【摘要】 目的:采用HPLC-MS-MS法,对桑叶总生物碱部位中的各生物碱成分进行分析和鉴别,采用柱前衍生化HPLCUV测定生物碱部位中总生物碱的含量。方法:采用HiQSiL C18色谱柱(4.6 mm×250 mm,5μm),以9-氯甲酸芴甲酯(FMOCCl)为柱前衍生化试剂,流动相乙腈-0.1%醋酸(50∶50),流速0.8 mL·min-1,检测波长254 nm,电喷雾离子源(ESI),正离子检测模式,以1-脱氧野尻霉素(DNJ)为对照,外标法计算桑叶总生物碱含量。结果:鉴定了6个生物碱类成分分别为DNJ,fagomine,3-epi-fagomine,DAB,calystegine B2和2-O-β-Glc-DAB;测定3批供试品中总生物碱含量均达到75%以上。结论:该法简便、准确、灵敏,可用于桑叶总生物碱及其制剂的定性定量分析。更多还原

【Abstract】 Objective: To use liquid chromatography-mass spectrometry techniques for qualitative analysis of alkaloids of Mori Folium and determine the content of total alkaloids in alkaloids in Mori Folium by HPLC-UV with pre-column derivatization. Method: The chromatographic separation was performed on a HiQSiL C 18 column( 4. 6 mm × 250 mm,5 μm) using acetonitrile and 0. 1% acetic acid aqueous solution under isocratic elution( 50∶ 50) at a flow rate of 0. 8 mL·min- 1. Mori Folium alkaloids was analyzed with 9-fluorenylmethyl chlorformate( FMOC-Cl) as the pre-column derivative agent. Detection wavelength was set at 254 nm with electrospray ionization source( ESI) and positive ion mode. And 1-deoxynojirimycin as the external standard to calculate mulberry leaf total alkaloid content. Result: Six alkaloid compounds were identified as DNJ,fagomine, 3-epi-fagomine,DAB,calystegine B 2 and 2-O-β-Glc-DAB. The content of 3 batches test samples were more than 75%. Conclusion: The method is sensitive,accurate,simple,and reliable. It can be used for quantitative analysis of Mori Folium alkaloids and preparation.更多还原