谷氨酸诺氟沙星氯化钠注射液有关物质测定方法考察

Determination of Related Substances in Norfloxacin Glutamate and Sodium Chloride Injections

目的：建立谷氨酸诺氟沙星氯化钠注射液中有关物质的检测方法，并与现行方法进行比较。方法：色谱柱：DiamonsilC18（2）（250mm×4.6mm，5μm）；流动相：A为0.025mol·L-1磷酸溶液-乙腈（87∶13），B为乙腈，梯度洗脱，流速：1.0ml·min-1;检测波长：278nm、262nm；进样量：20μl；柱温：25℃。结果：在梯度洗脱的条件下，样品的稳定性及分离度良好。杂质A在0.032～3.179μg·ml-1范围内线性关系良好（r=1.0000），检出限为0.159ng，平均回收率为98.3%，RSD为0.64%（n=9）。结论：梯度洗脱方法结果准确、灵敏度高、专属性强、重复性好，可用于谷氨酸诺氟沙星氯化钠注射液有关物质的检测。

Objective： To detect the related substances in norfloxacin glutamate and sodium chloride injections on the basis of norfloxacin related substances analysis method described in Chinese Pharmacopoeia 2010 edition to establish a more scientific and feasible method. Methods： HPLC was performed under the following conditions： a Diamonsil C18（2）（250 mm×4.6 mm，5 μm） column, mobile phase A of 0.025 mol·L-1 phosphoric acid acetonitrile（87∶13）, phase B of acetonitrile, with gradient elution at a flow rate of 1.0 ml·min-1, the detection wavelength of 278nm and 262nm, the injection volume of 20 μl, and the column temperature of 25℃. Results：Under the HPLC conditions, the samples had good stability and separation. An excellent linear relationship was achieved within the range of 0.032-3.179 μg·ml-1（r=1.000 0）,the detection limit of impurity A was 0.159 ng，and the average recovery was 98.3% with RSD of 0.64%（n=9）. Conclusion：Compared with the existing methods, the gradient elution method is accurate, sensitive, specific and reproducible, and can be used in the determination of related substances in norfloxacin glutamate and sodium chloride injections.