxifloxacin hydrochloride.

关 键 词：盐酸莫西沙星 有关物质 相对响应因子 质量控制 高效液相色谱法 梯度洗脱 

分 类 号：R917[医药卫生—药物分析学]