摘要
目的:建立注射用头孢米诺钠的有关物质测定方法,并进行验证。方法:色谱条件:选用反相色谱柱;流动相为冰乙酸水溶液(1→100)-甲醇-四氢呋喃(990∶5∶5),流速为1.0 mL/min,柱温为30℃,进样量为10μL,检测波长为254 nm。主峰保留时间约为19.6 min,杂质1~5的保留时间分别约为:4.6、8.8、25.8、12.1、10.2 min。筛选色谱柱并优化稀释剂。验证方法的专属性、准确度、重复性、定量限与检测限、线性及范围,并计算出各有关物质的校正因子。采用该方法检测了2个规格共6批注射用头孢米诺钠。结果:最适合的色谱柱型号:Agilent Zorbax SB-Aq,250 mm×4.6 mm,5μm;稀释剂为水-甲醇-四氢呋喃(990∶5∶5);方法专属性良好,准确度、精密度均满足要求;根据定量限与检测限及线性,确定了主物质及各杂质的浓度范围,进而得出各杂质的校正因子;杂质1~5的校正因子分别为:2.73,0.32,1.05,1.21及1.15;6批供试品的有关物质检测结果均符合质量标准的规定。结论:成功建立了检测注射用头孢米诺钠中的有关物质的HPLC方法,该方法具有良好的专属性、准确度、重复性、线性范围。
Objective:To develop and validate a method for the determination of related substances in Cefminox Sodium for injection.Methods:The reversed-phase column was used;the mobile phase was acetic acid in water(1→100)-methanol-tetrahydrofuran(990∶5∶5),the flow rate was 1.0 mL/min,the column temperature was 30℃,the injection volume was 10μL,and the detection wavelength was 254 nm.The retention time of the main peak is about 19.6 min,and the retention time of impurities 1-5 are about 4.6,8.8,25.8,12.1 min and 10.2 min.The column and the diluent were optimized.The specificity,accuracy,repeatability,LOQ and LOD,linearity and range of the method were validated,and the correction factors of related substances were calculated.Six batches of Cefminox Sodium for injection of two specifications were detected by this method.Results:The most suitable column was:Agilent ZorbaxSB-AQ,250 mm×4.6 mm,5μm,and the diluent was:water-methanol-tetrahydrofuran(990∶5∶5).The method has good specificity,accuracy and precision meet the requirements.According to the limit of quantitation,detection limit and linearity,the concentration range of main substance and impurities was determined,and then the correction factors of impurities were obtained.The correction factors of impurities 1-5 are 2.73,0.32,1.05,1.21 and 1.15.The test results of related substances of 6 batches of test samples were all meet the quality standard.Conclusion:The HPLC method for the determination of related substances in Cefminox Sodium for injection is successfully developed.The method has good specificity,accuracy,repeatability,range of linearity.
作者
于涵光
徐亮
YU Han-guang;XU Liang(Department of Pharmaceutical Analysis,College of Pharmacy,Tianjin Medical University,Tianjin 300070,China;Benova(Tianjin)innovation Pharmaceutical Research Co.,Ltd,Tianjin 300022,China)
出处
《天津医科大学学报》
2021年第5期529-532,537,共5页
Journal of Tianjin Medical University
基金
国家自然科学基金(81402889)。
