摘要
目的采用高效液相色谱-二极管阵列光谱检测-电喷雾离子化质谱联用技术对铁皮石斛叶中黄酮碳苷类成分进行分析和鉴别。方法用XB C18色谱柱(4.6 mm×250 mm,5μm);0.4%甲酸水溶液-甲醇为流动相,梯度洗脱,流速为1.0 mL.min-1;柱温30℃;DAD扫描范围190～400 nm;检测波长335 nm。Agilent电喷雾离子阱多级质谱仪;负离子检测模式;毛细管电压4 500 V;干燥气温度350℃,干燥气流量12.0 L.min-1,雾化气压力241 kPa;扫描范围m/z 50～600。结果首次从铁皮石斛叶中快速发现和鉴定了苷元均为芹菜素的8种黄酮二碳糖苷类化合物,单糖均连接在C-6位和C-8位。并探讨了黄酮碳苷化合物电喷雾质谱(ESI-MSn)特征碎裂规律。结论该方法灵敏度高、分离度好,适用于铁皮石斛叶化学成分的快速鉴定。黄酮二碳糖苷ESI-MSn特征碎裂规律为快速发现和鉴定黄酮碳苷类化合物有一定借鉴作用。
OBJECTIVE To identify flavone C-glycosides in Dendrobium officinale leaves by high performance liquid chromatography with DAD and electrospray ionization mass spectrometry （ HPLC-DAD-ESI-MS^n ）. METHODS The chromatographic separation was carried out at 30℃ on a XB C18 column （4.6mm×250mm,5μm） eluted with gradient program. The mobile phase consisted of methanol and water containing 0. 4% formic acid. The detection wavelength was 335 nm and the on-line UV spectra was recorded in the range of 190 -400 nm. The mass spectra was obtained by Agilent ion trap mass spectrometer in the negative ion mode with capillary voltage 4 500 V, dry gas temperature 350℃, dry gas flow 12. 0 L·min^-1, nebulizer pressure 241 kPa; mass range recorded m/z 50 -600. RESULTS Eight flavone di-C-glycosides from D. officinale leaves, whose aglycone was apigenin and monosaccharide was connected with C-6 and C-8, were identified by HPLC-DAD-ESI-MS^n for the first time. The study further proved the characteristics of fragmentation pattern of flavone C-glycosides in ESI-MSn. CONCLUSION The method is simple and rapid for the identification of D. officinale leaves. The characteristics of fragmentation pattern of ESI-MS^n in flavone di-C-glycosides provide a reference for rapid de- tection and identification of flavone C-glycosides.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2012年第1期13-19,共7页
Chinese Pharmaceutical Journal
基金
浙江省科技厅重大专项(2006C13014)
浙江省科技厅项目(2009F70034)
浙江省教育厅项目(Y200804797)
2010年浙江省高等学校优秀青年教师资助项目
