摘要
目的:建立LC-PDA-MS/MS法分析高三尖杉酯碱及其注射液的杂质谱。方法:采用Phenomenex C18色谱柱,以0.01 mol·L^-1乙酸铵(0.1%乙酸)-乙腈为流动相,进行梯度洗脱,流速为0.3 mL·min^-1;通过光电二极管阵列检测器及电喷雾质谱检测法,采集杂质谱的PDA数据及各杂质的碎片离子数据,结合杂质的色谱行为及相关对照品的裂解规律,对未知杂质结构进行解析。结果:从原料药中分离出14个杂质,注射液中分离出15个杂质,并与对照品比对确定了其中1个杂质为三尖杉酯碱,另外分析了各杂质的归属与关联性。结论:建立的方法可有效分离高三尖杉酯碱及其注射液的杂质,通过对杂质谱的分析推断出各杂质的结构,为高三尖杉酯碱原料及其注射液质量控制提供一定的参考依据。
Objective:To establish an LC-PDA-MS/MS method for the determination of impurity profile in homoharringtonine and its injection. Methods:The HPLC separation was performed on a Phenomenex C18 column by gradient elution,with a mobile phase consisting of 0.01 mol·L^-1 ammonium acetate(0.1% acetic acid)aqueous solution and acetonitrile at a flow rate of 0.3 mL·min^-1. The results were obtained by PDA and tandem mass spectrometry.The PDA data, debris ion data of all impurity in homoharringtonine were collected and the unknown impurity structure was elucidated according to chromatographic behavior of impurity and the fragmentation regularity of related reference substances. Results:The fourteen and fifteen impurity peaks were separated in homoharringtonine and its injection,respectively. One impurity peak could be identified as harringtonine by comparison with the behaviour of a reference substance in the same conditions. Also the attribution and association of each impurity were analyzed. Conclusion:The established method is effective for the separation of the related substances in homoharringtonine and its injection. The structure of the impurity can be determined by the analysis of impurity profile,which provide a reference for quality control of the homoharringtonine and its injection.
作者
杨丽萍
刘泽涛
独家启
崔广青
董庆斌
YANG Li-ping;LIU Ze-tao;DU Jia-qi;CUI Guang-qing;DONG Qing-bin(Shanxi Provincial Institute of Food and Drug Control,Taiyuan 030000,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2019年第10期1882-1894,共13页
Chinese Journal of Pharmaceutical Analysis
关键词
高三尖杉酯碱
高三尖杉酯碱注射液
杂质谱
裂解规律
液质联用
homoharringtonine
homoharringtonine injection
impurity profile
fragmentation regularity
LC-PDAMS/MS
