摘要
目的:建立HPLC-CAD法测定硫酸卡那霉素注射液中卡那霉素和卡那霉素B含量的方法。方法:采用Boston Green ODS C18(250 mm×4.6 mm,5μm)色谱柱,以0.2 mol·L^(-1)三氟醋酸溶液-甲醇(95∶5)作为流动相,流速:1.0 ml·min^(-1),柱温:30℃,喷雾温度:55℃,喷雾压力:56.4 psi。结果:卡那霉素在0.385~38.500μg·ml^(-1)之间呈现良好的线性关系(r=0.999 9),检出限为0.075μg·ml^(-1),定量限为0.154μg·ml^(-1),回收率为100.97%(n=9)。卡那霉素B在0.374~37.400μg·ml^(-1)之间呈现良好的线性关系(r=1.000 0),检出限为0.075μg·ml^(-1),定量限为0.150μg·ml^(-1),回收率为100.44%(n=9)。结论:建立的HPLC-CAD测定卡那霉素和卡那霉素B含量的方法检出限低,操作简单准确,可以有效控制硫酸卡那霉素注射液的质量。
Objective： To establish an HPLC with charge aerosol detection（ HPLC-CAD） method for the determination of kanamycin and kanamycin B in kanamycin sulfate injection. Methods： The samples were injected into a Boston Green ODS C18（ 250 mm×4. 6 mm,5 μm） column. The mobile phase was composed of 0. 2 mol·L-1 trifluoroacetic acid aqueous solution-methanol（ 95 ∶ 5）,the flow rate was 1. 0 ml·min-1 and the column temperature was maintained at 30 ℃. The nebulization temperature for the CAD was maintained at 55℃ and the gas pressure was 56. 4 psi. Results： The linear range of kanamycin was 0. 385-38. 500 μg · ml-1（ r =0. 999 9）,and the limit of detection was 0. 075μg·ml-1,the limit of quantitation was 0. 154 μg·ml-1,and the average recovery of the method was 100. 97%（ n = 9）. The linear range of kanamycin B was 0. 374-37. 400 μg·ml-1（ r=1. 000 0）,and the limit of detection was 0. 075μg·ml-1,the limit of quantitation was 0. 150 μg·ml-1,and the average recovery of the method was 100. 44%（ n= 9）. Conclusion： The method for the determination of kanamycin and kanamycin B by HPLC-CAD is simple and accurate,the limit of detection is lower than HPLC-ELSD,and the quality of kanamycin sulfate injection can be effectively controlled.
作者
郭永辉
李香荷
Guo Yonghui;Li Xianghe(Hebei Institute for Drug Control, Shijiazhuang 050011, China)
出处
《中国药师》
CAS
2018年第6期1090-1092,共3页
China Pharmacist
基金
河北省食品药品监督管理局2015年度食品药品安全科技项目计划(编号:QN2015008)
