醋酸氟孕酮原料药相关物质分析  

Study on the related substances of flugestrone acetate

作　　者：张玉峰[1] 史培颖[1] 程翼宇[1] 

机构地区：[1]浙江大学药物信息学研究所,杭州310058

出　　处：《药物分析杂志》2007年第11期1735-1737,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:鉴定醋酸氟孕酮原料药中的含量大于0.1%的相关物质。方法:运用液相色谱-光电二极管阵列检测-电喷雾离子阱质谱联用技术对醋酸氟孕酮原料药中的相关物质进行分离检测,然后比较相关物质与醋酸氟孕酮类似物的紫外光谱特征和二级质谱的裂解特征,确定相关物质的结构。结果:在醋酸氟孕酮原料药中检测到5个相关物质,其中17-乙酰氧基-9-氟-11,17-二羟基-孕甾4,6-二烯-3,20-二酮(P5,t_R=13.13 min)的含量大于0.1%,综合使用 LC/MS^n 和 DAD技术确定了其结构。结论:所鉴定的相关物质为醋酸氟孕酮的新副反应产物。Objective： To identify the related impurities in flugestone acetate. Method： A hyphenated HPLC - DAD - MS^n method was developed to analyze the related impurities of flugestone acetate. Their relative molecular mass can be determined according to their quasi - molecular ions and adduct ions. Two model compounds were analyzed at the same condition and their multi - stage mass spectra and UV spectra were compared with the spectra of flugestone acetate impurities. Results：5 Related compounds were detected and one peak＇ s（tR = 13. 13 rain）content was more than 0. 1% ,which was identified to be 17 - acetoxy - 9 - fluoro - 11, 17 - dihydroxy - pregn - 4,6 - diene - 3,20 - dione. Conclusion： 17 - Acetoxy - 9 - fluoro - 11,17 - dihydroxy - pregn - 4,6 - diene - 3,20 - dione（ P5 ） is a new byproduct of flugestone acetate.

关 键 词：醋酸氟孕酮 HPLC—DAD—ESI/MS^n 17-乙酰氧基-9-氟-11 17-二羟基-孕甾-4  6-二烯-3  20-二酮(P5) 

分 类 号：R917[医药卫生—药物分析学]