诺氟沙星葡萄糖注射液有关物质检测方法的研究

Study on Detection Method of Related Substances in Norfloxacin Glucose Injection

目的:建立诺氟沙星葡萄糖注射液有关物质检查的高效液相色谱方法。方法:色谱柱为SHISEIDOC18柱(4.6 mm×250 mm,5μm),流动相A为0.02 mol/L磷酸溶液(用三乙胺调节pH至(3.0±0.1))-乙腈(90∶10),流动相B为乙腈,按不同比例梯度洗脱,流速:1.0 mL/min;检测波长:278 nm;柱温:40℃;进样量:20μL;以诺氟沙星对照品峰面积按外标法计算有关物质含量。结果:诺氟沙星葡萄糖注射液主成分峰及各降解产物峰间能较好分离,15批样品中未检出杂质A、E、H,杂质K的含量为0.05%,样品中单个最大杂质的平均含量为0.08%~0.10%,总杂质的平均含量为0.20%。酸、碱、氧化、紫外光破坏试验证明方法的专属性良好。结论:所建立的方法专属性强、灵敏度高,各峰的分离良好,可用于诺氟沙星葡萄糖注射液的有关物质检查。

Objective:To establish a high performance liquid chromatography method for the detection of related substances in norfloxacin glucose injection.Methods:Chromatographic column is SHISEIDO C18 column(4.6 mm×250 mm,5μm),mobile phase A is 0.02 mol/L phosphoric acid solution(adjusted to pH(3.0±0.1)by triethylamine)-acetonitrile(90:10),and mobile phase B is acetonitrile,with gradient elution in different proportions.Flow rate:1.0 mL/min;detection wavelength:278 nm;column temperature:40℃;injection volume:20μL.The peak area of norfloxacin was used to calculate the content of related substances according to the external standard method.Results:The main component peaks in norfloxacin glucose injection and the peaks of each degradation product can be separated well.Impurity A,E,and H were not detected in 15 batches of samples.The content of impurity K was 0.05%.The average content of single maximum impurity was 0.08%-0.10%,and the average content of total impurities was 0.20%.Research of destructive test under acid,alkaline,oxidation and ultraviolet light,proved that the method has good specificity.Conclusion:The established method has good specificity,high sensitivity,and good separation of each peaks.It can be used for the detection of related substances in norfloxacin glucose injection.