基于UPLC-Q-TOF-MS/MS技术分析利拉萘酯中主要杂质  

Analysis on major impuritiy in liranaftate based on UPLC-Q-TOF-MS/MS

作　　者：陈丹红[1] 顾勇[1] 陈文明[2] 龙红萍[2] CHEN Danhong;GU Yong;CHEN Wenming;LONG Hongping(The Fifth Hospital of Jiangyin,Jiangyin 214415,China;The First Affiliated Hospital of Hunan University of Chinese Medicine,Changsha 410007,China)

机构地区：[1]江苏省江阴市第五人民医院,江苏江阴214415 [2]湖南中医药大学第一附属医院,湖南长沙410007

出　　处：《中国医药科学》2017年第11期36-39,共4页China Medicine And Pharmacy

摘　　要：目的采用液相色谱-四极杆飞行时间串联质谱法(HPLC-Q-TOF-MS)分析利拉萘酯原料中主要杂质并对其结构进行鉴定。方法色谱柱为Agilent Extend C18(2.1×100 mm,1.8μm),流动相为0.1%甲酸水(A)-乙腈(B),梯度洗脱,体积流量为0.4m L/min;离子源:ESI离子源;扫描模式:正离子扫描。结果根据各降解杂质的二级质谱图以及高分辨数据,利拉萘酯原料中主要存在6个有关物质,主要来源于原料中间体和降解产物。结论建立的方法能有效地分离主成分利拉萘酯与有关物质,为利拉萘酯原料药的质量控制、工艺优化及贮存提供参考。Objective To analyze major impuritiy in liranaftate by ultra performance liquid chromatographyquadrupole-time of flight mass spectrometry(HPLC-Q-TOF-MS).Methods Chromatographic column was Agilent Extend C18(2.1×100mm,1.8μm)and mobile phase was0.1%formic acid-water(A)-acetonitrile(B)with gradient elution.Volume flow was0.4m L/min.Ion source was electrospray ionization(ESI)ion source.Scanning mode was positive ion scanning.Results According to secondary mass spectrum of degradation impurity and high resolution data,liranaftate mainly had6related substances which are mainly from raw material intermediate and degradation product.Conclusion The established method can effectively separate principal component liranaftate and related substances,which can provide reference for quality control,technology optimization and storage of liranaftate raw medicine.

关 键 词：利拉萘酯 有关物质 杂质结构鉴定 超高效液相色谱-四极杆飞行时间串联质谱法 

分 类 号：R927.2[医药卫生—药学]