HPLC-CAD法测定硫酸核糖霉素有关物质及含量  

Simultaneous detection of ribostamycin sulfate and its related substances using a HPLC-CAD method

作　　者：孟飞 史孙亮 侯玉荣 赵恂 施海蔚 张锦琳 周小华 袁耀佐 MENG Fei;SHI Sun-liang;HOU Yu-rong;ZHAO Xun;SHI Hai-wei;ZHANG Jin-lin;ZHOU Xiao-hua;YUAN Yao-zuo(Nanjing University of Chinese Medicine,Nanjing 210023,China;Jiangsu Institute for Food and Drug Control,Nanjing 210019,China;NMPA Key Laboratory for Impurity Profile of Chemical Drugs,Nanjing 210019,China;Nanjing Real Mind Biotech,Nanjing 210034,China)

机构地区：[1]南京中医药大学,南京210023 [2]江苏省食品药品监督检验研究院,南京210019 [3]国家药品监督管理局化学药品杂质谱研究重点实验室,南京210019 [4]南京仁迈生物科技有限公司,南京210034

出　　处：《药物分析杂志》2023年第10期1766-1773,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立用于测定硫酸核糖霉素有关物质及含量的高效液相色谱-电喷雾检测器(HPLC-CAD)法,优化补充2020年版《中华人民共和国药典》方法。方法:采用Agilent Zorbax SB-C_(18)(250 mm×4.6 mm,5μm)色谱柱,以0.15%(v/v)五氟丙酸+0.2%(v/v)三氟乙酸-甲醇(95∶5)作为流动相,流速1.0 mL·mL^(-1),柱温40℃;电喷雾检测器温度50℃。结果:所建立方法使核糖霉素及其有关物质实现良好分离,核糖霉素质量浓度在2~200μg·mL^(-1)范围内,其峰面积与浓度呈良好的线性关系(r=0.9983),检测限(LOD)为0.8μg·mL^(-1),定量限(LOQ)为2μg·mL^(-1),重复性和精密度试验RSD均<2.0%。HPLC-CAD法测定硫酸核糖霉素及有关物质含量为0.81%~1.02%、74.64%~75.22%。结论:相比于2020年版《中华人民共和国药典》硫酸核糖霉素的检测方法,该方法专属性强,灵敏度和稳定性好,为硫酸核糖霉素质量控制提供了可靠的分析手段。Objective:To establish a high performance liquid chromatography-charged aerosol detector(HPLC-CAD)method for the determination of ribostamycin sulfate and its related substances,and optimize and supplement Chinese Pharmacopoeia(2020 edition).Methods:Agilent Zorbax SB-C_(18)(250 mm×4.6 mm,5μm)column was used with 0.15%(v/v)pentafluorpropionic acid+0.2%(v/v)trifluoroacetic acid-methanol(95∶5)as the mobile phase,and the flow rate was 1.0 mL·mL^(-1).The column temperature was 40℃.The temperature of the CAD was set at 50℃.Results:The established method achieved good separation of ribostamycin and its related substances.The peak area and concentration of ribostamycin showed a good linear relationship in the mass concentration range of 2μg·mL^(-1)to 200μg·mL^(-1)(r=0.9983),the limit of detection(LOD)was 0.8μg·mL^(-1)and the limit of quantification(LOQ)was 2μg·mL^(-1).The RSD of the repeatability and precision experiments were both less than 2.0%.HPLC-CAD method was used to determine the impurities and contents of ribostamycin sulfate in the range of 0.81%-1.02% and 74.64%-75.22%.Conclusion:Compared with the detection method of ribostamycin sulfate in Chinese Pharmacopoeia(2020 edition),the method has good specificity,sensitivity and stability,and provides a reliable analytical means for the quality control of ribostamycin sulfate.

关 键 词：硫酸核糖霉素 电喷雾检测器 蒸发光散射检测器 纳克级激光计数检测器 含量测定 有关物质 

分 类 号：R917[医药卫生—药物分析学]