基于LCMS-IT-TOF技术分析注射用头孢他啶聚合物杂质  

Analysis of ceftazidime polymer impurities for injection based on LCMS-IT-TOF technology

作　　者：杨俊斌 傅小雅 Yang Junbin;Fu Xiaoya(Hainan Provincial Institute of Inspection and Testing Drug Control,Haikou 570216)

机构地区：[1]海南省检验检测研究院,海口570216

出　　处：《中国抗生素杂志》2025年第3期336-343,共8页Chinese Journal of Antibiotics

摘　　要：目的对注射用头孢他啶聚合物杂质进行分析。方法采用高效液相-离子肼与飞行时间串联质谱(LCMS-IT-TOF)技术,利用杂质对照品,结合强制聚合法制备富含聚合物杂质的降解溶液,对注射用头孢他啶中聚合物杂质进行定位分析。进行RP-HPLC法和葡聚糖凝胶G10(Sephadex G10)色谱法检测注射用头孢他啶聚合物杂质的比较。结果LCMS-IT-TOF技术共推定7个未知杂质(杂质N1、N2、未知杂质3、O、P1、P2、T)和3个已知杂质(Q1、Q2、R)的化学结构,并证明已知杂质D在实际样品中不存在。较葡聚糖凝胶G10色谱法,RP-HPLC法分析头孢他啶聚合物杂质专属性强,结果客观准确。结论LCMS-IT-TOF技术,正负极性可高速切换,具有极好的质量稳定性,可保证正离子模式和负离子模式下的高质量精确度,从而获得更可靠的质谱分析结果。Objective To analyze ceftazidime polymer impurities for injection.Methods The polymer impurities in ceftazidime for injection were localized and analyzed by using high-performance liquid-phase ion trap and time-of-flight tandem mass spectrometry(LCMS-IT-TOF).Use an impurity control combined with forced polymerization to prepare a degradation solution rich in polymer impurities.A comparison was made between RPHPLC and Sephadex G10 for the determination of impurity in ceftazidime polymer for injection.Results The LCMS-IT-TOF technique inferred the chemical structure of 7 unknown impurities(impurities N1,N2,3,O,P1,P2,T)and 3 known impurities(impurities Q1,Q2 and R).It was also proved that the known impurity D did not exist in the actual sample.Compared with Sephadex G10 chromatography and RP-HPLC methods,this ceftazidime polymer impurity analysis was more specific,objective,and accurate.Conclusion The LCMS-IT-TOF technology,with positive and negative polarity switched at high speed and excellent mass stability,could ensure high-quality accuracy in positive and negative ion mode,resulting in more reliable mass spectrometry results.

关 键 词：注射用头孢他啶 聚合物杂质 LCMS-IT-TOF 分子质量 化学结构 

分 类 号：R917[医药卫生—药物分析学]