地佐辛注射液有关物质的色谱-质谱结构鉴定  

Structure Identification of the Related Substances of Dezocine Injections by LC-MS Techniques

作　　者：秦皖宁 殷康明 唐天 杭太俊[1] 宋敏[1] QIN Wanning;YIN Kangming;TANG Tian;HANG Taijun;SONG Min(Department of Pharmaceutical Analysis,China Pharmaceutical University,Nanjing 210009,China)

机构地区：[1]中国药科大学药物分析系,南京210009

出　　处：《药学与临床研究》2023年第6期486-496,共11页Pharmaceutical and Clinical Research

摘　　要：目的:采用色谱-质谱联用技术鉴定地佐辛注射液中的有关物质。方法:采用Agilent Eclipse Plus C_(18)(150 mm×4.6 mm,5μm)色谱柱,以甲醇-10 mmol·L^(-1)甲酸铵缓冲溶液(甲酸调节pH至2.7)为流动相梯度洗脱,对地佐辛注射液有关物质进行分离,电喷雾正离子化-四极杆-飞行时间串联高分辨质谱(ESI-Q-TOF/MS)测定各有关物质母离子及其子离子的准确质量和元素组成,通过光谱解析鉴定其结构。结果:在所建立的分析条件下,地佐辛及其有关物质分离良好,检测并鉴定出地佐辛注射液及其强制降解试验样品中20个含量大于0.1%的有关物质,其中2个为已知杂质,其他杂质均未见报道。结论:色谱-质谱联用技术能有效地分离鉴定地佐辛注射液中的有关物质,为其质量控制提供参考依据。Objective:This study aimed to identify the related substances of dezocine injections by liquid chromatography mass spectrometry.Methods:To separate the related substances of dezocine injections,gradient elution was performed using methanol,10 mmol·L^(-1) of ammonium formate(formic acid adjusts the pH to 2.7)as mobile phase on an Agilent Eclipse Plus C_(18) column(150 mm×4.6 mm,5μm).The accurate mass and elemental composition of the parent ions and their product ions of related substances were determined by electrospray-ionization quadrupole time-of-flight high resolution mass spectrometry(ESI-Q-TOF/MS).Results:The structures of the related substances were identified by spectral analysis.Under the established analytical condition,dezocine and its related substances were adequately separated,and 20 related substances with contents greater than 0.1%were detected and identified by hyphenated techniques in dezocine injections and its stressed samples.Among them,two were the known impurities and none of the other impurities had been reported.Conclusion:The LC-MS techniques can effectively separate and identify the related substances of dezocine injections and provide reference for the establishment of quality control.

关 键 词：地佐辛注射液 有关物质 降解产物 结构鉴定 色谱-质谱联用 

分 类 号：R914.1[医药卫生—药物化学] R927.11[医药卫生—药学]