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目的:建立液相色谱-紫外光谱-离子阱质谱法分析灰黄霉素原料中主要杂质。方法:采用反相梯度色谱系统对灰黄霉素溶液进行分离,以紫外检测。对其中的主要杂质采用电喷雾离子阱质谱进行多级质谱分析,鉴定结构。结果:经多级质谱解析,鉴定了灰黄霉素原料中的6个杂质,分别为去氯灰黄霉素、去氢灰黄霉素、异灰黄霉素、灰黄霉酸、4-去甲灰黄霉素和6-去甲灰黄霉素。结论:本研究为测定灰黄霉素中相关杂质提供了新的分析方法,有助于加强灰黄霉素的质量控制。
Objective: To establish a method for the analysis of major impurities in griseofulvin by liquid chromatography-ultraviolet spectrum-ion trap mass spectrometry. Methods: The griseofulvin solution was separated by reversed-phase gradient chromatography and detected by UV. The main impurities were analyzed by electrospray ion trap mass spectrometry to identify the structure. Results: Six impurities of griseofulvin were identified by mass spectrometry. They were griseofulvin, gliadin, griseofulvin, fulvic acid, Nordic griseofulvin and 6-nordic griseofulvin. Conclusion: This study provides a new analytical method for the determination of related impurities in griseofulvin, which helps to improve the quality control of griseofulvin.