电喷雾离子阱质谱分析17-烯丙胺基-17-脱甲基格尔德霉素及其代谢物

Analysis of 17-allylamino-17-demethoxygeldanamycin and Its Active Metabolites by Electrospray Ionization Mass Spectrometry

目的旨在确立17-烯丙胺基-17-脱甲基格尔德霉素(17AAG)及其代谢物的质谱分析条件。方法采用电喷雾离子阱质谱,同时用液质联用方法,对17AAG及其主要活性代谢产物17-氨基-17-脱甲基格尔德霉素(17AG)进行了探讨,同时分离并考察了其在大鼠胆汁中的代谢物及其一般裂解规律。结果在电喷雾负离子模式下,所产生的准分子离子峰均为[M-H]-峰,在MS2质谱中均产生失去43u的碎片峰,在MS3质谱中均产生失去98u,18u的碎片峰。结论这些裂解特征可用于该类化合物的结构鉴定及代谢物的分析。

Objective To determine the analysis conditions of 17-allylamino-17-demethoxygeldanamycin and its metabolites by mass spectrometry. Methods Electrospray ionization mass spectrometry and liquid chromatography- mass spectrometry （LC-MS） were adopted to investigate the 17 - allylamino - 17 - demethoxygeldanamycin （17AAG） and its main active metabolite 17 - amino - 17 - demethoxygeldanamycin （17AG）. Its metabolites in the bile of rats were separated and the regular separation rules were studied as well. Results It was found that the quasi-molecular peaks produced under electrospray ionized mode were all [M-H]^-. Fragmented peaks lost 43 u were produced in mass spectrum of MS2. Fragmented peaks lost 98 u and 48 u were both produced in MS3 spectrum. Conclusion These splitting properties can be used for the identification of the structure of this type of compound and the analysis of its metabolites.