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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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高三尖杉酯碱及其注射液杂质谱的研究

Impurity profile analysis of homoharringtonine and its injection

分类号:R917
出版年·卷·期(页码):2019,39 (10):1882-1894
DOI: 10.16155/j.0254-1793.2017.01.01
-----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。

-----英文摘要:---------------------------------------------------------------------------------------

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.

-----参考文献:---------------------------------------------------------------------------------------

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