HPLC-DAD-MS／MS法快速分析布格呋喃降解产物

Analysis and identification of degradation products of buagafuran by high performance liquid chromatography-diode array detection-tandem mass spectrometry

利用HPLC-DAD-MS/MS对布格呋喃降解产物进行快速分离分析和结构鉴定。以Zorbax C8(5μm,4.6 mm×150 mm)为色谱柱,乙腈水(78∶22)为流动相,采用电喷雾离子源,正离子模式检测。通过高效液相色谱串联质谱和DAD检测器联用,在线分离并检测降解产物。根据降解产物的保留时间、紫外光谱及MS、MS/MS数据,结合布格呋喃的可能降解反应推断降解产物的结构。结果表明布格呋喃中6个主要降解产物均为布格呋喃的氧化或过氧化产物。降解产物A为布格呋喃的双键环氧化产物,降解产物B、C、D、E是在降解产物A的基础上进一步氧化形成的二级或多级产物,降解产物F为布格呋喃的过氧化产物。本文建立的HPLC-DAD-MS/MS法可快速分析布格呋喃中的降解产物,为降解产物鉴定提供重要的结构信息。

An HPLC-DAD-MS/MS method was developed for rapid analysis and identification of degradation products of buagafuran. Buagafuran and degradation products were separated on a Zorbax C s column （5 μm, 4.6 mm × 150 mm） using aeetonitrile-water （78 ： 22） as mobile phase. The elutes were detected with diode array detector and tandem mass spectrometer via electrospray ionization source in positive ion mode. According to analysis of the retention time, UV spectra and MS, MS/MS data, combined with the possible degradation reaction of buagafuran, the structures of main degradation products were inferred. The results showed that six main degradation products were oxidation or peroxidation productions of buagafuran. Degradation product A was a double bond epoxidation product of buagafuran, degradation products B, C, D and E were the further oxidation products of degradation product A, degradation product F was a peroxidation product of buagafuran. The results indicated that the established method was effective in the rapid identification of the degradation products of buagafuran.