液相色谱-紫外光谱-离子阱质谱法分析灰黄霉素中的相关杂质

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 develop an LC-UV/MS method for analysis of impurities of griseofulvin. Methods: Reversed-phase gradient chromatography was used to separate griseofulvin solution,which was detected by UV detector.The major impurities were identified by ion trap mass spectrometry equipped with ESI source in the positive ion mode. Results: Six impurities of griseofulvin,including dechlorgriseofulvin,dehydrogriseofulvin,isogriseofulvin,griseofulvic acid,4-demethylgriseofulvin and 6-demethylgriseofulvin were identified. Conclusion: The new developed method for the analysis of the related impurities in griseofulvin is useful to control the quality of griseofulvin.