HPLC-ELSD分析硫酸异帕米星及其注射液  

Determination of Isepamicin Sulfate and its Injection by HPLC-ELSD

作　　者：王建 阮丹[2] 王知坚 

机构地区：[1]浙江省食品药品检验研究院,杭州310004 [2]浙江工业大学,杭州310014

出　　处：《中国现代应用药学》2013年第4期411-416,共6页Chinese Journal of Modern Applied Pharmacy

基　　金：国家药典委员会国家药品标准提高研究项目[国药典化发(2010)84号]

摘　　要：目的建立HPLC-ELSD测定硫酸异帕米星及其注射液的有关物质、硫酸盐和含量的方法。方法采用AgilentSB-C18柱(4.6 mm×250 mm,5μm),有关物质测定采用梯度洗脱法,流动相A为0.2 mol.L 1三氟乙酸溶液,流动相B为甲醇。硫酸盐和含量测定采用等度洗脱法,流动相为0.2 mol.L 1三氟乙酸溶液,流速为0.8 mL.min 1。Alltech 3300 ELSD检测器,漂移管温度为50℃。结果异帕米星与中间体、副产物完全分离。异帕米星、硫酸盐、庆大GE-B、庆大霉素B、3N-异帕米星在一定的浓度范围内呈较好的线性关系,硫酸异帕米星注射液含量测定的平均回收率为100.0%(RSD=0.8%,n=9),有关物质测定庆大GE-B、3N-异帕米星、庆大霉素B的回收率分别为104.4%,97.6%和109.0%,异帕米星、庆大GE-B、庆大霉素B、3N-异帕米星的检测限分别为5.1,4.5,5.1和5.0μg.mL 1。结论本方法简便、灵敏、重复性好,可用于本品的质量控制。OBJECTIVE To develop a new HPLC-ELSD method for the determination of isepamicin sulfate and its injection. METHODS The column was Agilent SB-C18（4.6 mm×250 mm, 5 μm）. The mobile phase for the determination of related substances consisted of 0.2 mmol.L-1 trifluoroacetic acid （A） and methanol （B） with gradient program. The mobile phase for the determination of isepamicin and sulfate was 0.2 mol.L-1 trifluoroacetic acid. The flow rate was 0.8 mL＇min-1. Detector used was an Alltech 3300 ELSD detector. The drift tube temperature was 50 ℃. RESULTS Good separation of isepamicin from main intermediates could be achieved. The standard curves of isepamicin, sulfate, HAPA-gentamine-B, 3N-isepamicin and gentamine-B were linear in the certain range. The average recovery of isepamicin for the determination of isepamicin sulfate injection was 100.0% （RSD=0.8%, n=9）. The average recoveries of HAPA-gentamine-B, 3N-isepamicin and gentamine-B for the determination of related substances were 104.4%, 97.6% and 109.0%, respectively. The detection limits of isepamicin, HAPA-gentamine-B, gentamine-B and 3N-isepamicin were 5.1, 4.5, 5.1 and 5.0 μg·mL^-1, respectively. CONCLUSION The method is simple, sensitive and reproducible, and can be used for quality control of isepamicin sulfate and its injecton.

关 键 词：硫酸异帕米星 有关物质 硫酸异帕米星注射液 梯度洗脱 高效液相色谱-蒸发光散射检测法 

分 类 号：R917.101[医药卫生—药物分析学]